September 2010 - uni-hohenheim.de...quantification of 5–15 (depending on the matrix) and 30...

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The versatility of HPTLC – From Bio Analysis to the Detection of Pollutants in Water

AMD chromatogram of Stratum corneum lipids

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CAMAG BIBLIOGRAPHY SERVICE

No. 105, September 2010CAMAG Bibliography Service Planar Chromatography Edited by Gerda Morlock [email protected] published by CAMAG Switzerland

CAMAG (Switzerland) Sonnenmattstr. 11 • CH-4132 Muttenz 1 Tel. +41 61 4673434 • Fax +41 61 4610702 [email protected] • www.camag.com

CAMAG Scientific Inc. (USA) 515 Cornelius Harnett Drive Wilmington, NC 28401 Phone 800 334 3909 • Fax 910 343 1834 [email protected] • www.camagusa.com

IN THIS ISSUE

Procedures, applicationsTLC/HPTLC-ELSD-MS coupling ...... 2–4

Determination of the glycoalkaloids -solanine and -chaconine in potatoes at different steps of potato processing ..................... 5–6

1H-Benzotriazole and tolyltriazole in the aquatic environment..................... 7–9

Optimization of an AMD 2 method for determination of stratum corneum lipids ............. 10–12

Determination of additives in plastic foils ........................... 13–15

Products featured in this issue TLC Scanner 4 .................................. 4

Automated Multiple Development (AMD 2) ....... 11

TLC-MS Interface ........................... 16

Column: Know CAMAGSeminar, held by CAMAG Berlin at the University of Zittau/Görlitz ...... 8

Printed on FSC/PEFC-certified paper

Planar Chromatography in Practice

TLC/HPTLC-ELSD-MS coupling

Mr. François Bretin and Dr. Francis Maquin (right)

The Lead Generation to Candidate Realization (LGCR) platform identifies small molecule leads and progresses them up to registration. LGCR Ana-lytical Sciences (AnSci) is a new department in Sanofi-Aventis R&D, which is dedicated to support Business Divisions and Therapeutics Units. For LGCR-AnSci, Dr. Maquin* and F. Bretin in the research center in Vitry-sur-Seine use various analytical techniques (further locations are in Strasbourg, Chilly-Mazarin, Toulouse and Montpellier).

IntroductionMS coupled to chromatography supports the chemist’s decision for compound identification or follow-up in a synthesis mixture. Therefore, HPLC/UPLC-MS is mainly used, but TLC/HPTLC is also widely applied by the chemists as a rapid and reliable method to follow reaction processes.

This is especially true for cases, when compounds remain on the column, due to high polarity or weak solubility, or when analyte detection is poor (no chromophore). In such cases, the HPTLC/MS platform with the new TLC-MS Interface is ideal for structural analysis. The TLC-MS Interface was complemented by a MS soft-ware controlled valve, adding some automation to the process, and by an Evaporative Light Scattering Detector (ELSD). The latter enables the analyst to distinguish between compounds that were not eluted from the plate from those that were not sufficiently ionized for MS detection.

Sample preparationThe samples were taken directly from the reactor and diluted with an ap-propriate solvent, usually an organic solvent of medium polarity.

Standard preparationEducts or known intermediate products were dissolved and diluted with an appropriate solvent.

CBS 105 3

Chromatogram layersTLC and HPTLC plates silica gel 60 F254 10 x 20 and 10 x 10 cm, respectively. If required, the plate size was reduced with the Smartcut.

Sample applicationManually with disposable micropipettes of 5 to 20 µL volumes.Note: The Nanomat 4 is recommended to ensure precise positioning without damage of the layer. Especially for polar extracts, small volumes should be applied (

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Elution profiles obtained by ELSD and ESI-MS (top) and mass spectrum of the eluted zone (bottom)

An intensive use of the TLC/HPTLC-ELSD-MS instru-mentation requires frit cleaning twice a week. The requirement of a cleaning cycle is indicated by an increased pump pressure likely from clogging of the inline filter frit (> 10 MPa).

To conclude, our experience underlines the interest in HPTLC/TLC-MS in an advanced analytical environ-ment. The automatization, reliability of the data, and speed were the convincing arguments, which fully comply with our routine analytical needs.

Further information is available on request from the authors.

Contacts• Dr. Francis Maquin and Mr. François Bretin, Sanofi-Aventis, Centre de Recherche, 13, quai Jules Guesde, 94403 Vitry- sur-Seine cedex, France, [email protected]

• Mr. Pierre Bernard-Savary, Chromacim SAS, Pommiers la Placette, France

• Mr. Henri Gangloff, Sedere SA, Alfortville, France

• Mrs. Véronique de Nailly, BCP Instruments, Irigny, France

4

CAMAG TLC Scanner 4

Classical densitometry uses monochromatic light in the form of a slit of selectable length and width to scan the tracks of a chromatogram, measuring the diffusely reflected light. The TLC Scanner 4 – the successor of TLC Scanner 3 – is the most advanced workstation for densitometric evaluation of Thin-Layer Chromatograms currently available.

Analysts can now benefit from a wider spec-tral range for measurements from 190 to 900 nm. The optimized positioning stage and its open access allow for robust use.

For the screening of water samples in this application, densitometric determination is performed by the multi-wavelength scan covering the wavelength range between 190 and 300 nm. In combination with AMD the whole polarity range of UV-active compounds is detected. This procedure is proven to be helpful in routine search for potential water contaminants.

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Determination of the glycoalkaloids -solanine and -chaconine in potatoes at different steps of potato processing

Dr. Jens Mäder, Prof. Dr. Lothar W. Kroh

Prof. Dr. Kroh*, TU Berlin, and his group, concen- trate on carbohydrate chemistry and food analysis, especially in Maillard reaction chemistry, carameliza-tion and melanoidin formation. A further research field of both authors is the characterization of bioactive compounds of processed and unproc-essed food. Dr. Mäder is now head of product development at Milchwerke Mittelelbe, Stendal. This study [1] was performed by Dr. Mäder, Ms Hanschen and Ms Zietz (both not pictured) dur-ing their graduation.

IntroductionThe potato as a plant of the Solanaceae family contains bioactive steroidal alkaloids, which are de-terrent to herbivores and pathogens and reported to be membrantoxic, embryotoxic and teratogenic for mammalians. They influence the flavor of fresh and processed potatoes from a bitter taste toward a burning sensation at higher concentrations [2]. At the moment no limit values are fixed in Europe, and potatoes, as the most important food source of glycoalkaloids, are regarded as safe for humans if they do not contain more than 200 mg total al-kaloids per kg of fresh weight. Both main alkaloids -solanine and -chaconine exist at high levels in the tuber peel in a ratio of 1:2 to 1:7.

Chemical structure of the potato alkaloids -solanine and -chaconine

The potato is one of the world’s most important food crops. Quality-management systems demand food safety and traceability as they often follow the from farm to fork policy of regulatory authorities. Therefore, easy to use, inexpensive, and reliable analytical methods are needed to evaluate the content of toxicologically relevant compounds like glycoalkaloids after harvest and during potato stor-age and processing.

HPTLC is especially suited for effective and rapid determination of alkaloids [4] because up to 16 samples can be simultaneously separated without any matrix influence on the quality of the results. Consequently, all processing stages and by-products from one batch can be moni-tored and traced simultaneously within one analysis on one plate.

Sample preparationSamples were collected at different stages of the production chain in a commercial potato flake process. After fourfold extraction of the lyophilized, ground potato powder with methanol - acetic acid 99:5, the extracts were concentrated and directly applied.

Standard solutions5 mg each of -solanine and -chaconine were dis-solved in 25 mL methanol – acetic acid 99:1, mixed 1:1 and diluted 1:20.

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Chromatogram layerHPTLC plate silica gel 60 (Merck), 20 x 10 cm

Sample applicationBandwise with Automatic TLC Sampler 4, band length 5 mm, track distance 9.2 mm, distance from the lower edge 8 mm, application speed 70 nL/s, application volume 2–22 µL

ChromatographyIn the Horizontal Developing Chamber after 15 min chamber saturation with dichloromethane – metha-nol – ammonia (2.5 %) 70:30:4.4, migration dis-tance of 75 mm from the lower edge of plate

Post-chromatographic derivatizationWith the Chromatogram Immersion Device III the plate was dipped after 25 min drying time at 90 °C into the Carr-Price reagent (70 g SbCl3 is dissolved in 250 mL of a mixture of acetic acid – dichloro-methane 1:3), followed by heating on the TLC Plate Heater at 110 °C for 3 min.

DensitometryAbsorption measurement at 560 nm with TLC Scanner 3 and winCATS software within 15 min after derivatization, before the glycoalkaloid zones change the color from red to violet.

Results and discussionThe densitogram clearly shows the good separation of -solanine and -chaconine in the different sam-ple extracts. The extremely sensitive and selective coloring of both glycoalkaloids by dipping into the Carr-Price reagent allowed a limit of detection and quantification of 5–15 (depending on the matrix) and 30 ng/band, respectively, with a recovery rate between 94 and 105 %. Linear calibration was very satisfactory in the range of 30 to 700 ng/band (r = 0.9998, sdv = 2.5 %), polynomial even up to 1500 ng/ band (r = 0.9999, sdv = 1.5 %).

In conclusion, this method ideally complies with the analytical demands mentioned in the introduction.

Densitogram of standard substances (track 1–6) and sample extracts of different steps of potato processing (track 7–21)

Further information is available from the author on request.

*Prof. Dr. Lothar W. Kroh, lnstitut für Lebensmitteltechnologie und Lebensmittelchemie, TU Berlin, Gustav-Meyer-Allee 25, 13355 Berlin, [email protected]

Literature

[1] J. Mäder et al. J Planar Chromatogr 22 (2009) 43.

[2] S.L. Sinden , K.L. Deahl and B.B. Aulenbach, J Food Sci 41 (1976) 520.

[3] A.J.A. Essers et al. Environ Toxicol Phar 5 (1998) 155.

[4] J. Mäder, H. Rawel and L.W. Kroh, J Agric Food Chem 57 (2009) 6292.

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continuation on page 9


1H-Benzotriazole and tolyltriazole in the aquatic environment

Dr. Walter H. Weber

Dr. Wolfram Seitz, Stefan C. Weiss, Alexander Müller and Dr. Wolfgang Schulz (from left to right)

Lead by Dr. Weber* the laboratory for operation con-trol and research of Zweckverband Landeswasserver-sorgung (LW) in Langenau, Germany, is active in the analysis of drinking water as well as in the monitoring of ground and waste water from the water protection area Donauried-Hürbe and of surface water from the surrounding area. HPTLC, preferably with automated multiple development (AMD), and online hyphenation of HPTLC-MS are part of the methods applied in routine analysis [1–3].

IntroductionWithin the scope of a monitoring program of raw water resources used by LW, comprehensive chemical, physico-chemical and microbiological analyses are performed regularly. In addition non-target screening analyses for the detection of not yet considered contaminants or unknown substances were performed.

In one of the HPTLC/AMD screening tests of ex-tracts from secondary effluents and of surface and ground water samples the resulting chroma-tograms showed a zone which could not be identi-fied as any of the substances known from target analysis at LW.

Sample preparationAnalyte enrichment from a 100 mL water sample was done by solid phase extraction (SPE) using 0.2 g of Iso-lute ENV+ sorbent at pH 3 or 7. The SPE sorbent was conditioned consecutively with 6 mL each of n-hexane, acetone, methanol and water (pH = 3 or 7). After drying 6 mL of methanol were used for elution and after eva-

poration to dryness the residue was taken up in 200 µL of methanol.

LayerHPTLC plates Lichrospher F254, 20 x 10 cm (Merck) were pre-cleaned with 2-propanol and dried for 30 min at 120 °C on the TLC Plate Heater.

Sample applicationWith Automatic TLC Sampler (ATS4) as area of 6 x 3 mm

ChromatographyIn the AMD 2 system with a 25-step gradi-ent starting in isocratic mode with 5 steps acetonitrile – dichloromethane 1:1 for focusing, followed by 15 steps from acetonitrile – dichlo-romethane 1:1 to dichloromethane and then in 5 steps from dichloromethane – n-hexane 4:1 to n-hexane. The final migration distance was 80 mm.

Densitometric evaluationMulti-wavelength scan at 190, 200, 220, 240, 260, 280 and 300 nm with the TLC Scanner and winCATS software

DocumentationUnder UV 254 nm with the TLC Visualizer

Results and discussionDuring routine screening of extracts from secondary effluents as well as of surface and ground water samples a high peak was ob-served in the chromatograms. To further inves-tigate this peak the unknown zone was eluted from the HPTLC plate by means of the TLC-MS Interface and analyzed by Nano LC followed by QTOF-MS (ESI+). The analysis revealed that the zone consisted of two substances, peak A at RT = 3.2 min and peak B at RT = 3.4 min.

Dear friends

This CBS issue has been delayed a bit, but in my de-fense, I would like to men-tion that during the hot fi-nal phase of the September issue, I was co-organizing the 39th German Food Congress. It was held in Stuttgart-Hohenheim this year and attended by over 600 participants. I think the congress was quite fruitful for the progress of HPTLC in food analysis, especially due to a workshop for the Young Food Chemists.

