Ultivo Applications Terri Sosienski LC/MS Applications Scientist. June 14, 2017

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1 Ultivo Applications Terri Sosienski LC/MS Applications Scientist 1

2 Ultivo Triple Quad LC/MS Designed for the user! Easy maintenance Compact size Robust, reliable and accurate An ideal tool for the food and environmental laboratory. 2

3 Food Applications 3

4 Mycotoxin Analysis in Foods Toxic byproducts of fungi on crops. Found in many types of foods. Grains Nuts Spices Fruits and vegetables Dairy Mycotoxins are regulated around the world. MRL range from <1ppb to >1 ppb EU reg No. 1881/26 and 15/21 Mycotoxin screening is a common analysis for a food laboratory 4

5 Mycotoxin Analysis in Foods Mycotoxin screen in foods 12 mycotoxins in corn and peanut matrix 5 mycotoxins in black pepper matrix 129 Infinity II HPLC 1 minute gradient method Column: Eclipse Plus C18 3.x15mm, 1.8um Mobile Phase: Water and Methanol,.5mM NH 4 F 5 mm NH 4 formate.1% Formic Acid Flow Rate:.45 ml/min Corn Peanut Black Pepper 5

6 # of Mycotoxins Mycotoxin Analysis in Foods Ultivo Triple Quad MS Dynamic MRM /5 MRL 1/1 MRL 1/2 MRL Quantitation limit 2x lower than MRL for most compounds Corn Peanut Black Pepper Matrix Limit of Quantitation 6

7 # of Mycotoxins Mycotoxin Analysis in Foods 6 replicate injections at LOQ RSD<1% at quantitation limit for all mycotoxins RSD<5% at quantitation limit for most mycotoxins. Aflatoxin B1 EU MRL: 2 ppb corn and peanut 5 ppb black pepper Aflatoxin B1 2ppt RSD%: 1.75 Avg. S/N: 326 Precision Corn Peanut Black Pepper Matrix Aflatoxin B1 2ppt RSD%: 2.34 Avg. S/N: 169 RSD 5-1% RSD -5% Corn Peanut Black Pepper 3 2 Aflatoxin B1 5ppt RSD%: 5.65 Avg. S/N: x lower than MRL 7

8 Pesticide Analysis in Foods Dorothy Yang Pesticides in Foods Crop productivity and success Pesticides in food Need to screen hundreds of pesticides in one method. MRL: 1ng/g 8

9 Pesticide Analysis in Foods 246 pesticides post-spiked into matrix. Extracted with Agilent EN QuEChERs with different clean-up for each matrix: 129 Infinity II HPLC Column: Eclipse Plus C18 3.x15mm, 1.8um Mobile Phase: Water and Methanol,.5mM NH 4 F 4.5 mm NH 4 formate.1% Formic Acid Flow Rate:.45 ml/min Avocado Orange Black Tea Modified EMR-Lipid PSA Kit Dispersive SPE - pigment Ultivo Triple Quad MS Dynamic MRM 9

10 Number of Pesticides # of pesicides detected Pesticide Analysis in Foods Avocado Orange Outstanding sensitivity LOQ 1ng/g and 5ng/g for most compounds Excellent Precision RSD% below 2% for >98% of the compounds Black Tea ng/g 5ng/g 1ng/g 2ng/g Pesticides Spike Levels Avocado Orange Black Tea % 5-1% 1-15% 15-2% >2% %RSD 1

11 Responses Pesticide Analysis in Foods Real World Samples Analysis: Non-Organic Orange and Avocado No pesticides could be detected in non-organic avocado 3 pesticides were detected in non-organic orange above MRL Agilent MassHunter Software makes sample analysis easy 22. -> 145., 22. -> 127.1, 22. -> 116.9, 22. -> x > x1 2, > 123.1, > ng/g 11 ng/g > 82.1, 2.1 -> 167.9, 2.1 -> 17.1, 2.1 -> 8.1 x ng/g Acquisition Time (min) x1 4 4 Responses Responses x x Carbaryl R^2 = Propiconazole R^2 = Pyrimethanil R^2 = Concentration (ng/g) 11

