QUICK POLAR PESTICIDES METHOD

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Frederick Benjamin Booth
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1 QUICK POLAR PESTICIDES METHOD

Quick Polar Pesticides Method QuPPe-Method allows the analysis of residues of very polar, non-quechers-amenable, pesticides in foods of plant origin PO (fruits, vegetables, cereals and processed

2 Quick Polar Pesticides Method QuPPe-Method allows the analysis of residues of very polar, non-quechers-amenable, pesticides in foods of plant origin PO (fruits, vegetables, cereals and processed products) and animal origin AO (milk and eggs). The new kit designed for the application of the QuPPe-PO method includes: Isotopically labeled analogues as internal standards (ISTDs); Standard mixtures of polar pesticides. Quick Method for the Analysis of numerous Highly Polar Pesticides in Foods of Plant Origin via LC-MS/MS involving Simultaneous Extraction with (QuPPe-Method) - Version 8.1 (March 2015, Document History, see page 58) Authors: M. Anastassiades; D. I. Kolberg; E. Eichhorn; A. Benkenstein; S. Lukačević; D. Mack; C. Wildgrube; I. Sigalov; D. Dörk; A. Barth The new kit designed for the application of the QuPPe-AO method includes: Centrifuge tubes containing ODS (octadecylsilane) as sorbent; Isotopically labeled analogues as internal standards (ISTDs); Standard mixtures of polar pesticides. Quick Method for the Analysis of Residues of numerous Highly Polar Pesticides in Food Commodities involving Simultaneous Extraction with and Determination via LC-MS/MS (QuPPe-AO-Method) II. Food of Animal Origin - Version 2 (Jan 2016, Document History, see page 16) Authors: M. Anastassiades; D. Kolberg; A. Benkenstein; S. Zechmann; Ready to use Standards: safer handling and application Cost-effective: frequently delivering fresh batches More accurate quantification: isotopically labeled analogues Evaluation of container/content interaction phenomena

PROCEDURE PLANT ORIGIN PRODUCTS ANIMAL ORIGIN PRODUCTS Weigh a representative portion of the sample homogenate into a 50 ml centrifuge tube Fresh fruits, vegetables and juices: 10 g ± 0,1 g Dried

nature of the matrix, add water to a total content of ca. 10 g (Table 19) Ad

3 PROCEDURE PLANT ORIGIN PRODUCTS ANIMAL ORIGIN PRODUCTS Weigh a representative portion of the sample homogenate into a 50 ml centrifuge tube Fresh fruits, vegetables and juices: 10 g ± 0,1 g Dried fruits and dried mushrooms: 5 g ± 0,05 g or 13,5 g ± 0,1 g of the re-hydrated and homogenized sample (corresponding to 5 g dried sample) Cereals, dried pulses and honey: 5 g ± 0,05 g Depending on the nature of the matrix, add water to a total content of ca. 10 g (Table 19) Add 10 ml acidified methanol (CH 3 OH + 1% F.A.) and 50 μl of IS (IS-working solution I) containing isotopically labeled analogues of one or more of the analytes of interest Weigh a representative portion of the sample homogenate into a 50 ml centrifuge tube Fresh milk and fresh eggs: 10 g ± 0,05 g Add water to a total content of ca. 10 g. In the case of cow milk (88% H 2 O) add 1,2 g of water and in the case of chicken eggs (76% H 2 O) add 2,4 g of water Add 10 ml acidified methanol (CH 3 OH + 1% F.A.) and 50 μl of IS (IS-working solution I) containing isotopically labeled analogues of one or more of the analytes of interest Shake vigorously for 1 min by hand or for 5-20 min by a mechanical shaker Shake vigorously by a mechanical shaker (Fresh products: 5-15 min; Dried products: min). Alternatively shake by hand for 1 min; in the case of dried products the shaking by hand is to be followed by a soaking period (15-30 min) and a subsequent second vigorous shaking by hand (1 min) For Paraquat and Diquat determination the shaking (1 min) is followed by a thermal treatment of 15 min at 80 C in a water bath. Then shaking again for 1 min and wait for the sample to cool down to room temperature Centrifuge for 5 min at >3000 g Transfer an aliquot (2 ml) into a 10 ml tube, containing 100 mg of ODS sorbent (Code: QPPAO01) and 2 ml of acetonitrile Centrifuge for 5 min at 4000 rpm Shake vigorously for 1 min by hand Filter an aliquot (3 ml) of the extract into a sealable storage vessel Use plastic flasks if pesticides (Paraquat, Diquat, Streptomycin, Glyphosate, etc.) that tend to interact with glass-surfaces are present Centrifuge for 5 min at >3000 g Filter an aliquot (ca. 3-4 ml) of the cleaned-up extract into a sealable storage vessel Transfer one or more aliquots (1 ml) of the filtered extract into vials for LC analysis Transfer one or more aliquots (1 ml) of the filtered extract into vials for LC analysis