It was noted that many international compa-nies reported an increase in the need for more food analyses, for which HPTLC offers excel-lent preconditions. There is great pent-up de-mand in countries like China, India, Thailand, and other countries where food safety is more and more forced by law.

Due to the increased demand for food analysis, three articles in this CBS relate to this field. By the way the study of food chemistry is a Ger-man unicum – there is no comparable study in other countries.

Please keep in mind that preparations for the HPTLC Symposium in Basel, 6–8. July 2011 proceed. Information (Call for Papers) can be found on the last yellow page. Do we meet in Basel? I would enjoy it!

Sincerely,

Gerda Morlock [email protected]

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CAMAG LITERATURDIENSTCAMAG BIBLIOGRAPHY SERVICEPLANAR CHROMATOGRAPHY

Liebe Freunde

Dieser CBS erscheint leider mit Verspätung. In der Zeit, in der die Bearbeitung der September-Ausgabe in das Endstadium rückt, war ich als Mitorganisator stark eingebunden in die Orga-nisation des 39. Deutschen Lebensmittelche-mikertages in Stuttgart-Hohenheim. Dieser er-wies sich für die Verbreitung der HPTLC in der Lebensmittelanalytik als erfreulich ergiebig, vor allem im Workshop der jungen Lebensmittel-chemiker.

Erfreulich ist, dass viele international tätige Un-ternehmen einen stark ansteigenden Bedarf an Lebensmittelanalytik haben, für die die HPTLC vorzügliche Voraussetzungen bietet. Grossen Nachholbedarf auf diesem Gebiet haben Län-der wie China, Indien oder Thailand, in denen Lebensmittelsicherheit verstärkt gesetzlich ge-fordert wird.

Wegen der wachsenden Bedeutung der Le-bensmittelanalytik stammen drei Anwendungs-beiträge dieses CBS aus diesem Bereich im wei-teren Sinne. Übrigens ist der Studiengang Le-bensmittelchemie einzigartig in Deutschland - international gibt es nichts Vergleichbares.

Die Vorbereitungen zum HPTLC Symposium in Basel, 6.–8. Juli 2011, schreiten zügig voran. Informationen (Call for Papers) finden Sie auf der letzten gelben Seite. Sehen wir uns in Basel? Ich würde mich freuen!

Herzlichst

Gerda Morlock [email protected]

SEPTEMBER

2010

THE CBS CLASSIFICATION SYSTEM1. Reviews and books

a) Books on TLC b) Books containing one or several chapters on TLC c) Books containing frequent TLC information spread over several chapters of other information

2. Fundamentals, theory and general a) General b) Thermodynamics and theoretical relationship c) Relationship between structure and chrom. behaviour d) Measurement of physico-chemical and related values e) Optimization of solvent systems f) Validation of methods

3. General techniques (unless they are restricted to the application within one or two classification sections) a) New apparatus/techniques for sample preparation b) Separation material c) New apparatus for sample application/dosage d) New apparatus/techniques for chromatogram development e) New apparatus/techniques for pre- or post- chromatographic derivatization f) New apparatus/techniques for quantitative evaluation g) New apparatus/techniques for other TLC steps (distinguished from section 4)

4. Special techniques a) Automation of sample preparation/application b) Automation of complex chromatogram developing techniques c) Automation, computer application in quantitative chromatogram evaluation d) Combination of TLC with other chromatographic techniques e) Combination of TLC with other (non-chromatographic) techniques...MS, IR...etc.

5. Hydrocarbons and halogen derivatives a) Aliphatic hydrocarbons b) Cyclic hydrocarbons c) Halogen derivatives d) Complex hydrocarbon mixtures

6. Alcohols

7. Phenols

8. Substances containing heterocyclic oxygen a) Flavonoids b) Other compounds with heterocyclic oxygen

9. Oxo compounds, ethers and epoxides

10. Carbohydrates a) Mono- and oligosaccharides, structural studies b) Polysaccharides, mucopolysaccharides, lipopolysaccharides

11. Organic acids and lipids a) Organic acids and simple esters b) Prostaglandins c) Lipids and their constituents d) Lipoproteins and their constituents e) Glycosphingolipids (gangliosides, sulfatides, neutral glycosphingolipids)

12. Organic peroxides

13. Steroids a) Pregnane and androstane derivatives b) Estrogens c) Sterols d) Bile acids and alcohols e) Ecdysones and other insect steroid hormones

14. Steroid glycosides, saponins and other terpenoid glycosides

15. Terpenes and other volatile plant ingredients a) Terpenes b) Essential oils

16. Nitro and nitroso compounds

17. Amines, amides and related nitrogen compounds a) Amines and polyamines b) Catecholamines and their metabolites c) Amino derivatives and amides (excluding peptides)

18. Amino acids and peptides, chemical structure of proteins a) Amino acids and their derivatives b) Peptides and peptidic proteinous hormones

19. Proteins

20. Enzymes

21. Purines, pyrimidines, nucleic acids and their constituents a) Purines, pyrimidines, nucleosides, nucleotides b) Nucleic acids, RNA, DNA

22. Alkaloids

23. Other substances containing heterocyclic nitrogen a) Porphyrins and other pyrroles b) Bile pigments c) Indole derivatives d) Pyridine derivatives e) other N-heterocyclic compounds

24. Organic sulfur compounds

25. Organic phosphorus compounds (other than phospholipids)

26. Organometallic and related compounds a) Organometallic compounds b) Boranes, silanes and related non-metallic compounds c) Coordination compounds

27. Vitamins and various growth regulators (non-peptidic)

28. Antibiotics, Mycotoxins a) Antibiotics b) Aflatoxins and other mycotoxins

29. Pesticides and other agrochemicals a) Chlorinated insecticides b) Phosphorus insecticides c) Carbamates d) Herbicides e) Fungicides f) Other types of pesticides and various agrochemicals

30. Synthetic and natural dyes a) Synthetic dyes b) Chloroplasts and other natural pigments

31. Plastics and their intermediates

32. Pharmaceutical and biomedical applications a) Synthetic drugs b) Pharmacokinetic studies c) Drug monitoring d) Toxicological applications e) Plant extracts, herbal and traditional medicines f) Clinico-chemical applications and profiling body fluids

33. Inorganic substances a) Cations b) Anions

34. Radioactive and other isotopic compounds

35. Other technical products and complex mixtures a) Surfactants b) Antioxidants and preservatives c) Various specific technical products d) Complex mixtures and non-identified compounds

36. Thin-layer electrophoresis

37. Environmental analysis a) General papers b) Air pollution c) Water pollution d) Soil pollution

38. Chiral separations

XX. (abstract number underlined) refers to HPTLC related publication or application using HPTLC materials

CAMAGBIBLIOGRAPHYSERVICE No.105�

1. Reviews and books

105001 P.K.JAISWAL(CentralAgmarkLaboratory,Govt.ofIndia,NorthAmbazariRoad,Nagpur440010, India):High-performance thin-layerchromatography in foodanalysis.CBSPublishers&DistributorsPvtLtd,NewDehli,2010.Shortreviewonplanarchromatographyinfoodanalysis.Certainwell-knownapplicationsarementionedbutimportantpublicationsandrecentscientificdataislacking.

foodanalysis,HPTLC 1a

105002 MonikaJANICKA*,A.WASIK,J.NAMIESNIK(*GdanskUniversityofTechnology,ChemicalFaculty,DepartmentofAnalyticalChemistry,80-22�Gdansk,Poland,[email protected]):Analytical procedures for determination of cocaine and its metabolites in biological samples.TrAC29,209-224(2010).Thedangerouseffectsofcocaineonlivingorganismsandcurrentpro-blemsassociatedwithitswideuseandavailabilityhaveledtothedevelopmentofvariousana-lyticalprocedures.Thisreviewdiscussesanalyticalmethodsproposedduringthepasttenyearsfor theverificationof cocaineand itsmetabolites inbiological samples.Challenges regardingsamplepreparationandextractiontechniquesaredescribed.Differentapproachesusingthin-lay-erchromatographyarediscussed,andespeciallythepossibilityofsimultaneousdeterminationofparent,metaboliteandinterferingdrugsinurinesamples,aswellastheidentificationofmarkersforcombinedconsumptionofcocaineandalcohol.

toxicology,comparisonofmethods,review 1,22

10500� A.ZEB*,M.MURKOVIC(*Institute forBiochemistry,GrazUniversityofTechnology,Graz,Austria;[email protected]):Thin-LayerChromatographicanalysisofcarotenoidsinplantand animal samples. J.PlanarChromatogr. 2�, 94-10� (2010)This reviewdescribes availabledataonanalysisofcarotenoidsbyTLC.Petroleumether,acetone,andhexanearethemajormo-bilephasesusedforTLC.Thistechniquewasfoundtohavethepotentialtobethefirstchoiceforanalysisofcarotenoidsinbiologicalsamples.Theusesofother,orthogonalchromatographicmethods,forexampleHPLC,MS,scanningdensitometry,andimageanalysiswithTLCcanen-ablepreciseanalysisofcarotenoids.Thereviewconsistsofthefollowingparts:1.Introduction;1.1Functionofcarotenoids;1.2Occurrenceofcarotenoids;2.Analysisofcarotenoids;2.1Sam-pling;2.2Samplepreparation;2.�Extractionofcarotenoids;2.4Saponification;2.5Chromato-graphicanalysis;�.Thin-layerchromatographicanalysisofcarotenoids;�.1TLCofcarotenoidsfrommicrobialandanimalsources;�.2TLCofcarotenoidsfromplantsources;�.�Normal-pha-seTLCanalysisofcarotenoids;�.4Reversed-phaseTLCanalysisofcarotenoids;�.5TLCana-lysisofcarotenoidswithscanningdensitometry;4.AdvantagesofTLCincarotenoidanalysis;5.Conclusionandfuturestudies.1�4References.

foodanalysis,review 1,�0b

2. Fundamentals, theory and general

105004 Rodica Domnica BRICIU*, Agata KOT-WASIK, A. WASIK, J. NAMIESNIK, C. SARBU(*Babes-BolyaiUniversity,FacultyofChemistryandChemicalEngineering,AranyJanosStr.,No11,400028ClujNapoca,Romania):Thelipophilicityofartificialandnaturalsweetenersesti-matedbyreversed-phasethin-layerchromatographyandcomputedbyvariousmethods.J.Chro-matogr.A1217(2�),�702-�706(2010).Evaluationof thechromatographicbehaviorof someartificial and natural sweeteners by HPTLC on RP18, RP18W, RP8, cyano and amino phaseswithmixturesofacetonitrile-waterindifferentvolumeproportions.ThelipophilicityisgiventhroughchromatographicdescriptorssuchasRM0,meanofRM(mRM),andscoresofRMva-luescorrespondingtothefirstprincipalcomponent(PC1/RM).Inaddition,scoresandloadingsresultingfromcovariancematrixofretentiondataprovidenewinformationaboutsimilarityanddifferencesofinvestigatedcompoundsandbetweenthestationaryphaseandthemobilephases.Theexperimentallipophilicityindicesestimatedfromretentiondatawerecorrelatedwithcom-

CAMAGBIBLIOGRAPHYSERVICE No.1054

putedvalues,viacomputersoftwareandinternetmodule.Resultswereinaccordanceatahighlysignificantstatisticallevel.

qualitycontrolfoodanalysis,HPTLC 2c

105005 K. FERENCZI-FODOR, B. RENGER*, Z. VÉGH (*Vetter Pharma-Fertigung GmbH & Co.KG,Schuetzenstrasse87,88212Ravensburg,Germany;[email protected]):Thefrustratedreviewer-recurrantfailuresinmanuscriptsdescribingvalidationofquantitativeTLC/HPTLCproceduresforanalysisofpharmaceuticals.J.PlanarChromatogr.2�,17�-179(2010).Manymanuscriptsandalreadypublishedarticlesonanalyticalprocedurestobeusedinpharma-ceuticalqualitycontrolarecharacterizedbyseveraltypicalmethodologicalfailuresandmiscon-ceptions.Theautorspresentacollectionoftypicalfailures,misconceptions,andmisleadingdatafromarticlespublishedoverthelasttwoyearsinsevenwell-knownchromatographicpublicationsandprovideatthesametimealistofreferencesdescribingoptimumapproachestovalidationofspecificTLC/HPTLCprocedures.Inparticular,methodspecificity,linearity,accuracy,andpreci-sionveryoftenarenotdeterminedproperlyandinaccordancewithbestpractise.

qualitycontrol,HPTLC,quantitativeanalysis,validationofmethods 2f

105006 T.HANAI(HealthResearchFoundation,InstitutPasteur5F,Sakyo-ku,Kyoto606-8225,Japan;[email protected]):Quantitative insilicoanalysisof retention innormalphase liquidchro-matography.J.Liq.Chromatogr.Relat.Technol.��,297-�04(2010).Retentioninnormalphaseliquidchromatographicwasquantitativelyanalyzedinsilicousingassamplessleepingmedicinesinacidic,basic,andneutralorganicsolventmixtures.Hydrogenbondingisthemajorcontributionintheretentionthatwassupportedbyahighcorrelationcoefficientbetweenlogkandhydrogenbondingenergyvaluescalculatedusingamolecuarmechanicsprogram.TLConsilicagelwithchloroform-acetone9:1,benzene-aceticacid9:1anddioxane-benzene-aqueousammoniumhydroxide20:75:4.

