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Quick Method for the LC-MS/MS Analysis of Highly …

EU Reference Laboratory for pesticides requiring Single Residue Methods (EURL-SRM) CVUA Stuttgart, Schaflandstr. 3/2, DE-70736 Fellbach, Germany Website: , E-Mail: 1 of 76 Quick Method for the Analysis of numerous Highly Polar Pesticides in Foods of Plant Origin via LC-MS/MS involving Simultaneous Extraction with Methanol (QuPPe- Method ) Version (August 2017, Document History, see page 73) Authors: M. Anastassiades; D. I. Kolberg; A. Benkenstein; E. Eichhorn; S. Zechmann; D. Mack; C. Wildgrube; I. Sigalov; D. D rk; A. Barth Note: Changes from to are highlighted in yellow 1.

QuPPe Method Version 9.3, August 2017 2 of 76 1. Scope and Short Description A method is described for the residue analysis of very …

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1 EU Reference Laboratory for pesticides requiring Single Residue Methods (EURL-SRM) CVUA Stuttgart, Schaflandstr. 3/2, DE-70736 Fellbach, Germany Website: , E-Mail: 1 of 76 Quick Method for the Analysis of numerous Highly Polar Pesticides in Foods of Plant Origin via LC-MS/MS involving Simultaneous Extraction with Methanol (QuPPe- Method ) Version (August 2017, Document History, see page 73) Authors: M. Anastassiades; D. I. Kolberg; A. Benkenstein; E. Eichhorn; S. Zechmann; D. Mack; C. Wildgrube; I. Sigalov; D. D rk; A. Barth Note: Changes from to are highlighted in yellow 1.

2 Scope and Short Description .. 2 2. Apparatus and Consumables .. 2 3. Chemicals .. 4 4. Disclaimer .. 6 5. Procedure .. 7 Sample preparation .. 7 Extraction / Centrifugation / Filtration .. 7 Blank extracts .. 9 Recovery 9 Preparation of calibration standards .. 10 QuPPe-PO- Method at a glance .. 12 LC-MS/MS Measurement .. 13 Method Glyphosate & Co. AS 11 .. 16 Method Glyphosate & Co. AS 11-HC .. 19 Method Glyphosate & Co. Hypercarb .. 23 Method PerChloPhos .. 30 Method 2 Fosetyl and Maleic Hydrazide .. 36 Method 3 Amitrole & Co.

3 38 Method Quats & Co Obelisc R .. 40 Method Quats & Co BEH Amide .. 42 Method 5 Quats & Co. MonoChrom MS .. 45 Method 6 Streptomycin and Kasugamycin .. 46 Method 7 Morpholine, Diethanolamine and Triethanolamine .. 47 Method 8 Triazole derivative metabolites (TDMs) .. 48 Method 9 Difluoroacetic acid and Trifluoroacetic acid .. 49 Calibration and Calculations .. 50 6. Performance Data .. 54 7. References .. 61 8. ANNEX .. 62 QuPPe Method Version , August 2017 2 of 76 1. Scope and Short Description A Method is described for the residue Analysis of very polar, non-QuEChERS-amenable, pesticides in foods of plant origin such as fruits (including dried fruits), vegetables, cereals and processed products thereof as well as honey.

4 Residues are extracted from the test portion following water adjustment and the addition of acidified methanol. The mixture is centrifuged, filtered and directly analyzed by LC-MS/MS . Various options for the simultaneous LC-MS/MS Analysis of different combinations of pesticides are provided. Quantification is in most cases performed with the help of isotopically labeled analogues of the target analytes, which are used as internal standards (ILISs). So far available, these ILISs are added directly to the test portion at the beginning of the procedure to compensate for any factors having an influence on the recovery-rates such as volume-deviations, analyte losses during sample preparation as well as matrix-effects during meas-urement.

5 2. Apparatus and Consumables Powerful sample processing equipment, Stephan UM 5 or Retsch Grindomix GM 300. 50 mL centrifuge tubes with screw caps, : a) reusable 50 mL Teflon centrifuge tubes with screw caps ( Nalgene/Rochester, USA; Oak-ridge, article-no. 3114-0050) or b) disposable 50 mL centrifuge tubes ( Sarstedt / N mbrecht, Germa-ny, 114x28 mm, PP, article-no. ). Automatic pipettes, suitable for handling volumes of 10 to 100 L, 200 to 1000 L and 1 to 10 mL. 10 mL solvent-dispenser, for the acidified methanol ( ).

6 Centrifuge, suitable for the centrifuge tubes employed in the procedure ( ) and capable of achieving > 4000 rpm. For the cleaning of extracts of commod that pose difficulties during filtration centrifugation at 10,000 g are needed. In this case the tubes should be checked if they are suitable for higher velocities. QuPPe Method Version , August 2017 3 of 76 Syringe filters, Cellulose mixed esters filters m pore size, Polyester filters m pore size (both from Ma-cherey-Nagel, D ren, Germany). Note: Significant levels of Perchlorate and Chlorate were detected in the above mentioned polyester fil-ters.

7 Cellulose mixed esters filters were found to be appropriate for these two compounds. For this suita-bility test take the worst case scenario into account where the filters are clogged by the extracts, not allow-ing large volumes ( 200 L) to pass. Thus elute only small volumes through the filters ( 200 L). Such clogging was observed when filtering extracts of industrially milled cereals, pears and pineapples. Furthermore, special attention is required if filters are used for diluted extracts as any detected levels in the extracts will have to be multiplied accordingly when calculating the levels in the sample.

8 To avoid clogging in many cases centrifugation at higher speeds (>10,000 g for 5 min) is helpful. Syringes, 2 or 5 mL disposable polypropylene syringes suitable for the above mentioned filters 0. Autosampler vials, suitable for LC auto-samplers, Use plastic vials if pesticides that tend to interact with glass-surfaces are present ( Phosphonate, Par-aquat, Diquat, Streptomycin and Glyphosate)1. Volumetric flask with stoppers, for the preparation of stock and working solutions. 20 mL; 25 mL; 50 mL, 100 mL glass flasks. Use plastic flasks and stoppers if pesticides that tend to interact with glass-surfaces are present ( Phosphonate, Paraquat, Diquat, Streptomycin and Glyphosate).

9 LC-MS/MS instrumentation, equipped with ESI source and appropriate columns, see details in chapters till 1 The list of compounds requiring plastic vessels is not necessarily comprehensive (this remark applies to the entire document). Such interactions with glass surfaces are typically more pronounced in solutions consiting of aprotic sol-vents ( acetonitrile). Increasing water content and/or acidity typically reduce such interactions. QuPPe Method Version , August 2017 4 of 76 3. Chemicals Unless otherwise specified, use reagents of recognized analytical grade.

10 Take every precaution to avoid possible contamination of water, solvents, sorbents, inorganic salts, etc. Water (deionized) Methanol (HPLC quality) Acetonitrile (HPLC quality) Formic acid (concentrated; > 95%) Acetic acid (concentrated; >98%) Acidified methanol Acidified methanol, pipette 10 mL formic acid ( ) in a 1000 mL volumetric flask and fill up to volume with methanol ( ). Citric acid-monohydrate ( ) Dimethylamine Dimethylamine, 40 % by Fluka (article-no. 38940). Ammonium formate ( ) Ammonium citrate-tribasic, anhydrous ( ) Sodium hydroxide ( ) Di-Sodiumtetraborate-decahydrate ( ) Dry ice Dry ice, technical grade can be used, it should be periodically checked not to contain pesticides at rele-vant levels.


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