4 Method: QuPPe-AO V14 g MgSO₄, 1 g NaCl, 1 g SCTD, 0,5 0,1 g ODS Packaging 50 Tubes (10 ml) Code QPPAO01 STANDARD MIX 1.1 CRM3G11L344 Ethephon HEPA Glyphosate AMPA Glufosinate MPPA N-Acetyl Glufosinate STANDARD MIX 1.2 CRM3G11L345 Ethephon HEPA Glyphosate AMPA Glufosinate MPPA N-Acetyl Glufosinate Fosetyl-Aluminium N-Acetyl AMPA Phosphonic acid STANDARD MIX 1.3 CRM3G11L346 Ethephon HEPA Glyphosate AMPA Glufosinate MPPA N-Acetyl Glufosinate Fosetyl-Aluminium N-Acetyl AMPA Phosphonic acid Maleic hydrazide Perchlorate Chlorate Cyanuric acid Bialaphos STANDARD MIX 1.4 CRM3G11L347 Phosphonic acid Perchlorate Chlorate CRM3G11L348 Fosetyl-Aluminium Maleic hydrazide Perchlorate STANDARD MIX 3 CRM3G11L349 Amitrole Daminozide ETU PTU Trimethylsulfonium Cyromazine

5 website/e-commerce STANDARD MIX 4.1 CRM3G11L350 Diquat Paraquat Daminozide N,N-Dimethylhydrazine Cyromazine Trimethylsulfonium Nereistoxin Melamine Propamocarb STANDARD MIX 4.2 CRM3G11L351 Amitrole ETU Daminozide PTU Cyromazine Trimethylsulfonium Nereistoxin Melamine Propamocarb Morpholine Diethanolamine Triethanolamine STANDARD MIX 5 CRM3G11L352 ETU PTU STANDARD MIX 6 CRM3G11L353 Streptomycin Kasugamycin STANDARD MIX 7 CRM3G11L354 Morpholine Diethanolamine Triethanolamine STANDARD MIX 8 CRM3J11L355 Water 1,2,4-Triazole Triazole-alanine Triazole-acetic acid Triazole-lactic acid 1,2,3-Triazole N.A

6 Accreditations and Certifications ISO Guide 34:2009 ISO/IEC 17025:2005 UNI EN ISO 14001:2004 UNI EN ISO 9001:2008 Download certificates alessandronitti graphicdesigner Produced by: LAB. INSTRUMENTS S.r.l. - High Pure Standards & Chemicals Division Tel Fax: SS 172 (Putignano-Alberobello) km Castellana Grotte (BA) Site: info@labinstruments.it,, and are trademarks of Lab.Instruments srl (Italy). All rights reserved. Specifications, term and pricing are subject to change. Not all products are available in all countries. Please consult your local rapresentative to details. QP 01 E 02/16

Analysis of Polar Pesticides Using a Mixed-Phase Mode HPLC Column

Analysis of Polar Pesticides Using a Mixed-Phase Mode HPLC Column Narong Chamkasem, Southeast Food and Feed Laboratory (SFFL), U.S. Food and Drug Administration, Atlanta, GA Disclaimer The findings and