2c

3. General techniques

105007 V.BEREZKIN*,SvetlanaKHREBTOVA,NataliaKULAKOVA(*Topchiev InstituteofPetro-chemicalSynthesis,RussianAcademyofSciences,Leninskypr.29,Moscow,119991,Russia):Four-dimensionalTLC on plates with open and closed adsorbent layers. Chromatographia 71(9-10),907-911(2010).Descriptionoffour-stageTLC,anewversionofmultidimensional(mul-ti-stage)planarchromatography.Inthefirststageamulticomponentmixtureisfractionatedintothreegroupsofchromatographiczones(fractions)byTLCwheretheadsorbentisdepositedonanaluminumfoil.Inthesecondstage,theTLCplateisdriedandcutbyscissorsintothreenar-rowstripscontainingtheseparatedfractions.Inthenextstagestheisolatedfractionsoneachofthese strips („daughter“ plates) are separated into individual components with an appropriatemobilephaseandbyusinga solventflowperpendicular to theflowof themobilephase.Thepracticalapplicationofthemethodisshownusingasanexampletheseparationofamixtureofdyes.Themethodcanbeexpandedforseparationofmixturescontainingfourormorefractions.Thisfour-dimensionalversionofmultidimensionalTLCwascarriedoutonplateswithbothopen(conventional)andclosedadsorbentlayers.

�d

105008 J.E.CLARK*,SusanOLESIK(*TheOhioStateUniversity,DepartmentofChemistry,120West18thAve,Columbus,OH4�210,USA):Electrospunglassycarbonultra-thinlayerchromatogra-phydevices. J.Chromatogr.A1217 (2�), 4655-4662 (2010).Development and applicationofelectrospunglassycarbonnanofibers forultra-thin layerchromatography (UTLC).ThecarbonnanofiberstationaryphasewascreatedthroughelectrospinningandpyrolysisofSU-82100pho-toresist,whichresultedinglassycarbonnanofiberswithdiametersof200-�50nmthatforma


matstructurewithathicknessof15µm.ThechromatographicpropertiesofUTLCdevicespro-ducedfrompyrolyzedSU-8heatedtotemperaturesof600,800,and1000°Cwereinvestigated.ByuseofRaman spectroscopy and scanning electronmicroscopy thephysical andmolecularstructureofthenanofibersateachtemperaturewasdetermined.ThecarbonUTLCdevicesweresuitablefortheanalysisvariousdyemixturesandalsoallowedseparationofthreeFITC-labeledessentialaminoacids (lysine, threonine,phenylalanine).TheelectrospunglassycarbonUTLCplatesshowedgoodretentionproperties,platenumbervaluesabove10000,andphysicalandche-micalrobustnessforarangeofmobilephases.

doping,HPTLC,qualitativeidentification,quantitativeanalysis �b

105009 P.PLOCHARZ*,AnnaKLIMEK-TUREK,T.H.DZIDO(*DepartmentofPhysicalChemistry,Medical University of Lublin, Staszica 6, 20-081 Lublin, Poland): Pressurized planar electro-chromatography, high-performance thin-layer chromatography and high-performance liquidchromatography-Comparisonofperformance.J.Chromatogr.A1217(2�),4868-4872(2010).Comparisonofthekineticperformance,measuredbyplateheight,ofhigh-performancethin-lay-erchromatography(HPTLC),high-performanceliquidchromatography(HPLC)andpressurizedplanarelectrochromatography(PPEC).HPTLConRP18Wwithmobilephasescomposedoface-tonitrile-buffer.TheHPLCcolumnwaspackedwiththesameadsorbent,whichwasscrappedfromanRP18WHPTLCplate.AnadditionalHPLCcolumnwaspackedwithC18-typesilicaba-sed(LiChrosorbRP18)adsorbentof5µmparticlediameter.TheplateheightofbothHPLCandPPECsystemsdependsontheflowvelocityandthemigrationdistanceofthemobilephase.Astestsolutionprednisolonesuccinatewasused.ThebestperformancewasobtainedbythePPECsystem.Theseparationefficiencyofthesystemswasinvestigatedandconfirmedbyuseofatestcomponentmixturecomposedofsixhormones.

qualitycontrol,HPTLC,comparisonofmethods,pressurizedplanarelectrochromatography �

4. Special techniques

105010 P. HOFFMANN, M. HULSEWIG, S. DUVAR, H. ZIEHR, M. MORMANN, J. PETER, A.FRIEDRICH,H.KARCH,J.MUTHING*(*InstituteofHygieneandInterdisciplinaryCenterforClinicalResearch,UniversityofMunster,Munster,Germany,[email protected]):OnthestructuraldiversityofShigatoxinglycosphingolipidreceptorsinlymphoidandmyeloidcellsde-terminedbynanoelectrosprayionizationtandemmassspectrometry.RapidCommun.MassSpec-trom.24,2295-2�04(2010).HPTLCofglycosphingolipids(GSLs)onsilicagelwithchloroform-methanol-water120:70:17.TheplatewasoverlaidwithShigatoxin(Stx),andthemicrobesweredetectedwithprimaryanti-Stxandappropriatealkalinephosphataselabeledsecondaryantibo-dies.Boundantibodieswerevisualizedbycolordevelopmentusing0.05%5-bromo-4-chloro-�-indolylphosphatep-toluidinesalt inglycinebuffer.TheGSLswereextractedfromtheplateand analyzed by electrospray ionization mass spectrometry (ESI-MS). Using the combinationofaTLCoverlayassayandnanoESI-QTOF-MS,thestructuralcharacterizationofthefunctionalStx1receptorsofRajiandTHP-1cellsisreported.

pharmaceuticalresearch,HPTLC 4e

105011 A. MUELLER, S. WEISS, W. SCHULZ*, W. SEITZ, R. ALBERT, W. RUCK, W. WEBER(*Zweckverband Landeswasserversorgung, Betriebs- und Forschungslaboratorium, Am Spit-zigen Berg 1, 89129 Langenau, Germany, [email protected]): Combination of differentliquidchromatography/massspectrometry technologies for the identificationof transformationproductsofrhodamineBingroundwater.RapidCommun.MassSpectrom.24,659-666(2010).HPTLCof rhodamineBandfivede-ethylated transformationproducts (N,N,N‘-tryethylrhoda-mine (1), N,N‘-dyethylrhodamine (2), N,N-dyethylrhodamine (�), N-ethylrhodamine (4), andrhodamine(5))ingroundwateronsilicagelbyautomatedmultipledevelopmentwitha2�-stepgradientbasedonmethanol(withtheadditionofformicacid)anddichloromethane.Thedrying


timeaftereachstepwas2min.Fordetectionbybioluminescencetheplatewasdippedintoasus-pensionofVibriofischerifor2sataspeedof�cm/s.ThehRfwere72,66,60,5�,48,and�6forcompounds(1)-(5).Combinationofdifferentseparationanddetectiontechniquesenabledafastandeffectivescreeningofthegroundwatersample.

environmental,HPTLC,qualitativeidentification,postchromatographicderivatization,AMD 4e

105012 A.MUSKEN,J.SOUADY,K.DREISEWERD,W.ZHANG,U.DISTLER,J.PETER,H.MIL-LER,H.KARCH,J.MUTHING*(*InstituteofHygieneandInterdisciplinaryCenterforClini-calResearch,UniversityofMunster,Munster,Germany, [email protected]):Applicationofthin-layerchromatography/infraredmatrix-assistedlaserdesorption/ionizationorthogonaltime-of-flightmassspectrometrytostructuralanalysisofbacteria-bindingglycosphingolipidsselectedbyaffinitydetection.RapidCommun.MassSpectrom.24,10�2-10�8(2010).HPTLCofglycos-phingolipids(GSLs)onsilicagelwithchloroform-methanol-water120:70:17.TheplatewasoverlaidwithGSL-specificbacteria,andthemicrobesweredetectedwithprimaryantibodiesandappropriate alkaline phosphatase labeled secondary antibodies, and by in situ MS analysis ofbacteria-specificGSLreceptors.Thethin-layerchromatographyinfraredmatrix-assistedlaserde-sorption/ionization orthogonal time-of-flight mass spectrometry (TLC/IR-MALDI-o-TOF-MS)methodrepresentsoneof themostpowerfulapproachesfor thedetectionofGSLreceptorsofmicroorganisms.

pharmaceuticalresearch,HPTLC 4e

10501� K.NIMPTSCH,R.SUESS,T.RIEMERA,A.NIMPTSCH,M.SCHNABELRAUCH,J.SCHIL-LER(*UniversityofLeipzig,MedicalFaculty,InstituteofMedicalPhysicsandBiophysics,Här-telstr.16-18,04107Leipzig,Germany):Differentlycomplexoligosaccharidescanbeeasilyiden-tifiedbymatrix-assistedlaserdesorptionandionizationtime-of-flightmassspectrometrydirectlyfromastandardthin-layerchromatographyplate.J.Chromatogr.A1217(2�),�711-�715(2010).Oligosaccharides(derivedfromdextran,alginate,hyaluronanandchondroitinsulfate)werecha-racterizedbymatrix-assistedlaserdesorptionandionizationtime-of-flight(MALDI-TOF)massspectrometry (MS) directly on a normal phaseTLC plate.The applied oligosaccharides wereeithercommerciallyavailableorobtainedfromthepolysaccharidesbyHCl-inducedhydrolysis.TLCwasfollowedbyMALDI-TOFMSsubsequenttomatrixdeposition.Thehighqualitymassspectraobtainedallowforunequivocalassignments.Thehighcontentofformicacidinthesol-ventdoesnotcausemajorproblemsbutisresponsibleforthepartialformylationoftheanalyteandaminorN-acetyllossfromhyaluronanandchondroitinsulfate.

qualitativeidentification,HPTLC,oligosaccharides 4e

105049 W.SCHWACKetal.,seesection�0

6. Alcohols

105014 AnnaNIESTROJ(SilesianUniversity,InstituteofChemistry,9SzkolnaStreet,40-006Katowice,Poland;[email protected]):Comparisonofmethodsforcalculationofthepartitioncoefficientsofselectedaliphaticcompounds.J.PlanarChromatogr.2�,198-200(2010).PropositionofnewmethodsforcalculationofthepartitioncoefficientsofaliphaticcompoundsfromexperimentalRfvaluesandthenumericalvaluesofselectedtopologicalindexes.Theexperimentalpartitioncoefficient(logPexp)ofcetylalcoholwasdeterminedforthen-octanol-watersystem.Numericalvaluesobtainedwerecomparedwiththeoreticalvaluesfromadatabase(AlogPs,AC_logP,AB/LogP,ALOGP,milogP,andXLOGP2).HPTLCofcetylalcohol,stearylalcohol,palmiticacid,stearicacid,alpha-hydroxypalmiticacid,and12-hydroxystearicacidonRP18withmethanolandwithmethanol-water19:1inahorizontalchamberatroomtemperature.Detectionaftervisuali-zationiniodinevapor.


comparisonofmethods,qualitativeidentification 6,11a

7. Phenols

105015 T. HOFMANN*,T. RÉTFALVI, L.ALBERT, P. NIEMZ (*University of West Hungary, De-partment for Chemistry,Ady Endre u. 5, 9400 Sopron, Hungary; [email protected]):High-performancethin-layerchromatographicassessmentofthermallymodifiedwood.J.PlanarChromatogr.2�,227-229(2010).HPTLCofphenoliccompounds(syringicacid,vanillicacid,pyrocatechin, thymol,sinapicacid,2,6-dimethoxyphenol,resorcin,guaiacol)onsilicagelwithdiisopropylether-formicacid9:1inanunsaturatedtwintroughchamber.OPLCofsugars(suc-rose,galactose,glucose,mannose,fructose,arabinose,xylose,ribose,rhamnose,stachyose,raf-finose,maltose)onsilicagelwithacetonitrile-water17:�.DetectionofphenoliccompoundsbysprayingwithFolin-Ciacalteaureagentandofsugarsbysprayingwithaniline-diphenylaminereagent.

agricultural,HPTLC,qualitativeidentification 7

105016 SayyadaKHATOON*,H.SINGH,K.SINGH,A.K.GOEL(*PharmacognosyandEthnophar-macologyDivision,CouncilforScientificandIndustrialResearch,NationalBotanicalResearchInstitute, Rana Pratp Marg, Lucknow-226001, India; [email protected]):TLC evaluationandquantificationofphenoliccompoundsindifferentpartsofDendrophthoefalcata(Linn.f.)Etting.J.PlanarChromatogr.2�,104-107(2010).TLCof(+)-catechin,ellagicacid,quercetin,and ferulic acid on silica gel with toluene - ethyl acetate - fomic acid 6:4:1 in a twin-troughchamberpreviouslysaturatedfor�0minat25°C.Othermobilephasecompositionswereethylacetate-methanol-water10:1:1,n-butanol-aceticacid-water4:1:5(upperlayer),n-butanol-ethanol-water20:5:11,n-butanol-aceticacid-water6:2:1,toluene-ethylacetate-formicacid5:5:1 and7:�:1, and toluene - ethyl acetate -methanol - formic acid140:60:1:1.Quantitativedeterminationbyabsorbancemeasurementat�20nm.Detectionbydippinginanisaldehydere-agent,followedbydryingandheatingat110°Cfor5min.Characteristicbandsof(+)-catechin,ellagicacid,quercetin,andferulicacidwereobservedathRf �5,41,6�and66, respectively.Precision(CV,n=7)was0.�9,0.44,0.55and0.16%andrepeatability(CV,n=7)0.65,0.95,0.�7and0.18%,respectively.LODwas54,�40,48and78ng/band,andLOQ4.1,6.5,1.6and1.5µg/band,respectively.Linearregressionwas0.999�(100-500ng/band),0.988�(1000-5000ng/band),0.9989(100-500ng/band)and0.9987(100-500ng/band),respectively.

