Innovations in Elemental Analysis for Food, flavors, fragrances and consumer product analysis Presented by

Michelle Conkin

Atomic Spectroscopy Product Specialist

Determination of Metals in Food, Flavoring, Fragrances, and Natural and Synthetic consumer products

Wide Range of Matrices • Dairy, Meat, Fish, Grain, Vegetables, Fruit, etc • Processed goods • Nutraceuticals/pharmaceuticals • Consumer Products • Healthcare

Other Important Matrices • Drinking Water • Soil • Fertilizer • Food additives / flavors / colors • Packaging material

Which Elements are Monitored? 1. Toxic trace elements As, Cd, Hg, Pb, Tl, Cr(VI) - low level analysis (ppt to ppb)

2. Common elements that are toxic in excess Al, Ni, Cu, Zn, Se, Mo, Sn, etc.

3. Essential minerals at high levels (100 ppb to 1000 ppm) Na, Mg, P, S, K, Ca, Fe

4. Essential elements at low levels (100 ppt to 10 ppb) V, Cr(III), Co, Se, I

5. For some elements, chemical form may determine toxicity / bioavailability Chromatographic separation before ICP-MS analysis

6. Screening (semi-quant) analysis ICP-MS can measure almost every element at ng/L levels and is virtually free from interferences – ideal

screening tool Full mass range scan of food digest (e.g., microwave digestion)

ICP-QQQ

Flame and GF AAS

4100 MP-AES

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Innovation at Agilent: Atomic Spectroscopy Creating the world’s best, most complete atomic spectroscopy portfolio!

ICP-MS

ICP-MS

4200 MP-AES

ICP-OES ICP-OES

Drivers for product development

Analytical performance Increase sensitivity/lower background

Increase matrix tolerance

Faster/more productive solutions

Improve flexibility of operation – autosamplers, speciation, LA, etc.

New products to expand application range – right tool for the job

Practical/operational improvements

Operating cost – standby and running costs

Lab safety – flammable gases

Unattended operation and remote monitoring

Software – ease-of-use “walk up” software, ability to quickly develop methods

Decrease bench space requirements

Increase serviceability/access

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Finding the right tool for the job

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Atomic Absorption

4200 MP-AES 5100 ICP-OES 7900 ICP-MS 8800 ICP-QQQ

Single (few) element DLs ~100’s ppb (GF ppt) Fast (for single element) Good elemental coverage Low running cost

Multi element DLs single to 10’s ppb Faster Broader elemental coverage Good matrix tolerance Lowest running cost

Multi element DLs typically single ppb Very fast Can measure most elements Excellent matrix tolerance Moderate running cost

Multi element DLs typically single or sub-ppt Fast Can measure almost all elements Excellent matrix tolerance Higher running cost

Multi element DLs typically single or sub-ppt** Fast Can measure almost all elements** Ultimate application flexibility** Higher running cost

Range of solutions to fit your analytical need and budget

Higher Performance

• Ideal flame AA alternative

• Handles major, minor & most trace levels

• Wider linear dynamic range • Lower detection limits

Easy Operation

• New generation software • Simultaneous auto background correction • Plug & Play torch

Safer Laboratory Operation

• No flammable gases • Unattended multi-element

operation

Key benefits of MP-AES

Lowest cost of ownership

• Runs on air! • Eliminates on-going gas

supply costs

Low cost of ownership

October 13, 2014

Agilent Confidential

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• Supply of gases is the major on going cost for any routine elemental spectrometer.

• 4200 MP-AES uses nitrogen extracted from air using Agilent 4107 nitrogen generator.

• Example, big USA fruit juice manufacturer doing 100 FAAS samples per day, 3 elements per sample.

Online cost estimator available at: http://www.chem.agilent.com/en-US/products-services/Instruments-Systems/Atomic-Spectroscopy/Pages/mpaes-estimator.aspx

Safety

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• Using inert nitrogen gas to sustain the atomization/ionization source eliminates the need to use combustible gases like acetylene.

• Not having to ever replace a gas cylinder reduces manual handling issues.

Ease of Use

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Ease of Use

Simple software • Applet quick start methods

• Auto optimization tools

• FLIC and IEC tools

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Sample Preparation NIES CRM 10c Rice Flour • Digested in Milestone Ethos microwave using preloaded

method

• 0.5g in 7 mL of HNO3 and 1 mL H2O2

• Digested, cooled then diluted to 25 mL

• Final total dissolved solids of 2%

No further sample preparation required

No modifiers or ionization buffers required

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Results Method Detection Limits

Element/ Wavelengt

h (nm)

Ca 422.673

Cd 228.802

Cu 324.754

Fe 438.354

K 766.491

Mg 280.271

Mn 403.076

P 214.915

Zn 213.857

MDL (mg/kg) In soild sample

0.10 0.16 0.05 0.44 3.0 0.06 0.05 13 0.15

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Excellent Detection Limits • 2nd generation waveguide and torch handle the 2% matrix • Standard, robust sample introduction setup • High temperature plasma source (~5000K) improves

performance

Results CRM Recoveries

mg/kg in solid

Ca 422.673

Cd 228.802

Cu 324.754

Fe 438.354

K 766.491

Mg 280.271

Mn 403.076

P 214.915

Zn 213.857

Mean 96.0 1.96 4.13 11.50 2700 1174 37.35 3139 22.02

SD 2.5 0.11 0.29 1.03 105 23 1.04 92 0.48

Certified value 95 1.82 4.1 11.4 2750 1250 40.1 3350 23.1

2SD certified 2 0.06 0.3 0.8 100 80 2.0 80 0.9

% Recovery 101.0 107.7 100.8 100.9 98.2 93.9 93.1 93.7 95.3

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• Accurate determinations over a wide concentration range • All in one sample measurement

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How does the 5100 DSC technology work? Patented DSC technology for ICP-OES provides DV without compromise. • Single reading of the plasma for both radial and axial.