12 Environmental Applications 12

13 Trace Organic Compounds in Drinking Water Patrick Batoon Trace Organic Compounds (TOrCs) not completely removed from wastewater and drinking water treatment. Stable and common compounds Sourced from both industrial and household wastes Pharmaceuticals Ibuprofen, Carbamazepine Personal care products Benzophenone, DEET Industrial compounds Benzotriazole, BPA Pesticides Atrazine 13

14 Abundance Trace Organic Compounds in Drinking Water 31 representative TOrCs 1 ppt, 75 µl injection Infinity II HPLC Column: Zorbax Eclipse plus C18 3.x5mm, 1.8µm Mobile Phase: H 2 O and ACN,.2mM NH 4 F Flow Rate:.35 ml/min Flex Cube Online SPE 75ul injection volume. No bench-top sample pretreatment. SPE Cartridge: Zorbax Extend C18, 4.6x12.5mm, 5µm Load: H2O,.1% Formic Acid Elution: 1:1 ACN/IPA Fast 16 min total! 14

15 Trace Organic Compounds in Drinking Water Ultivo Triple-Quad MS Sensitivity enhanced further with Agilent Flex Cube Online SPE. No complex sample preparation needed. a <.5 ng/ L, 19 TOrCs.5-5 ng/ L, 1 TOrCs b High linearity with R 2 >.99 for quantitation range.5-2ng/l Quantitation Limit <.5-5 ng/l for most analytes. c >5 ng/ L, 2 TOrCs 15

16 Per/Poly Fluoroalkyl Substances (PFAS) in Water Tarun Anumol PFASs are sourced from: Fire-fighting foams Non-stick cookware Food packaging Ubiquitous in the environment. USEPA drinking water health advisories for PFOA and PFOS 7 ng/l in drinking water US state public health guidelines for PFASs 2-4 ng/l in drinking water. 16

17 Per/Poly Fluoroalkyl Substances (PFAS) in Water 17 PFASs in drinking water. All 14 from USEPA 537 method. 25mL water samples. Extracted with Agilent Weak Anion Exchange (WAX) cartridges. 129 Infinity II LC Delay Column: Zorbax Eclipse plus C18 4.6x5mm, 3.5µm Analytical Column: Zorbax Eclipse plus C18 3.x5mm, 1.8µm Mobile Phase: H 2 O and 95:5 MeOH/H 2 O, 5mM Ammonium Acetate Flow Rate:.4 ml/min Runtime: 19 minutes Ultivo Triple Quad MS in negative ionization mode. 17

18 Recovery (%) Per/Poly Fluoroalkyl Substances (PFAS) in Water Recovery 7-12% for all compounds at 1 µg/l and 5 µg/l spiking levels g/l Post Spike 5 g/l Post Spike Excellent Linearity,.1 2 µg/l, R 2 >.99. RSD%:.3-1.8% for all compounds at both spiking levels (5 replicates) PFBA PFPeA PFBS PFHxA PFHpA PFHxS PFOA PFNA PFOS PFDA N-MeFOSAA PFDS PFUdA N-EtFOSAA PFDoA PFTeDA PFTrDA PFOS PFOA 18

19 Ultivo Triple Quad LC/MS Optimal sensitivity, robustness, accuracy No sacrifice in performance when compared to larger instruments. Unbelievably Powerful Remarkably Small! 19

20 Come Visit Us! Application Posters Today (6/6) TP-197 Mycotoxins in Foods, Terri Sosienski TP-28 Pesticides in Foods, Dorothy Yang TP-178 TrOCs in Drinking Water, Tarun Anumol Thursday (6/8) ThP-174 PFASs in Water, Terri Sosienski 2

21 Come Visit Us! R&D Presentations Today (6/6) Oral Presentation Room Twisted dual-field multiple converging ion guides: Achieving high performance in tandem mass spectrometers with reduced size, Haopeng Wang Thursday (6/8) ThP-38 Improving Quadrupole Performance with a thin DC only quadrupole pre-filter, Laura Pollum 21