Noteoftheeditor:ThereportedLOQareunusallyhighcomparedtotheLOD.ThereportedCV(standarddeviationdividedbymean)alsoarisesquestions.

herbal,traditionalmedicine,densitometry 7

105017 M.M.PANDEY,S.RASTOGI,A.K.S.RAWAT* (*PharmacognosyandEthnopharmacologyDivision,NationalBotanicalResearchInstitute,Lucknow-226001,India;[email protected]): Optimization of an HPTLC method for separation and identification of phenolic com-pounds.J.PlanarChromatogr.2�,108-111(2010).HPTLCofgallicacid,ferulicacid,syringicacid,catechin,protocatechuicacidandvanillinonsilicagelwithtoluene-ethylacetate-formicacid8:2:1inatwin-troughchamberpreviouslysaturatedfor15min.Quantitativedeterminationby absorbance measurement at 280 nm.Accuracy was between 96.� and 90.7 %, repeatabili-tybetween0.65and0.9�%,inter-dayprecisionbetween0.80and0.90%,intra-dayprecisionbetween0.72and0.95%,andprecisionbetween0.87and0.92%.LODandLOQwereabout100and400ng/band, respectively.StartingatLOQ, thecorrelationcoefficientswerebetween0.988and0.997.

herbal,traditionalmedicine,HPTLC 7

8. Substances containing heterocyclic oxygen

105018 V.GLAVNIK,B,SIMONOVSKA,IrenaVOVK*(*NationalInstituteofChemistry,Laboratory


forFoodChemistry,Hajdrihova19,SI-1001Ljubljana,Slovenia;[email protected]):ComparisonofTLCandHPLCmethodsusedforanalysisof(-)-epicatechinanditsdimerprocyanidinB2inchocolate. J.PlanarChromatogr.2�,2�0-2�2 (2010).HPTLCof (+)-catechin, (-)-epicatechin,(-)-epigallocatechin,(-)-epigallocatechingallate,(-)-epicatechingallate,procyanidinB2,procya-nidinA2,andmethylxanthines(theobromineandcaffein)oncellulosewithn-propanol-water-aceticacid20:80:1 inahorizontalchamber.Detectionbydipping for1s into4-dimethylami-nocinnamaldehydedetectionreagent.Quantitativedeterminationbyabsorbancemeasurementat655nm.BydensitometryLODfor(-)-epicatechinandprocyanidinB2was0.2and2ng/zone,respectively;LOQwas0.4ngand4ng/zone,respectively.Theselimitswerelowerbyafactor50for(-)-epicatechinandbyafactorof10forprocyanidinB2thanthoseobtainedbyHPLC.TheTLCmethodgaveamoreaccurateresultforthe(-)-epicatechincontentofbakingchocolatethantheHPLCmethodwhichwasalsomoretime-consuming.

foodanalysis,comparisonofmethods,HPTLC,densitometry,quantitativeanalysis 8a

105019 J.SUN(SunJia),Y.YUE*(YueYongde),F.TANG(TangFeng),X.GUO(GuoXuefeng)(*In-ternationalCentreforBambooandRattan,No.8FutongDongdajie),Wangjing,ChaoyangDis-trict,Beijing100102,Cina;[email protected]):SimultaneousHPTLCanalysisofflavonoidsintheleavesofthreedifferentspeciesofbamboo.J.PlanarChromatogr.2�,40-45(2010).HPTLCof flavonoids (vitexin, isovitexin, orientin, isoorientin, rutin) on polyamide at 2� +/- 2°C and40%relativehumiditywiththethree-componentmobilephaseA-B-C��:67:8,whereAisdo-decylsulfate-n-butanol-n-heptane147:158:28,Biswater,andCisformicacid.Thesolventmentionedgavethebestresolutionofvitexin(hRf61),isovitexin(hRf21),orientin(hRf28),isoorientin(hRf�4),andrutin(hRf52).Detectionbysprayingwith1%aluminiumtrichlorideinethanolfollowedbywaitingforapproximately1h.Quantitativedeterminationbyfluorescencemeasurementat�66nm.Precisionwasfoundtobe0.98,0.91,1.02,1.04and0.87%forisovite-xin, rutin,orientin, isoorientin,andvitexin, respectively.Average recoveries (at threedifferentconcentrations)werebetween98.9and100.6%fromP.pubescens,P.glaucaandP.yixingensis.

HPTLC,densitometry,quantitativeanalysis,qualitativeidentification 8a

9. Oxo compounds, ethers and epoxides

105020 P.DEEPIKA,K.N.SABHARWAL,N.SIVARAMAN,T.G.SRINIVASAN*,P.R.VASUDEVARAO(*FuelChemistryDivision,ChemistryGroup,IndiraGandhiCentreforAtomicResearch,Kalpakkam,TamilNadu60�102,India;[email protected]):Developmentofachromatographicprocedure for thepurification of 1,2-diketone. J.Liq.Chromatogr.Relat.Technol. ��, 97-108(2010).TLCofoctane-4,5-dioneonsilicagelwithhexane,dichloromethane,andhexane-di-chloromethane1:1.Detectionbyplacingtheplateinaiodinechamber.

qualitativeidentification 9

10. Carbohydrates

105021 J.GEISSER*,EvamariaKRATZ(*ChemicalandVeterinaryInvestigationLaboratory(CVUA),WeissenburgerStr.�,76187Karlsruhe,Germany,[email protected]):Determina-tionofaloeveragelincosmetics.CBS104,1�-15(2010).HPTLCofaloeverose,glucoseandgalactoseinaloeveraproductsonsilicagel(impregnatedwithNaH2PO4)withacetone- iso-propanol-0.1Mformicacid2:2:1(doubledevelopmentforproductswithhighglucosecontent).Detectionbyimmersionin4-aminobenzoicacidreagent(1g4-aminobenzoicacidin�6mLace-ticacid,with40mLwater,2mL85%phosphoricacidand120mLacetone),followedbyhea-tingat100°Cfor10min.Densitometricevaluationbyfluorescencemeasurementat�66nm.Thelimitofquantificationwasapprox.�%inaloeveraproducts.RSDforpolynomialcalibrationis2.1%formannoseintherangeof8-80ng/bandand4.0%usingmatrixcalibration.

herbal,HPTLC 10b


105022 P.MANDAL,A.MISRA*(*DivisionofMolecularMedicine,BoseInstitute,A.J.C.BoseBirthCentenaryCampus,Kolkata,India,[email protected]):Concisesynthesisofthepentasac-charideO-antigencorresponding to theShiga toxinproducingEscherichiacoliO171.Bioorg.Chem.�8,56-61(2010).TLCof4-methoxyphenylglycosideonsilicagelwithacetonitrile-me-thanol-water4:2:1.Detectionbysprayingwithwarm2%cericsulphatein2Nsulfuricacid.ThehRfof4-methoxyphenylglycosidewas�0.

pharmaceuticalresearch,qualitativeidentification 10b

10502� K.SONG,J.SHIM,J.PARK,S.KIM,Y.KIM,W.BOOS,K.PARK*(*DepartmentofBiology,UniversityofIncheon,Incheon,RepublicofKorea,[email protected]):Transglycosylationpropertiesofmaltodextringlucosidase(MaIZ)fromEscherichiacolianditsapplicationforsyn-thesisofanigerose-containingoligosaccharide.Biochem.Biophys.Res.Commun.�97,87-92(2010).PreparativeTLCofthehydrolysisreactionofmaltodextringlycosidaseonvarioussubs-trates(maltotriose,alpha-,beta-,gamma-cyclodextrinsandcycloamylose)onsilicagelwithethylacetate-methanol-aceticacid-water12:�:�:1.ThestructureoftheproductswasdeterminedbyMALDI-TOF/MS,1�CNMR,andenzymaticanalysis.

pharmaceuticalresearch,preparativeTLC 10b

105024 C.YANG(YangCheng),J.GUAN(GuanJia),J.-S.ZHANG(ZhangJiang-sheng),S.-P.LI*(LiShao-ping)(*InstituteofChineseMedicalSciences,UniversityofMacau,MacauSAR,China;[email protected]):UseofHPTLCtodifferentiateamongthecrudepolysaccharidesinsixtraditionalchinesemedicines.J.PlanarChromatogr.2�,46-49(2010).HPTLCofpolysac-charides (with galactose, glucose, mannose, arabinose, ribose, xylose, rhamnose, galacturonicacid,andglucuronicacidasstandards)beforeandafterhydrolysisonsilicagelwithchloroform-n-butanol - methanol - water - acetic acid 9:25:10:�:� with chamber saturation for �0 min atroomtemperature.Detectionbysprayingwithaniline-diphenylamine-phosphoricacidreagentandheatingat1�0°Cfor10min.Quantitativedeterminationbyabsorbancemeasurementat�80nm.Ninhydrinreagentwasusedfordetectionofothercompounds.

pharmaceuticalresearch,herbal,traditionalmedicine,HPTLC,densitometry 10b

11. Organic acids and lipids

105025 P.KUSHWALI*,SheejaEDWIN,K.VARSHNEY,E.JARALD,S.AHMAD,A.DAUA(*TI-FACOREinGreenPharma,B.R.NahataCollegeofPharma,Mhow-NeemuchRd.,Mandsaur(M.P.),India):Estimationofcurcuminand�-acetyl-11-keto-a-boswellicacidinamarketedher-balproduct rheumaxusingHPTLC. InternationalSeminaronHerbalDrugResearch,PN-028(2009).HPTLCofcurcuminand�-acetyl-11-keto-a-boswellicacidintheherbalproductRheu-max (containsCurcuma longa,Boswellia serrata,Tinospora cordifolia andVitexnegundo)onsilicagelwithchloroform-methanol�7:�forcurcuminandn-hexane-ethylacetate1:1fortheacid.Quantitativedeterminationbyabsorbancemeasurementat4�0nmforcurcuminand254nmfortheacid.Themethodwaslinearintherangeof100-500ng/bandforcurcuminand1500-4000ng/bandfortheacid.

traditionalmedicine,quantitativeanalysis,HPTLC 11a

105014 AnnaNIESTROJ,seesection6

105026 K.RIZWANBASHA*,M.SHANMUKHA,K.RAMRAO,N.MUNJUNATHA,V.SENTHIL,M.SAMANTA(*JSSCollegeofPharmacy,Dept.ofPharmaceutics,Oaty,India):Designanddevelopmentof triphala fastdispersable tablets and its characterization. InternationalSeminaronHerbalDrugResearch,PN-064(2009).HPTLCofgallicacidasmarkercompoundintriphala


fastdispersabletabletsonsilicagelwithethylacetate-toluene-methanol-glacialaceticacid75:20:�:2.ResultsfromHPLCanalysiswerecomparable.Themethodwassuitableforroutinequalitycontrolofdispersabletabletsformulation.

herbal,densitometry,HPTLC 11a

105027 KarinROTHENBUEHLER,E.REICH*,M.HAMBURGER (*CAMAGLaboratory,Sonnen-mattstr.11,41�2Muttenz,Switzerland):ValidatedHPTLCmethodforskinlipids.CBS1045-6(2010).HPTLCofskinlipids(squalene,triolein,palmiticacid,1,2-dipalmitoyl-sn-glycerol,stea-rylpalmitate,cholesterylpalmitate,andcholesterol)onsilicagel(prewashedwithmethanol)firstwithtoluenetoadevelopingdistanceof80mm,thenwithn-hexane-t-butylmethylether-aceticacid80:20:1to45mminatwin-troughchambersaturatedfor20min.Detectionbydippingincopper(II)sulfatereagent followedbyheatingfor�0minat140°C.Densitometricabsorbancemeasurementat�50nm.Stabilityofstandardsandsamplesduring�h insolutionandon theplatewasgood.ThedifferencesofthehRfvaluesof7compoundson�plateswasgood(<�).TheprecisionofmeasurementwaslowestonHPTLCLiChrosphersilicagelplates(RSDof<5%,n=9).Thelinearrangeforallbuttwocompoundswasbetween100and�50ng/bandandcorrela-tioncoefficientswere>0.9975.

