ANALYSIS OF BIOCIDES USING UPLC · MIT CMIT Carbendazim BIT Phenoxyethanol Benzoic acid...
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TO DOWNLOAD A COPY OF THIS POSTER, VISIT WWW.WATERS.COM/POSTERS Meet Regulatory Mandates to Protect Methylparaben Benzoic acid MIT CMIT Carbendazim BIT Phenoxyethanol ANALYSIS OF BIOCIDES USING UPLC ® Peter J. Lee and Alice J. Di Gioia Waters Corporation, Milford, MA, USA What Do They Have in Common? Solution for Biocide Analysis S N O S N O Cl S NH O NH N NH O O O OH O OH OH O O 1a 1b 2 3 4 5 6 MIT CMIT Carbendazim BIT Phenoxyethanol Benzoic acid Methylparaben Kathon™ MIT CMIT Carbendazim BIT Phenoxyethanol Benzoic acid Methylparaben AU 0.00 0.05 0.10 Minutes 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00 Kathon 5 ppm 1 2 3 4 5 6 7 8 9 Mean Std. Dev. % RSD MIT (min) CMIT (min) Carbendazim (min) BIT (min) Phenoxy ethanol (min) Benzoic acid (min) Methy lparaben (min) 0.286 0.286 0.287 0.286 0.286 0.286 0.287 0.286 0.287 0.286 0.001 0.19 0.908 0.908 0.908 0.908 0.908 0.908 0.908 0.908 0.909 0.908 0.000 0.04 1.147 1.147 1.147 1.148 1.148 1.149 1.148 1.150 1.150 1.148 0.001 0.10 1.600 1.601 1.601 1.602 1.601 1.602 1.601 1.602 1.602 1.601 0.001 0.03 2.141 2.141 2.141 2.142 2.141 2.142 2.141 2.142 2.142 2.142 0.001 0.03 2.400 2.401 2.400 2.401 2.400 2.401 2.400 2.401 2.401 2.401 0.001 0.02 2.671 2.672 2.671 2.672 2.671 2.672 2.671 2.672 2.672 2.672 0.001 0.02 Table 1. Component Summary For Retention Time 1 2 3 4 5 6 7 8 9 Mean Std. Dev. % RSD MIT CMIT Carbendazim BIT Phenoxy ethanol Benzoic acid Methy lparaben 34745 34730 34684 34741 34761 34673 34753 34781 34782 34739 38 0.1 68748 68894 69423 69168 68952 69132 68903 68736 69050 69001 219 0.3 134846 134698 134511 135187 134533 134817 135014 135018 134694 134813 229 0.2 227719 228692 227840 228238 228331 228461 228616 227710 228489 228233 383 0.2 57857 57882 57682 57388 58008 57802 57863 57845 57809 57793 174 0.3 172510 173440 170783 173125 170433 170579 172557 170954 172072 171828 1157 0.7 173458 172053 172192 172113 172156 171725 171723 171833 172143 172155 523 0.3 Table 2. Component Summary For Area 1 2 3 4 5 6 7 Component Match1 Spect. Name Match1 Angle Match1 Threshold Purity1 Angle Purity1 Threshold MIT CMIT Carbendazim BIT Phenoxy ethanol Benzoic acid Methy lparaben 2-methy l-4-isothiazolin-3-one 5-chloro-2-methy l-4-isothiazoline-3-one carbendazim 1,2-benzisothiazol-3-one 2-phenoxy ethanol benzoic acid methy lparaben 0.488 0.293 0.169 0.181 0.820 0.217 0.288 1.585 1.465 1.239 1.277 2.663 1.387 1.385 0.705 0.694 0.320 0.371 2.062 0.508 0.465 1.035 0.842 0.546 0.616 2.449 0.703 0.726 PDA library matching results table < < Calibration Plot Name: Kathon; R^ 2: 0.999934 Name: Carbendazim; R^2: 0.999941 Name: BIT; R^2: 0.999919 Name: Phenoxyethanol; R^2: 0.999958 Name: Benzoic acid; R^2: 0.999800 Name: Methylparaben; R^ 2: 0.999979 Area 0 100000 200000 300000 400000 500000 600000 700000 800000 900000 Amount 0.00 2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 (ppm) BIT Methylparaben Benzoic acid Carbendazim Kathon Phenoxyethanol ACQUITY UPLC ® System rapidly and accurately analyzes biocides ● Separate 7 components in 3 minutes ♦ Baseline resolution ● Excellent reproducibility ● Great sensitivity Empower™ data automation, from collection to reporting ● Peak purity & identification ● Calibration & quantification ● Custom calculations ● Automate report generation Ideal solution for: QC, product development, and problem-solving Experiment: Instrument and Operation Conditions LC: ACQUITY UPLC ® with PDA Software: Empower™ Column: ACQUITY UPLC BEH C 18 2.1 mm x 50 mm Weak Wash: 95:5 H 2 O/CH 3 CN (600 μL) Strong Wash: 50:50 H 2 O/CH 3 CN (600 μL) Mobile Phase A: 0.05v% of TFA in H 2 O Mobile Phase B: 0.05v% of TFA in CH 3 CN Linear Gradient: 5% B to 15% B in 2.9 min Flow Rate: 1 mL/min Sampling Rate: 20 pt/s Injection Volume: 5 μL Column Temperature: 30 °C PDA: 210-500 nm PDA Filter Response: 0.1 sec Overlay 9 Replicate Injections: PDA Timed Chromatograms UPLC ® RT Reproducibility UPLC ® Area Reproducibility 1. P. J. Lee, A. J. Di Gioia, ACQUITY UPLC PDA ANALYSIS OF BIOCIDES (PART 1), Waters Corporation, Application Note 720001832EN, 2006. 2. P. J. Lee, A. J. Di Gioia, ACQUITY UPLC PDA ANALYSIS OF BIOCIDES (PART 2): PASS OR FAIL CUSTOM CALCULATION, Waters Corporation, Application Note 720001833EN, 2006. Available for download at www.waters.com References Conclusions UV/PDA Calibration Curves 3-minute analysis of a blend of common biocides Biocides Kill Micro-organisms UV Spectra Extracted from PDA Chromatograms for Library & Peak Purity: ● Confirm peak identity ● Assure non-coelution of spectrally dissimilar components Protected by Biocides! No biocides With biocides Needs for Biocide Analysis Sensitivity Resolution Speed Innovation
Transcript of ANALYSIS OF BIOCIDES USING UPLC · MIT CMIT Carbendazim BIT Phenoxyethanol Benzoic acid...
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Meet Regulatory Mandates to Protect
Methylparaben
Benzoic acid
MIT
CMIT
Carbendazim
BIT
Phenoxyethanol
ANALYSIS OF BIOCIDES USING UPLC®
Peter J. Lee and Alice J. Di Gioia Waters Corporation, Milford, MA, USA
What Do They Have in Common? Solution for Biocide Analysis
S
N
O
S
N
O
Cl
SNH O
NH
N
NH
O
O
O
OH
O OH
OH
O O
1a 1b2
3 4 5 6
MITCMIT
Carbendazim
BIT Phenoxyethanol Benzoic acid Methylparaben
Kathon™
MIT C
MIT
Car
bend
azim
BIT
Phe
noxy
etha
nol B
enzo
ic a
cid
Met
hylp
arab
en
AU
0.00
0.05
0.10
Minutes0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20 2.40 2.60 2.80 3.00
Kathon
5 ppm
1
2
3
4
5
6
7
8
9
Mean
Std. Dev .
% RSD
MIT(min)
CMIT(min)
Carbendazim(min)
BIT(min)
Phenoxyethanol(min)
Benzoic acid(min)
Methy lparaben(min)
0.286
0.286
0.287
0.286
0.286
0.286
0.287
0.286
0.287
0.286
0.001
0.19
0.908
0.908
0.908
0.908
0.908
0.908
0.908
0.908
0.909
0.908
0.000
0.04
1.147
1.147
1.147
1.148
1.148
1.149
1.148
1.150
1.150
1.148
0.001
0.10
1.600
1.601
1.601
1.602
1.601
1.602
1.601
1.602
1.602
1.601
0.001
0.03
2.141
2.141
2.141
2.142
2.141
2.142
2.141
2.142
2.142
2.142
0.001
0.03
2.400
2.401
2.400
2.401
2.400
2.401
2.400
2.401
2.401
2.401
0.001
0.02
2.671
2.672
2.671
2.672
2.671
2.672
2.671
2.672
2.672
2.672
0.001
0.02
Table 1.Component Summary For Retention Time
1
2
3
4
5
6
7
8
9
Mean
Std. Dev .