• Vertical torch gives high matrix capability

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Dichroic Spectral

Combiner (DSC)

To detector

Mirror

DSC Hole

Vertical torch

5100 SVDV Pre-optics 5100 SVDV Mode Selector

Vertical Torch

• Plug and play • Auto gas connected • Auto aligned to axial preoptics • Design enables 25% TDS • 5 x longer life compared to

horizontal quartz torches • High sensitivity

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Benefits of the 5100

• Fastest sample throughput of difficult samples

• Low gas consumption

Lowest cost of ownership

• Analytical performance

• System robustness and reliability

Enhanced Performance

• Hardware • Software

Simple Operation

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1. Lowest cost of ownership • High throughput facilitates low Ar consumption per sample

- (a) DSC. (b) VistaChip II. (c) 80 rpm pump. (d) SVS 2+ • 50% Lower power and 50% lower exhaust requirements. • 27MHz Solid State RF • Robust vertical torch • Increased self maintainability

SVDV Vendor A Vendor B

USEPA 200.7 (min) 1.0 2.3 2.3

Ar L/sample 20.4 39.53 43.0228

Valve/No Valve Valve Valve Valve 05

101520253035404550

5100 SVDV Vendor A Vendor B

Ar/sample

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2. Enhanced Performance Long Term Stability

• 4Hr Long Term Stability with complex matrix • 25% NaCl spiked with 250 ppb multi-element solution • <2.4% RSD

0%

20%

40%

60%

80%

100%

120%

140%

0:00:00 0:28:48 0:57:36 1:26:24 1:55:12 2:24:00 2:52:48 3:21:36 3:50:24 4:19:12

% R

eadb

ack

Time (h:mm:ss) As 188.980 Cd 228.802 Pb 220.353 Se 196.026

250ppb As/Se/Pb/Cd solution in 25% NaCl

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3. Simple Operation

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Presenting Agilent’s Game-Changing 7900 ICP-MS

We took the world’s best-selling, highest performing quadrupole ICP-MS, and made it 10x better!

Jan. 2014

Agilent Restricted

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Agilent 7900 ICP-MS Key Performance Highlights Rewriting the rules on ICP-MS

10x better signal to noise (S/N) – even lower detection limits - 2x higher sensitivity, 3-5x lower background

10x higher matrix tolerance – handles even tougher samples - HMI is still unique to Agilent. On the new ICP-MS, the optional Ultra HMI

(UHMI) extends capability to matrix levels of up to 25%

10x wider dynamic range – increases upper measurement limit - 7700’s 9 orders was best in class and new ICP-MS extends this by at least a

further order of magnitude (up to 11 orders detector linear dynamic range), allowing % levels to be quantified - a first for ICP-MS

30x faster detector –faster transient signal measurement (TRA) - 0.1ms integration time means improved single nanoparticle analysis

Improved productivity - New ultra fast ORS4 with less than 3 seconds switching time between modes - New ISIS 3 for fast unattended start-up, autotune and sample delivery

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Agilent Restricted

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ICP-MS Maintenance & Trouble Shooting Mar. 2014

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Speciation with LC-ICP-MS and GC-ICP-MS

Emerging elements/compounds: • Pesticide and OP nerve agent residues • PBDEs • Nanoparticles

As Speciation using LC-ICP-MS

Agilent Application Note: Routine Analysis of Toxic Arsenic Species in Urine Using HPLC with ICP-MS, 5989-5505EN, by Tetsushi Sakai and Steven Wilbur, Agilent Technologies

Sn Speciation using GC-ICP-MS

ICP-MS is a sensitive, selective and specific detector for most compounds that contain an element that can be measured by ICP-MS (any element except H, He, N, O, F, Ne or Ar)

Conventional “organo-metallic” compounds: • Inorganic vs organic arsenic • Organo-tin • Methyl-mercury, etc

Chromatogram of mixed organo-tin standard, containing 20ng/mL (ppb) each compound. Elution order is: Sn, MBT, TPrT, DBT, MPhT, TBT, TeBT, TPeT, DPhT TPhT. DL’s typically fg

Determination of As Species HPLC-ICP-MS chromatograms are shown for a marine animal (oyster tissue) and marine algae (Hizikia fusiforme).

The distribution of different As species is apparent.

Courtesy of Ute Kohlmeyer, GALAB, Germany

Determination of As Species in Food

As species distribution varies dramatically in marine organisms. Non-toxic arsenobetaine is the main species found in marine animals (fish and shellfish), whereas toxic arsenate and arseno sugars are the main species in marine algae.

Courtesy of Ute Kohlmeyer, GALAB, Germany

Thanks Any questions?

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