HPTLC,pharmaceuticalresearch 11c

13. Steroids

105028 K.BOBER(FacultyofPharmacy,DepartmentofAnalyticalChemistry,MedicalUniversityofSilesia,4JagiellonskiStreet,PL-41-200,Sosnowiec,Poland;[email protected]):Densitometryapplicationforevaluationofthevisualizingagentsfordehydroepiandrosterone.J.Liq.Chroma-togr.Relat.Technol.�1,267�-2685(2008).TLCofdehydroepiandrosteroneonsilicagelwithchloroform-acetone17:�withchambersaturationfor�0min.Detectionbydippinginto0.05%aqueoussolutionsofvisualizingagents(methyleneviolet,gentianviolet,janusblue,methyleneblue,malachitegreen,rhodamineB)andmethanolicchloramineT/methanolicsulfuricacidso-lution.Quantitativedeterminationbydensitometryat200nm(beforederivatizationandforme-thyleneviolet),657nm(gentianviolet),487nm(janusblue),488nm(malachitegreen),580nm(rhodamineB),and�61nm(chloramineT).LODwas0.29µg/5mL(withoutvisualizingagent,withchloramineTandwithrhodamineB),4.19µg/5mLwithmethyleneviolet,1.10µg/5mLwithgentianviolet,2.14µg/5mLwithjanusblue,and4.19µg/5mLwithmalachitegreen.

densitometry,quantitativeanalysis 1�a

15. Terpenes and other volatile plant ingredients

105029 B.QIN, J.EAGLES,F.MELLON,P.MYLONA,L.PEÑA,A.OSBOURN*(*SainsburyLa-boratory,NorwichNR47UH,UK,[email protected]):High throughput screeningofmutantsofoat thataredefectivein triterpenesythesis.Phytochemistry.71,1245-1252(2010).TLCofsqualene(1),2,�-oxidosqualene(2)andbeta-amyrin(�)intherootsofAvenastrigosaonsilicagelwithhexane-chloroform2�:2,hexane-chloroform1:1,andhexane-acetone4:1for(1),(2)and(�),respectively.Detectionbyexposuretoiodinevapor.QuantitativedeterminationbyGC-MS.

pharmaceuticalresearch,HPTLC,quantitativeanalysis,densitometry 15a

1050�0 A.VARMA,NeetaSHRIVASTAVA*(*B.V.PatelPharmaceuticalEducationandResearchDe-velopment(PERD)Centre,Sarkhej-GandhinagarHighway,Thaltej,Ahmedabad-�80054,Guja-rat,India;[email protected]):Microscaleprocedureforanalysisofandrogra-pholideinAndrographispaniculataleaves.J.PlanarChromatogr.2�,50-55(2010).HPTLCofandrographolideonsilicagelwithchloroform-methanol-ethylacetate12:�:2inatwin-troughchamber previously saturated for 15 min. Quantitative determination by absorbance measure-mentat22�nm.Therelativestandarddeviationofintra-dayandinter-dayanalysiswasintheran-


geof0.56-1.��%.Lineartiywasgivenbetween200-700ng/band;thecorrelationcoefficientwas0.9998andtheRSD0.97%.Thelimitsofdetectionandquantificationwere60and150ng/band.Averagerecoverywas98.8+-0.41%.

pharmaceuticalresearch,herbal,traditionalmedicine,HPTLC,densitometry,quantitativeanalysis 15a

17. Amines, amides and related nitrogen compounds

10506� R.DEEPAetal.,seesection�2

105087 B.MEHTAetal.,seesection�2

10511� JyotiSHRIVASTAVAetal.,seesection�2

18. Amino acids and peptides, chemical structure of proteins

1050�1 P.VENKATAKRISHNAN,E.NAKAYASU,I.ALMEIDA,R.MILLER*(*DepartmentofBiolo-gicalSciences,UniversityofTexasatElPaso,ElPaso,Texas,TheUnitedStatesofAmerica,[email protected]):Arginaseactivityinmitochondria-aninterferingfactorinnitricoxidesynthaseactivityassays.Biochem.Biophys.Res.Commun.�94,448-452(2010).HPTLCof[14C]-L-ar-ginineand[14C]-L-citrullineofanitricoxidesynthaseconversionassayinmitochondriaratliver,onsilicagelwithbutanol-aceticacid-water�:1:1.Detectionbydippinginasolutionof2%ninhydrin inacetone, followedbyheatingonaplateheater for1min.Aftervisualization, theplateswereexposedtoX-rayfilmfor4.5days.

pharmaceuticalresearch,HPTLC,quantitativeanalysis,autoradiography 18a

19. Proteins

1050�2 K.NISHIYAMA*,M.MAEDA,M.ABE,T.KANAMORI,K.SHIMAMOTO,S.KUSUMO-TO,T.UEDA,H.TOKUDA(*InstituteofMolecularandCellularBiosciences,TheUniversityofTokyo,Tokyo, Japan,[email protected]):Anovelcomplete reconstitution system formembraneintegrationofthesimplestmembraneprotein.Biochem.Biophys.Res.Commun.�94,7��-7�6(2010).TLCofliposomescontainingmembraneproteinintegrase(MPIase),onsilicagelwithethanol-chloroform-water7:�:4.Detectionbysprayingwithasolutionofanisalde-hyde-concentratedsulphuricacid-aceticacid�:4:1.ThehRfvalueofMPIasewas�5.

pharmaceuticalresearch,qualitativeidentification 19

21. Purines, pyrimidines, nucleic acids and their constituents

1050�� E. MINCSOVICS (OPLC-NIT Ltd,Andor Street 60, 1119 Budapest, Hungary, and CorvinusUniversity,FacultyofHorticulturalSciences,DepartmentofGeneticsandPlantBreeding,Bu-dapest,Hungary;[email protected]):Increaseddetectionsensitivityinfullyoff-lineOPLCbybilateralbandcompression.J.PlanarChromatogr.2�,190-192(2010).Aftersampleapplicationasbandsandfullyoff-lineOPLCseparationfollowedbydrying,theseparatedbandswerecompressedbilaterally,inparallel,perpendiculartothedirectionofdevelopment,byuseofastrongeluentandcapillarydrivenchromatography.Tointroducetheeluentforbandcompressi-onontothelayerasimplemanualtoolequippedwithparallelfoamstripswasconstructed.OPLCofablacktealeafextractandcaffeine,theophylline,andtheobromineonsilicagel(prewashedwithacetonitrile-water17:�)withtoluene-aceticacid�:2.Quantitativedeterminationbyden-sitometryat280nm.Afterbandcompression20ng/zonetheophyllinandtheobrominecouldbedetectedbydensitometryinthexanthinestandardmixtureataloadingof20µg/10mm.Thesecompoundswerenotvisibleintheoriginal,uncompressedchromatogram.

herbal,quantitativeanalysis,densitometry 21a


1050�4 K.VINODKUMAR*,T.VETRICHELVAN(*DeptofPharmaceuticalAnalysis,AdhiParasakthiCollege of Pharmacy,Tamil Nadu, India): Method development for risedronate sodium hemipentahydratebyUVspectroscopicmethodandhigh-performancethin-layerchromatography.IPAConvention,2010,RA-PO26.HPTLCofrisedronatesodiumonsilicagelwithwater-methanol-25%ammonia20:�:�.Densitometricevaluationat262nm.Themethodwaslinearintherangeof�-6ng/band,recoverywas98.6%.ResultswerecomparablewithHPLCresults.Theadvan-tageoftheHPTLCmethodisthesimultaneousanalysisofseveralsamples.

pharmaceuticalresearch,qualitycontrol,densitometry,comparisonofmethods,quantitativeanalysis,HPTLC 21a

22. Alkaloids

105002 MonikaJANICKAetal.,seesection1

1050�5 J.KENNEDY,J.WISEMAN*(*ProsoliaInc.,Indianapolis,IN46202,USA,[email protected]):DirectanalysisofSalviadivinoriumleavesforsalvinorinAbythinlayerchromatographyanddesorptionelectrosprayionizationmulti-stagetandemmassspectrometry.RapidCommun.MassSpectrom.24,1�05-1�11(2010).HPTLCofsalvinorinA(1),salvinorinC(2),divinatorinB(�),andsalvinorinB(4)intheleavesofSalviadivinoriumonsilicagelwithmethyltert-butylether-hexane�:1asmobilephase.Detectionbydesorptionelectrosprayionizationmulti-stagetandemmassspectrometry(TLC/DESI-MS).ThehRfwere49,64,85,and95forcompounds(1)-(4),respectively.TheuseofasimpleHPTLCprotocolincombinationwithDESI-MSallowedforimproveddetectionofdifferentspeciesofsalvinorinintheleafextracts.

toxicology,herbal,HPTLC,qualitativeidentification 22

23. Other substances containing heterocyclic nitrogen

1050�6 M. DOLOWY*,A. NIESTRÓJ (*Department ofAnalytical Chemistry, Faculty of Pharmacy,SilesianUniversityofMedicine,4JagiellonskaSt.,PL-42-200Sosnowiec,Poland;[email protected]):Densitometricdeterminationofursodeoxycholicacidinpharmaceuticalformulationsinformoftabletsandcapsules.J.Liq.Chromatogr.Relat.Technol.��,109-117(2010).TLCofur-sodeoxycholicacidonsilicagelwithn-hexane-ethylacetate-aceticacid22:22:5atroomtem-peraureinahorizontalchamber.ThehRfvaluewas48.Detectionbysprayingwith10%sulfuricacid and heating at 120 °C for 20 min. Quantitative determination by densitometric scanningat�60nm.LODandLOQwas0.014and0.041mg/spot,respectively.Thelinearityrangewas0.0�0-0.120mg/spot.Thecorrelationcoefficientrwas0.006�.Theaccuracyofthequantitativeanalysis of ursodeoxycholic acid in extracts from examined pharmaceutical formulations was95.�%and97.2%,andtheprecisionwas5.29and6.15%intabletsandcapsules,respectively.

qualitycontrol,densitometry,quantitativeanalysis 2�b

1050�7 AnnaPETRUCZYNIK(DepartmentofInorganicChemistry,MedicalUniversityofLublin,St-aszica6,20-081Lublin,Poland; [email protected]):Effectof chromatographicconditions on separation and system efficiency in HPTLC of selected quinoline standards oncyanopropylstationarypases.J.PlanarChromatogr.2�,56-64(2010).HPTLCofthirteenquino-lines(quinoline,isoquinoline,2,4-dihydroxyquinoline,8-hydroxyquinoline,5,6-benzoquinoline,2,2‘-diquinoline,8-methylquinoline,5-aminoquinoline,1-ethylquinoline,2-chlorquinoline,6-ni-troquinoline,2,6-dimethylquinoline,5-hydroxyquinoline)oncyanophasewithdifferentmobilephasespreparedfrommixturesofmethanol,acetonitrile,2-propanol, tetrahydrofuran,anddio-xanewithadditionofbufferatdifferentpH,ion-pairingreagents,orsilanolblockers.DetectionunderUVlightat254nmandbydensitometricabsorbancemeasurementat254nm.Improvedpeaksymmetrywasobservedformobilephasescontainingion-pairingreagent.Themostsym-metricalpeakswereobtainedbyuseofmobilephasecontainingdiethylamineassilanolblocker.

qualitativeidentification,HPTLC,densitometry 2�e

CAMAGBIBLIOGRAPHYSERVICE No.1051�

1050�8 T.M.SHAH*,S.S.SAVLE,M.T.CHHABRIA,I.S.RATHOD,C.J.SHISHOO,P.S.BRAHM-KSHATRIYA (*Dept. ofPharmaceuticalChem.&Dept. ofQ.A.,L.M.CollegeofPharma-cy,Navranga,Ahmedabad�80009,India):PharmacokineticstudyofanovelantihyperlipidemicagentLM-1�765-Aprodrug.Ind.J.Pharma.Science7161,644-650(2009).HPTLCofthenovelantihyperlipidemicagentLM-1�765inrabbitplasmaonsilicagel(pre-washedwithmethanol)withbenzene-methanol4:1inasaturatedchamberat25°C.Densitometricevaluationat�14nm.Themethodwaslinearintherangeof12.5-100ng/band.AlsoHPTLCofLM-1�765-C,ametaboliteoftheparentcompoundLM-1�765,onsilicagelwithtoluene-methanol2�:2.Densi-tometricevaluationat274nm.Detailsareprovidedonthecompleteextractionprocedurefortheextractionoftheparentcompoundanditsmetabolitefromplasma.

pharmaceuticalresearch,clinicalroutineanalysis,HPTLC,densitometry,quantitativeanalysis 2�b

24. Organic sulfur compounds

1050�9 K.PLUTA*,B.MORAK-MLODAWSKA,M.JELEN,R.KORLACKI(*DepartmentofOrganicChemistry,TheMedicalUniversityofSilesia,Jagiellonska4,41-200Sosnowiec,Poland;[email protected]):TLCseparationofisomericdiazinodithiinsanddiazinylsulfidesastheSmilesrearrangementproducts.J.Liq.Chromatogr.Relat.Technol.�1,�020-�0�1(2008).TLCoftwelfthioazinesonsilicagelwithchloroform-ethanol10:1andchloroform,andonaluminumoxidewithdichloromethaneandbenzene-chloroform1:1inachambersaturatedfor�0min.DetectionunderUV254and�66nm.Theretentionparametersweremeasuredandthencalculatedassepa-rationfactorsdeltaRf,RS,andalpha.ThehRfvalueswerecorrelatedwiththedipolemomentsofthioazinesandthesymmetryofdiazinodithiins.

qualitativeidentification 24

27. Vitamins and various growth regulators

105040 A.HOSU,ClaudiaCIMPOIU*,M.SANDRU,L.SESERMAN(*FacultyofChemistryandChe-micalEngineering,„Babes-Bolyai“University,11AranyJanos,400028Cluj-Napoca,Rumania;[email protected]): Determination of the antioxidant activity of juices by thin-layerchromatography.J.PlanarChromatogr.2�,14-17(2010).TLCofvitaminCofdifferentconcen-trations(0.45,0.50,0.55,0.60,and0.65mg/mL)andjuice(e.g.orangewithgrapefruit,orangewithappleandcarrot,„multi-fruit“)mixedwithamethanolicsolutionofDPPH(2,2-diphenyl-1-picrylhydrazyl)onsilicagel.Imagesofplateswereevaluatedusingaspecificcomputersoftware.Theequivalenceoftheresultsobtainedusingtheproceduredescribedwasdemonstratedbyap-plyingthetraditionalUV-visiblespectrophotometry.