% RSD
MIT CMIT Carbendazim BIT Phenoxyethanol Benzoic acid Methy lparaben
34745
34730
34684
34741
34761
34673
34753
34781
34782
34739
38
0.1
68748
68894
69423
69168
68952
69132
68903
68736
69050
69001
219
0.3
134846
134698
134511
135187
134533
134817
135014
135018
134694
134813
229
0.2
227719
228692
227840
228238
228331
228461
228616
227710
228489
228233
383
0.2
57857
57882
57682
57388
58008
57802
57863
57845
57809
57793
174
0.3
172510
173440
170783
173125
170433
170579
172557
170954
172072
171828
1157
0.7
173458
172053
172192
172113
172156
171725
171723
171833
172143
172155
523
0.3
Table 2.Component Summary For Area
1
2
3
4
5
6
7
Component Match1Spect. Name
Match1Angle
Match1Threshold
Purity1Angle
Purity1Threshold
MIT
CMIT
Carbendazim
BIT
Phenoxyethanol
Benzoic acid
Methy lparaben
2-methy l-4-isothiazolin-3-one
5-chloro-2-methy l-4-isothiazoline-3-one
carbendazim
1,2-benzisothiazol-3-one
2-phenoxyethanol
benzoic acid
methy lparaben
0.488
0.293
0.169
0.181
0.820
0.217
0.288
1.585
1.465
1.239
1.277
2.663
1.387
1.385
0.705
0.694
0.320
0.371
2.062
0.508
0.465
1.035
0.842
0.546
0.616
2.449
0.703
0.726
PDA library matching results table
< <
Calibration Plot
Name: Kathon; R 2̂: 0.999934Name: Carbendazim; R 2̂: 0.999941Name: BIT; R 2̂: 0.999919Name: Phenoxyethanol; R 2̂: 0.999958Name: Benzoic acid; R 2̂: 0.999800Name: Methylparaben; R 2̂: 0.999979
Area
0
100000
200000
300000
400000
500000
600000
700000
800000
900000
Amount0.00 2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00
(ppm)
BIT
Methylparaben
Benzoic acid
Carbendazim
Kathon
Phenoxyethanol
ACQUITY UPLC® System rapidly and accurately analyzes biocides
● Separate 7 components in 3 minutes ♦ Baseline resolution
● Excellent reproducibility ● Great sensitivity
Empower™ data automation, from collection to reporting
● Peak purity & identification ● Calibration & quantification ● Custom calculations ● Automate report generation
Ideal solution for: QC, product development, and problem-solving
Experiment:
Instrument and Operation Conditions
LC: ACQUITY UPLC® with PDA Software: Empower™ Column: ACQUITY UPLC BEH C18 2.1 mm x 50 mm Weak Wash: 95:5 H2O/CH3CN (600 µL) Strong Wash: 50:50 H2O/CH3CN (600 µL) Mobile Phase A: 0.05v% of TFA in H2O Mobile Phase B: 0.05v% of TFA in CH3CN Linear Gradient: 5% B to 15% B in 2.9 min Flow Rate: 1 mL/min Sampling Rate: 20 pt/s Injection Volume: 5 µL Column Temperature: 30 °C PDA: 210-500 nm PDA Filter Response: 0.1 sec
Overlay 9 Replicate Injections: PDA Timed Chromatograms
UPLC® RT Reproducibility
UPLC® Area Reproducibility
1. P. J. Lee, A. J. Di Gioia, ACQUITY UPLC PDA ANALYSIS OF BIOCIDES (PART 1), Waters Corporation, Application Note 720001832EN, 2006.
2. P. J. Lee, A. J. Di Gioia, ACQUITY UPLC PDA ANALYSIS OF BIOCIDES (PART 2): PASS OR FAIL CUSTOM CALCULATION, Waters Corporation, Application Note 720001833EN, 2006.
Available for download at www.waters.com
References
Conclusions
UV/PDA Calibration Curves
3-minute analysis of a blend of common biocides
Biocides Kill Micro-organisms
UV Spectra
Extracted from PDA Chromatograms for Library & Peak Purity: ● Confirm peak identity ● Assure non-coelution of spectrally dissimilar components
Protected by Biocides!
No biocides With biocides
Needs for Biocide Analysis
Sensitivity
Resolution
Speed
Innovation
drelingc
Text Box
© 2007 Waters Corporation
drelingc
Text Box
720002096EN
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