Notefromeditor:Thetitleismisleading.ThisisnotTLCasthereisnochromatographyatall.Silicagelisusedascarrierandnotasstationaryphaseforaseparation.

foodanalysis,qualitativeidentification 27

28. Antibiotics, Mycotoxins

105041 M.BROSZAT,C.WELLE,M.WOJNOWSKI,H.ERNST,B.SPANGENBERG*(*UniversityofOffenburg,InstituteofProcessEngineering,Badstrasse24,77652Offenburg,Germany;[email protected]):AversatilemethodforquantificationofaflatoxinsandochratoxinAindriedfigs.J.PlanarChromatogr.2�,19�-197(2010).HPTLCofochratoxinA,aflatoxinB1,G1,B2,andG2onsilicagelwitht-butylmethylether-water-methanol-cyclohexane48:1:2:1inanunsaturatedhorizontaldevelopingchamberandonRP18withmethanol-4%aqueouszincsulfatesolution-ethylmethylketone5:5:1.Afterdevelopmentthesilicagelplatewasdippedfor2sinsiliconeoil-hexane1:2whichenhancedaflatoxinfluorescencebyafactorof2andochra-toxinAfluorescencebyafactorof�-10.RP18platesweredevelopedtoadistanceof75mminan unsaturated vertical chamber.Averaged densitograms were obtained in the emission wave-length range from445 to485nm.SamplepretreatmentwasbymodifiedQuEChERS(Quick,Easy;Cheap,Effectice,Rugged,Safe)extractionwithtetahydrofuranoracetone.Linearitywas


intherangeof�to100pg/zoneforaflatoxinsB2andG2,10to�50pg/zoneforaflatoxinsB1andG1,and0.25to2.5ng/zoneforochratoxinA.LOQfortheaflatoxinswerebetween1�and�5pg/zone(equivalenttoto1.5and2.5ppb);forochratoxinAitwas970pg/zone(56ppb).

toxicology,HPTLC,densitometry,quantitativeanalysis 28b

105042 MicheleHOELTZ*,J.WELKE,I.NOLL(*InstitutodeCiênciaeTecnologiadeAlimentos,Uni-versidadeFederaldoRioGrandedoSul,Av.BentoGonçalves,9500,91570-901PortoAlegre-RS,Brasil,[email protected]):Photometricprocedureforquantitativeanalysisofaf-latoxinB1inpeanutsbythin-layerchromatographyusingchargecoupleddevicedetector.Quim.Nova��,4�-47(2010).HPTLCofaflatoxinB1inpeanutsonsilicagelwithchloroform-acetone99:1.Quantitativedeterminationbyabsorbancemeasurementat�66nm,usingaCCDcamerafollowedbyimageprocessingusingthesoftwareImageJ.Linearitywasbetween0.8and4.8ng/zone.Theintra-dayandinter-dayprecisionshadaRSDlowerthan5.2%.LODwas0.4ng/zonewhileLOQwas1.2µg/kg.Theaveragerecoverywas94.9%.Theproposedmethodisasimple,efficientandlowcosttoolforquantitativeanalysisofaflatoxinB1inpeanutsamples.

foodanalysis,HPTLC,quantitativeanalysis,densitometry 28b

10504� JulianeWELKE,M.HOELTZ,H.A.DOTTORI,I.B.NOLL(*InstitutodeCienciaeTecnologiadeAlimentos,UniversidadeFederaldoRioGrandedoSul,Av.BentoGoncalves,9500,91570-901,PortoAlegre,RS,Brasil;[email protected]):Rapid,simple,andeconomicalmethodforquantificationofochratoxinAinredwine.J.PlanarChromatogr.2�,116-118(2010).HPTLCofochratoxinAonsilicagelwithtoluene-ethylacetate-formicacid6:�:1inasaturatedcham-ber.Detectionbysprayingwithethanolicsodiumbicarbonatesolution(6gsodiumhydrogencar-bonate,100mLwater,20mLethanol);afterdrying,evaluationandvideodensitometryunder�66nm.ThelinearregressioncoefficientofthecalibrationforOTAintheconcentrationrange0.8to12ng/zonewas0.9992.Themeanrecoverywas92+-8.9%.Recoveryfromwinesamplesatlevelsof0.5,2,and5µg/Lwas84,90,and102%,respectively,andtherespectiverelativestan-darddeviationswere5.7,8,and7%.LODwas0.�2ng/spotandLOQ0.1µg/L.foodanalysis,HPTLC

quantitativeanalysis 28b

105044 JulianeWELKE*,MicheleHOELTZ,H.DOTTORI, I.NOLL(*InstitutodeCiênciaeTecno-logia deAlimentos,UniversidadeFederal doRioGrande doSul,Av.BentoGonçalves, 9500,91570-901PortoAlegre-RS,Brasil, [email protected]) :DeterminationofochratoxinAinwinebythin-layerchromatographyusingchargecoupleddevice.J.Braz.Chem.Soc.21,441-446(2010).HPTLCofochratoxinAinwineonsilicagelwithtoluene-ethylacetate-chlo-roform-formicacid6:�:1.Quantitativedeterminationbyabsorbancemeasurementat�66nm,usingaCCDcamerafollowedbyimagesprocessingusingthesoftwareImageJ.Linearitywasbetween0.8and�2µg/L.Theintra-dayandinter-dayprecisionshadaRSDlowerthan9.9%and11.5%,respectively.LODwas16ng/zonewhileLOQwas100ng/zone.Theproposedmethodisasimple,efficientandlowcosttoolforquantitativeanalysisofochratoxinAinwinesamples.

foodanalysis,HPTLC,quantitativeanalysis,densitometry 28b

29. Pesticides and other agrochemicals

105045 A.FITTLER*,B.KOCSIS,Z.MATUS,L.BOTZ(*PharmaceuticalInstituteandCentralPhar-macy,FacultyofGeneralMedicine,UniversityofPécs,Honvédu.�.,Pécs7624,Hungary;[email protected]):Asensitivemethodforthin-layerchromatographicdetectionofampho-tericinB.J.PlanarChromatogr.2�,18-22(2010).TLCofamphotericinBonsilicagelwithchlo-roform-methanol-boratebuffer(pH8.�)4:5:1inachamberpre-saturatedfor20min.DetectionunderUV�66nm.ThehRf of themaincomponentwas46,andof theminorcomponent�1.


Quantitativedeterminationbyabsorbancemeasurementat�85nm.DirectbioautographywithCandidaalbicansproved tobe themostsensitivemethod,withadetection limitof0.8ngperspot.Fordensitometricevaluationofplatesat�85nmtentimesmoresubstanceisrequired.

pharmaceuticalresearch,qualitycontrol,densitometry,quantitativeanalysis,comparisonofmethods 29e

105046 G.OROS,T.CSERHÁTI*(*ResearchInstituteofMaterials,andEnvironmentalChemistry,Che-mical Research Center, HungarianAcademy of Sciences, Budapest, Hungary; [email protected]):Relationshipbetweenthecalculatedphysicochemicalparametersandreversedphasethin-layerchromatographicretentionbehaviorofcarboxamidefungicidesandrelatedcompounds.J.Liq.Chromatogr.Relat.Technol.��,880-89�(2010).TLCof6carboxamidefungicidesand11phenylbenzamidederivativesonsilicagelandaluminiumoxideimpregnatedbyovernightprede-velopmentinn-hexane-paraffinoil19:1withmixturesofmethanol-water,acetonitrile-water,tetrahydrofurane-water,andacetone-waterwiththeconcentrationoforganicmodifiervaryinginstepsof5%.DetectionunderUVlight.TheRMOandbvaluesrelatedtothemolecularlipo-philicityandtothespecifichydrophobicsurfacearea(b)ofthesoluteswerecalculatedseparatelyfor eachRP-TLCsystemand for eachanalyte.Thecorrelationsbetween thephysicochemicalparametersmeasuredwerecalculatedbylinearregressionanalysis.

environmental,qualitativeidentification 29e

105047 T.TUZIMSKI(DepartmentofPhysicalChemistry,FacultyofPharmacy,MedicalUniversityofLublin,6StaszicaStreet,20-081Lublin,Poland;[email protected]):Newprocedureforanalysisofcomplexmixturesbyuseofmultidimensionalplanarchromatographyincombinationwithdiode-arrayscanningdensitometryandhigh-performance liquidchromatographycoupledwithdiode-arraydetection.J.PlanarChromatogr.2�,184-189(2010).MultidimensionalplanarchromatographyonmonolayerormultiphaseplatesandmodernfiberopticalTLCdensitometerscannerswithDADisespeciallyusefulforcorrectidentificationofcomponentsofdifficult,com-plicatedmixtures,e.g.pesticidesinplantextracts(afterpreliminaryclean-upandconcentrationby,e.g.,solid-phaseextraction).TLCofclofentezine[�,6-bis(2-chlorophenyl)-1,2,4,5-tetrazine]inHerbaThymionsilicagelinahorizontalchamberwithtetrahydrofuran-n-heptane�:7inthefirstdirection,thenwithethylacetate-n-heptane1:4intheseconddirection.Detectionintherangeof200to600nmwithaTLC-DADscanner.AlsoTLCofthymeherbextractsonsilicagelandonRP18plateswithtetrahydrofuran-n-heptane�:7inthefirstdirectionandwithmethanol-water7:�intheseconddirection.LODandLOQwere0.2�and0.70µg/band,respectively, inTLC-DADand0.�5and1.06µg/mL,respectively,inHPLC-DAD.Averagerecoveriesfromthespikedplantmaterialsampleswere80.1%and100.5%at2.5µg/gand95.1%at5µ/gmeasuredat202nm.

agricultural,herbal,densitometry,quantitativeanalysis 29

105048 R. ZAKRZEWSKI*, W. CIESIELSKI (*Department of Instrumental Analysis, University ofLódz,Pomorska16�,90-2�6Lódz,Poland;[email protected]):Thinlayerchromato-graphywithpost-chromatographiciodine-azidereactionforthiuramanalysisinfoodsamples.J.Liq.Chromatogr.Relat.Technol.�1,2657-2672(2008).TLCandHPTLCofthiuramonsilicagelwithmethanolordichloromethaneinasaturatedhorizontalchamberfor15min.Detectionbysprayingwithimprovedandnon-improvediodine-azide,iodine,andcopper(II)reagentsandbyevaluationunderUV254nm.ForderivatizationthedevelopedplatesweresprayedwithfreshlypreparedmixturesofsodiumazideandstarchsolutionadjustedtopH6.0(5mLof10%aqueoussodiumazidesolutionand12.5mLof2%aqueousstarchsolutionweremixedandadjustedtopH6.0with0.1mol/Lhydrochloricacidsolution;thesolutionwasdilutedto25mLwithwater)andexposedtoiodinevaporfor5s.Quantitativeanalysisbyscanningwithanofficescanner(PCscanner)andafterdetectionwithimprovediodine-azidereagentdensitometricmeasurementat


48�nm.ThehRfvalueofthiuramwas29.LODwere�and0.5pmolperspotusingaiodine-azidedetectionsysteminTLCandHPTLC,respectively.Linearitywasintherangeof2-8pmolperspot;thecorrelationcoefficientrwas0.9981.ResultsobtainedbyuseofaPCscannerwerecomparabletomeasurementsusingaTLCdensitometer.

foodanalysis,postchromatographicderivatization,HPTLC,quantitativeanalysis,densitometry 29e

30. Synthetic and natural dyes

105049 W.SCHWACK*,ElodiePELLISSIER(*UniversityofHohenheim,InstituteofFoodChemistry,Garbenstrasse28,70599Stuttgart,Germany,[email protected]):Determinationofunauthorisedfat-solubleazodyesinspicesbyHPTLC.CBS10�,1�-15(2009).HPTLCofazodyes(SudanI,II,III,IV,B,SudanorangeG,Sudanred7B,Parared)inspicesamplesoncaffe-ineimpregnatedsilicagelwithisohexane-methylethylketone5:1withchambersaturationfor10min.Densitometricabsorptionmeasurementat�90,415,500,525and550nm.Thelimitsofdetectionwereapprox.10mg/kg.Confirmationofsuspectedcompoundsinsamplesbycompari-sonofUVspectra.TLC-MSanalysisinpositiveESImodefurtherconfirmspositivefindings.

foodanalysis,HPTLC,quantitativeanalysis,densitometry,TLC-MS �0a,4e

105050 R. SKIBINSKI*, L. KOMSTA (*Department of Medicinal Chemistry, Medical University ofLublin,Jaczewskiego4,20-090Lublin,Poland,[email protected]):ValidationofNP-HPTLCandRP-HPTLCmethodswithvideodensitometricdetectionforanalysisofziprasidoneinpharmaceuticalformulations.J.PlanarChromatogr.2�,2�-27(2010).HPTLCofziprasidone(5-[2-[4-(1,2-benzothiazol-�-yl)piperazin-1-yl]ethyl]-6-chloro-1,�-dihydroindol-2-one)on silicagelwithhexane-dioxane-propylamine5:45:2upto9cm(undersaturatedconditions)andonRP8withtetrahydrofuran-phosphatebuffer(pH9.0)1:1upto4.5cm(underunsaturatedcondi-tions),bothinhorizontalchambers.Quantitativedeterminationbyvideodensitometryat254nm.Calibrationwaslinearintherange0.2-1.2and0.1-1.1µg/spotziprasidoneforNP-HPTLCandRP-HPTLC,respectively.Theintra-dayprecisionsfor0.4-1.2µg/spotonNP-HPTLCwas2.0to5.2%andonRP-HPTLC4.0to6.1%;therespectiveinter-dayprecisionforNP-HPTLCwas2.0to6.7%andforRP-HPTLC4.1to7.1%.LOD/LOQonNP-HPTLCwas0.0�/0.09µg/spot;usingRP-HPTLC,LOD/LOQwas0.02/0.06µg/spot.Thespecificityofthemethodswasconfir-medbycomparisonofhRfvalues(74+/-2inNP-HPTLCand�6+/-1inRP-HPTLC,n=12).qualitycontrol,HPTLC

densitometry �0a

105051 B.YUANGSOI*,O.JINTASATAPORN,P.TABTHIPWON,C.KAMEL(*DepartmentofAqua-culture, Faculty of Fisheries, Kasetsart University, Bangkok 10900, Thailand; [email protected]):Comparativepharmacokineticsafterfeedingfancycarp(Cyprinuscarpio)withdietscon-tainingcarotenoids fromnatural sources (tea (Camellia sinensis),mulberry (Morusalba), andcassava(Manihotesculenta)leaf).J.PlanarChromatogr.2�,219-224(2010).TLCofcarotenoids(lutein,beta-carotene),astaxanthinandtanninonsilicagelwithpetroleumether-diethylether-acetone15:�:2inatwin-troughchambersaturatedfor�0minatroomtemperature.Quantitativedeterminationbydensitometricabsorbancemeasurementat450nm.ThehRfvaluesofluteinintea,mulberry,andcassavaleafwere19,22,and19andcorrespondedtoluteinstandard.TheleastpolarzonehadanaveragehRfvalueof98,98,and96fortea,mulberry,andcassavaleaf,respec-tively,andwasidenticalwithbeta-carotenestandard.

foodanalysis,densitometry,quantitativeanalysis �0b

105052 A.ZEB*,M.MURKOVIC(*Institute forBiochemistry,GrazUniversityofTechnology,Graz,Austria; [email protected]): High-performance thin-layer chromatographic method for


monitoring the thermal degradation of ß-carotene in sunflower oil. J. Planar Chromatogr. 2�,�5-�9(2010).HPTLCofbeta-caroteneonsilicagel(prewashedwithmethanol)withpetroleumether -hexane - acetone2:�:1 in a saturated twin-troughchamber.Quantitativedeterminationbyabsorbancemeasurementat450nm.Linearitywasbetween100and600ng/band.LODandLOQwere0.11and0.�7ng/band,respectively.Averageintra-dayprecisionandinter-day-precisi-onwere0.54%and0.50%,respectively.

foodanalysis,HPTLC,quantitativeanalysis,densitometry �0b

10500� A.ZEBetal.,seesection1

32. Pharmaceutical and biomedical applications

10505� R.ARAVIND*,J.SAJAN,K.BINDU,A.BINDU(*Dept.ofPharmaceuticalScience,Cheruvan-doorCampus,Kottayam,Kerala,India):QuantitativedeterminationofquercetinpresentintheleavesofCinnamomummalabatrum(Burman)BusingHPTLCmethod.AbstractNo.259,61stIPC(2009).HPTLCofquercetininalcoholicextractsoftheleavesofCinnamomummalabatrumonsilicagelwithtoluene-acetone-formicacid�6:12:5.Quantitativeabsorbancemeasurementat254nm.Thealcoholicextractwasfoundtocontain10.02mg/gofquercetin.Thetotalflavo-noidcontentwasestimatedusingacolorimetricmethodwithaluminumchloride.ResultswereingoodcorrelationwiththeHPTLCmethod.

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,comparisonofmethods,quantitativeanalysis �2e

10508� AmeliaM.AVACHAT*,S.B.BHISE(*DepartmentofPharmaceutics,SinhgadCollegeofPhar-macy,OffSinhgadRoad,Vadgaon(Bk.),Pune-411041,India;[email protected]):Sta-bility-indicatingvalidatedHPTLCmethodforsimultaneousanalysisofrifabutinandisoniazidinpharmaceuticalformulations.J.PlanarChromatogr.2�,12�-128(2010).HPTLCofrifabutinandisoniazidonsilicagelwithdichloromethane-acetone-methanol20:7:2inatwin-troughchamberpreviouslysaturatedfor25min.Quantitativedeterminationbyabsorbancemeasurementat504nmforrifabutin(hRf84)andat262nmforisoniazid(hRf48).Thelinearityrangewas10-70and5-�5µg/mL,thecorrelationcoefficientwas0.9991and0.9989,theprecision(RSD,n=6)0.90%and0.71%,andprecisionondifferentdays(RSD,n=�)was0.89%and1.01%.LODwas180µgand90µg/zone,LOQwas540and270µg/zone,andthesystemsuitability(RSD,n=6)was1.41%and1.86%forrifabutinandisoniazid,respectively.

qualitycontrol,HPTLC,quantitativeanalysis,densitometry �2a

105054 D.BAHETI*,P.SHINDE,M.AGRAWAL,R.BANGAR(*SitabaiThiteCollegeofPharmacy,Pune, Maharashtra, India): Quantitative estimation of withanolide A in marketed polyherbalspansules.AbstractNo.C-�72,61stIPC(2009).HPTLCofwithanolideAinextractsandspan-sulesdosageformonsilicagelwith toluene-ethylacetate-formicacid8:6:1.Densitometricevaluationat254nm.WithanolideAwaswellseparatedwithanhRfvalueof14.Thelinearityrangewas40-200ng/band.

pharmaceuticalresearch,qualitycontrol,herbal,densitometry,HPTLC,quantitativeanalysis �2e

105055 G.BANSAL*,ReechaMADAAN,S.KUMAR(*S.D.CollegeofPharmacy,Barnala,Punjab,India):PharmacognosticinvestigationonActaeaspicataL.AbstractNo.C-274,61stIPC(2009).TLCofpetroleumetherandchloroformextractsofActaeaspicatarootsonsilicagelwithn-he-xane-chloroform9:1(forpetroleumetherextracts)andtoluene-ethylacetate-glacialaceticacid80:50:15:1(forchloroformextracts).Detectionbysprayingwith50%methanolicsulfuric


acidfollowedbyheatingat105°C.Petroleumetherextractsshowed2bands,whereaschloro-formextractsshowed�bands.

qualitycontrol,herbal,qualitativeidentification �2e

105056 BharatiBARMECHA*,D.GHANAWAT,P.SHINDE,SmitaSHELKE(*SitabaiThiteCollegeofPharmacy,Pune,Maharashtra,India):Simultaneousdeterminationofgallicacidandpiperinebyhigh-performancethin-layerchromatography.AbstractNo.C-��8,61IPC(2009).HPTLCofgallicacidandpiperineincombinedformulationonsilicagelwithtoluene-ethylacetate-for-micacid16:8:1.Quantitativeabsorbancemeasurementat�20nm.Themethodwaslinearintherangeof200-800ng/bandforgallicacidand50-�50ng/bandforpiperine.

pharmaceuticalresearch,qualitycontrol,herbal,densitometry,HPTLC,quantitativeanalysis �2e

105057 P.BHARATI,A.VINODINI.A.S.REDDY,P.S.DEVI*(DepartmentofPharmaceuticalSci-ences,AndhraUniversity,Visakhapatnam-5�000�,India;[email protected]):Developmentandvalidationofaplanarchromatographicmethodwithreflectancescanningdensitometryforquan-titativeanalysisofanastrozole in thebulkmaterialand in tablet formulations. J.PlanarChro-matogr. 2�, 79-8� (2010). HPTLC of anastrozole (2-[�-(1-cyano-1-methyl-ethyl)-5-(1H-1,2,4-triazole-1-yl-methyl)-phenyl]-2-methyl-propanenitrile)onsilicagel(prewashedwithmethanol)withtoluene-acetone-ammonia60:40:�inatwin-troughchamberpreviouslysaturatedfor20min.Quantitativedeterminationbyabsorbancemeasurementat200nm.Recoveryofanastrozolefrom1mg tablet formulations ranged from98.9 to101.5%. Intra-dayand inter-dayprecisionwere1.�4%and1.59%,respectively.LODandLOQwere71and214ng/band.Thecorrelationcoefficientfortheanastrozolecalibrationwas0.998�overtherangeof500-1500ng/band(peakarea).

qualitycontrol,densitometry,quantitativeanalysis,HPTLC �2a

105058 K.BOBER(DepartmentofAnalyticalChemistry,FacultyofPharmacy,MedicalUniversityofSilesia,4JagiellonskaStreet,PL-41-200,Sosnowiec,Poland,bober@sum):Densitometricana-lysisofselectedfluorquinolines.J.Liq.Chromatogr.Relat.Technol.��,778-785(2010).TLCofofloxacinandpefloxacinonsilicagelwithacetonitrile-formicacid-water40:�:7inchambersaturatedfor�0min.Quantitativedeterminationbydensitometryat295nmforofloxacinandat280nmforpefloxacin.TheregressionequationswereachievedusingcomputerprogramSTATI-STICA7.1.

qualitycontrol,densitometry,quantitativeanalysis �2a

105059 M.BOMBAYWALA*,D.MOHALE,A.CHANDEWAR(*P.WADHWANICollegeofPharma-cy,Yavatmal,Mah,India):BioassayguidedfractionationofLagenariasicerariaforantihyperlipi-demicactivity.InternationalSeminaronHerbalDrugResearch,PN-009(2009).BioassayguidedfractionationofLagenariasicerariawascarriedoutonasilicagelcolumnwithsolventsinascen-dingorderofpolarity.EachfractionobtainedwassubjectedtopreparativeTLConsilicagelwithn-butanol-methanol-water�:1:1.FourbandswithdifferentRfvalueswerecollectedandactivecompoundswereextractedandscreenedforantihyperlipidemicactivity.

pharmaceuticalresearch,traditionalmedicine,clinicalchemistryresearch,herbal,preparativeTLC �2e

105060 A.BORKAR*,S.MULGUND,A.GAJBHAR,K.JAIN(*SinhgadCollegeofPharmacy,Pune,Maharashtra,India):HPLC-PADandHPTLCmethodsforquantitativeandchromatographicfin-


gerprintanalysisofEmbellaribes(Vidanga)Churnaformulation.AbstractNo.F-10,61stIPC(2009).HPTLCofEmbellaribesChurnaformulationonsilicagelwithchloroform-ethylacetate-formicacid5:4:1inatwintroughchamber.Densitometricmeasurementofembelinat291nm.Themethodwaslinearintherangeof600-1800ng/bandwithrecoveryvalueof99.1-101.2%.TheformulationwasalsoanalyzedbyHPLCandresultswerefoundtobecomparable. p h a r -maceuticalresearch,qualitycontrol

herbal,densitometry,HPTLC,comparisonofmethods,quantitativeanalysis �2e

105061 P.CHANDRA*,A.RATHORE,L.SATHIYANARAYANAN,K.MAHADIK(*BharatiVidya-peethUniversity,PoonaCollegeofPharmacy,Pune,Maharashtra,India):Developmentofvalida-tedHPLCandHPTLCmethodsforsimultaneousdeterminationoflevocetirizinedihydrochlorideandmontelukastsodiuminbulkdrugandpharmaceuticaldosageform.AbstractNo.F-18,61stIPC(2009).HPTLCoflevocetirizinedihydrochlorideandmontelukastsodiuminbulkandtabletdosageformulationonsilicagelwithtoluene-ethylacetate-methanol-25%ammonia5:14:5:2.BothdrugswerewellresolvedwithhRfvaluesof�1forlevocetirizineand44formontelukast.Quantitativeevaluationat2�1nm.Themethodwaslinearintherangeof500-2500ng/bandforlevocetirizineand1000-5000ng/bandformontelukast.BothdrugswerealsoanalysedbyHPLConRP18columnandresultswerecomparablewithHPTLC.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,comparisonofmethods �2a

105062 K.DATTA,A.SINGH*,A.MUKHERJEE,B.BHAT,B.RAMESH,A.BURMAN(*Molecu-larOncologyLab,DaburResearchFoundation,Sahibabad,India,[email protected]):Ecliptaalbaextractwithpotentialforhairgrowthpromotingactivity.J.Ethnopharmacol.124,450-456(2010). HPTLC fingerprinting of Eclipta alba on silica gel with chloroform - ethanol - water�5:10:2.Densitometricevaluationat254nm.Majorcompoundsidentifiedwerecoumestantsandwedelolactone,withhairgrowthpromotingactivity.

traditionalmedicine,herbal,HPTLC,qualitativeidentification �2e

10506� R.DEEPA*,K.MADHURI,R.SHANMUGAM,G.SADAGOBAN(*J.S.S.CollegeofPhar-macy,Ooty,T.N.,India):EstimationofharmalineinPeganumharmalabyHPTLC.InternationalSeminaronHerbalDrugResearch,PN-011(2009).HPTLCofharmalineinalcoholicextractsofPeganumharmalaonsilicagelwithchloroform-acetone-diethylamine5:4:1inasatura-tedchamberat25°C.ThehRfofharmalinewas50.Quantitativedeterminationbyabsorbancemeasurementat�51nm.

pharmaceuticalresearch,herbal,densitometry,quantitativeanalysis �2e,17a

105064 A.DHOBI*,N.VEKARIYA,G.PATEL,R.DHOLAKIYA,C.SHASHTRY(*ShreeDhanvan-taryPharmacyCollege,Kim,Gujarat,India):Developmentandvalidationofanalyticalmethodfor simultaneous determination of telmisartan and amlodipine besylate in bulk and tablets byHPTLC.AbstractNo.F-15961st IPC(2009).HPTLCof telmisartanandamlodipinebesylateonsilicagelwithtetrahydrofuran-dichloroethane-methanol-25%ammonia�0:10:5:2.BothcompoundswerewellresolvedwithhRfvaluesof22and45fortelmisartanandamlodipinebe-sylaterespectively.Densitometricevaluationat�26nm.Themethodwasfoundtobelinearintherangeof1200-7200ng/bandfortelmisartanand400-1400ng/bandforamlodipinebesylate.

qualitycontrol,densitometry,HPTLC,quantitativeanalysis �2a

105065 TatjanaDJAKOVIC-SEKULIC*,V.DESPOTOVIC,G.USCUMLIC(*DepartmentofChemistry,Biochemistry,andEnvironmentalProtection,UniversityofNoviSad,FacultyofSciences,Trg


DositejaObradovica�,21000NoviSad,RepublicofSerbia; [email protected]):Quantitativestructure-retentionrelationshipsstudyof theretentiondataof5,5-disubsti-tutedhydantoins.J.PlanarChromatogr.2�,201-207(2010).TLCandHPTLCof175,5-disubs-tituted hydantoins on silica gel with ethyl acetate - toluene (with �0-60 % ethyl acetate) andacetonitrile-toluene(with�0-50%acetonitrile)andonRP18withmethanol-water(with56-80%methanol)andacetonitrile -water (with�0-60%acetonitrile)at roomtemperaturewithoutchambersaturation.DetectionunderUV254nm.Theeffectofthestructuresofthederivativesontheirretentioninbothnormalandreversed-phasemodeswasinvestigatedbyuseofQSRRandmoleculardescriptors.Cross-validationindicatedthebestmodelsarereliableQSRRmodels.

qualitativeidentification,postchromatographicderivatization �2a

105066 N.DUBEY*,N.DUBEY,R.MEHTA,A.SALUJA(*SophisticatedInstrumentationCenterforAppliedResearchandTesting,VallabhVidyaNagar,Gujarat,IndiaandDeviAhilyaVishwavi-dyalaya,SchoolofPharmacy,Indore,MadhyaPradesh,India;[email protected]):SelectivedeterminationofaconitineinpolyherbaloilscontainingAconitumchasmanthumusinghigh-performance thin-layer chromatography. J.AOAC Int. 9�, 1617-1621 (2010). HPTLC ofaconitineonsilicagelwithethylacetate-ethanol�:1at22°Cinasaturatedtwin-troughchamber.ThehRfvalueofaconitinewas��.Quantitativedeterminationbyabsorptionmeasurementat2�8nm.LODandLOQwas20and70ng/band,respectively.Thelinearitywithrespecttopeakareawasintherangeof�00to1800ng/bandwithanrof0.9991.Therepeatability(RSD)was0.85%;andtheinter-dayandintra-dayprecision(RSD)was1.01-1.�8and1.04-1.�4%,respectively.

qualitycontrol,herbal,traditionalmedicine,HPTLC,densitometry,quantitativeanalysis �2e

105067 S.DWIVEDI*,J.BORKAR,A.SAOJI,P.YEOLE(*InstituteofPharmaceuticalEducationandResearch,Wardha,Maharashtra,India):PhytochemicalscreeningandevaluationbyTLCandUVspectrophotometerofpolyherbaltablets.AbstractNo.C-495,61stIPC(2009).Screeningofdif-ferent phytoconstituents in a polyherbal tablet formulation.TLCofn-hexane, chloroformandmethanolextractsofthetabletsonsilicagelwithn-hexane-ethylacetate7:�;chloroform-me-thanol9:1,andchloroform-glacialaceticacid-methanol-water8:40:15:10.EvaluationunderUV254nmaswellasunderUV�66nmaftersprayingwithdifferentreagents:20%sulfuricacid,aniline-hydrogenphthalatereagent,anisaldehyde-sulfuricacidreagent,andvanillin-sulfuricacidreagentfor thedetectionofpiperineandandrographide, theactiveconstituentspresent informulations likeTefrolivForte tablets.Otherconstituents(tanninsetc.)wereanalyzedbyUVspectrophotometry.

pharmaceuticalresearch,qualitycontrol,herbal,densitometry,qualitativeidentification �2e

105068 M.FAIYAZUDDIN*,J.ALI,S.AHMAD,N.AHMAD,J.AKHTAR,S.BABOOTA(*Formula-tionResearchLaboratory,DepartmentofPharmaceutics,FacultyofPharmacy,JamiaHamdard,NewDelhi-110062,India,andDepartmentofPharmaceutics,FacultyofPharmacy,IntegralUni-versity,Lucknow-226026,UttarPradesh,India;[email protected]):Chromato-graphicanalysisoftrans-andcis-citralinlemongrassoilandinatopicalphytonanocosmeceuti-calformulation,andvalidationofthemethod.J.PlanarChromatogr.2�,2��-2�6(2010).HPTLCoftrans-citralandcis-citralinlemongrassoilonsilicagelwithtoluene-ethylacetate17:�inatwin-troughchambersaturatedfor15min(at25°Cand55%RH).Detectionbysprayingwithvanillin-sulfuricacidreagent.Quantitativedeterminationbyabsorbancemeasurementat595nm.Intra-dayandinter-dayprecisionwereevaluatedbyreplicate(n=6)analysisofsamples(trans-citralat450,900,and1800ng/band,andcis-citralat470,940,and1880ng/band).Thelinearrangewas225-�600ng/bandfortrans-citral,and470-�760ng/bandforcis-citral.Thecorrelationcoefficientrwas0.99��fortrans-citraland0.99�7forcis-citral.Intra-dayprecision(n=6)was<�.56and5.66%fortrans-andcis-citral,respectively.Inter-dayprecisionwasassessedtobe<�.47and5.52%fortrans-andcis-citralbyrepeatingtheintra-dayassayonthreedifferentdays.


Repeatabilityofsampleapplicationandpeak-areameasurementwas0.98%,determinedbyper-forming six replicate analysesof the sameband (1800ng/band trans-citral and1880ng/bandcis-citral).TheRSDofrecoveryoftransandcis-citralwasintheranges1.�6-�.25and1.64-�.47,respectively.

herbal,qualitycontrol,cosmetics,HPTLC,quantitativeanalysis,densitometry �2e

105069 M. GANDHIMATHI*, M. SARAVANA KUMAR, R. BAGHLA (*College of PharmacySRIPMS,Coimbatore,TN,India):RP-HPTLCmethodfortheinvitroestimationofedaravoneinhumanplasma.IPAConvention,2010,RA-PO0�.HPTLCofedaravoneinsamplesofhumanplasma(purifiedbyliquid-liquidextraction)onRP-18withn-butanol-methanol-diethylether1:8:1.ThecompoundwaswellresolvedwithanhRfvalueof81.Densitometricevaluationat240nm.Thelimitofdetectionandquantificationwas25ngand150ngrespectively.Thelinearitywas600-2400ng/band.Recovery(%)basedonanalysisofspikedsamplewasmorethan65%.pharmaceuticalresearch,clinicalchemistryresearch,HPTLC,densitometry,

quantitativeanalysis �2c

105070 A.GANTAIT,S.PANDIT,N.K.NEMA,P.K.MUKJERJEE*(*JadavpurUniversity,SchoolofNaturalProductStudies,Kolkata-7000�2,India;[email protected]):Quantificationofglycyrrhizin inGlycyrrhizaglabra extract byvalidatedHPTLCdensitometry. J.AOAC Int.9�,492-495 (2010).HPTLCofglycyrrhizinon silicagelwithchloroform-methanol -water1�0:72:15inatwin-troughchambersaturatedfor�0min.DetectionunderUV254nmandaftersprayingwithanisaldehyde-sulfuricacidreagent.ThehRfvalueofglycyrrhizinwas22.Quanti-tativedeterminationbydensitometryat254nm.Thelinearitywasbetween0.96-4.80µg/spot,thecorrelationcoefficientwasr=0.99904andthestandarddeviationwas2.52%.Averagerecoverywas99.6%.LOQandLODwas246and81ng/spot.

herbal,traditionalmedicine,HPTLC,densitometry,quantitativeanalysis �2e

105071 TatanaGONDOVÁ*,D.HALAMOVÁ,K.SPACAYOVÁ(*DepartmentofAnalyticalChemistry,Faculty of Science, P. J. Safárik University, Moyzesova 11, Kosice SK-040 ß1, Slovak Repu-blic; [email protected]):Simultaneousanalysisofnewantidepressantsbydensitometricthin-layerchromatography. J.Liq.Chromatogr.Relat.Technol.�1,2429-2441 (2008).TLCofcitalopram,sertraline,fluoxetine,andfluvoxamineonsilicagelwithacetone-benzene-25%ammonia10:9:1ina twin-troughchambersaturatedfor15min.DetectionunderUV254nm.ThehRfvaluewas28forfluoxetine,44forcitalopram,56forfluvoxamine,and68forsertraline(withastandarddeviationless than0.02%inallcases).Quantitativedeterminationbyabsor-bancemeasurementat240nm.Thecalibrationcurvewaslinearintherangeof500-5000ng/spotforallanalyzedcompounds;correlationcoefficientswere found tobemore than0.998foralldrugs(exceptthe0.991forfluvoxamine).LODwas40ng/spotforcitalopramand50ng/spotforfluoxetine,fluvoxamine,andsertraline,respectively.LOQwasfoundtobe1�0and160ng/spotforcitalopramandfluoxetine,respectively.Intra-assayprecision(%RSD)waswithintherangeof0.52-0.87%and1.�4-1.84%forcitalopramandfluoxetine,respectively,inter-dayprecisionfortheanalysesconductedonthreeconsecutivedayswasbelow1.8%and2.5%forcitalopramandfluoxetine,respectively.Therecoveries(RSD)ofcitalopramadfluoxetinewerefoundtobeintherangeof99.�-100.�%(0.8%)and99.4-100.4%(1.9%),respectively.

qualitycontrol,densitometry,quantitativeanalysis �2a

105072 AnnaGUMIENICZEK*,A,BERECKA(*MedicalUniversityofLublin, Jaczewskiego4,20-090Lublin,Poland;[email protected]):Quantitativeanalysisofglicazideandglipi-zideintabletsbyanewvalidatedandstability-indicatingRPTLCmethod.J.PlanarChromatogr.2�,129-1��(2010).TLCofglicazideandglipizideonRP18silicagelwith60%acetonitrilein


pH2.�phosphatebufferinanunsaturatedhorizontalchambersatroomtemperature.Detectionandquantitativedeterminationbyabsorbancemeasurementat215nm.Linearitywasintherangeof0.8-1.8µg/zoneforbothdrugsandthecorrelationcoefficientsrwere0.998forgliazide(hRf�8)and0.99�forglipizide(hRf51).LODandLOQwere50and200ng/zone,respectively,forglicazide

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