Waters Application Notes Food Testing TO YOUR LABORATORY GC WITH THEPOWER OF XEVO ■ Engineered to maximize uptime ■ Minimalmethoddevelopment ■ Easily surpassregulatory limits ■ Reduce training time andcosts www.waters.com/tqgc Ensuring consistent, reliable security in the global food supply In these recently published application notes, learn how Waters’ comprehensive analytical solutions are helping food testing laboratories to identify diverse chemical compounds, meet compliance requirements, increase productivity, and most importantly, help ensure public safety. SINGLE RESIDUE METHODS Determination of Highly Polar Cationic Pesticides and Plant Growth Regulators in Food Using UPLC-MS/MS ................................................................................................................................................................5 Determination of Anionic Polar Pesticides in Wheat Flour Extracts Using UPLC-MS/MS with the Torus DEA Column ................................................................................................................................... 12 Oasis PRiME HLB Cartridge for Clean-up of QuEChERS Extracts of Soybean Pods Prior to UPLC-MS/MS Determination of Free Acidic Herbicides ............................................................................................ 17 MULTIRESIDUE PESTICIDE METHODS Determination of 208 Pesticide Residues and their Metabolites in Foods Using Oasis PRiME HLB and Xevo TQ-GC .....................................................................................................................................25 GC-MS/MS Pesticide Analysis in Green Tea Using Targeted MRM and Full Scan Analysis in a Single Acquisition with Xevo TQ-GC .......................................................................................... 38 UPLC and APGC Multiresidue Pesticide Analysis on a Single Tandem Quadrupole MS Platform .............................. 43 ALLERGENS Targeted and Sensitive Detection of Food Allergens in Complex and Processed Foodstuffs using UPLC-MS/MS.......................................................................................................................... 55 Identification and Quantitative Analysis of Egg Allergen Peptides Using Data Independent Ion Mobility MS ....................................................................................................................................... 61 VETERINARY DRUGS Rapid, Simple, and Effective Clean-up of Bovine Liver Samples Prior to UPLC-MS/MS Multiresidue Veterinary Drug Analysis ............................................................................................... 69 Rapid Detection of 7 Illegal Veterinary Additives in Animal Feed Using Oasis PRiME HLB Clean-up and UPLC-MS/MS ...............................................................................................................73 Determination of Fipronil and Its Metabolite Fipronil Sulfone in Eggs by Liquid Chromatography- Tandem Quadrupole Mass Spectrometry Using a Modified QuEChERS Method ..............................................................77 Utility of the ACQUITY UPLC I-Class System and Ion Mobility in a Routine Workflow to Understand the Challenge of Analyzing Fluoroquinolone Antibiotic Residues ............................................................ 82 FOOD CONTACT MATERIALS Quantifying Primary Aromatic Amines (PAAs) in Polyamide Kitchenware ......................................................................... 93 Identification of Non-Intentionally Added Substances (NIAS) in Food Contact Materials Using APGC-Xevo G2-XS QTof and UNIFI Software ..............................................................................102 [ 1 ] NATURAL TOXINS Analysis of Ergot Alkaloids in Cereal Samples by Liquid Chromatography-Tandem Quadrupole Mass Spectrometry ......................................................................................................................................................113 Sensitive Analysis of Nodularin and Microcystins of Concern in Drinking Water Using Simplified Sample Preparation ............................................................................................................................................120 FOOD PROFILING/RESEARCH Rapid Determination of Cinnamomum Species Using the DART QDa System with LiveID for Ground Spice Authenticity Testing ...................................................................................................................125 A Real-Time Lipidomics Approach for Detecting Fish Fraud Using Rapid Evaporative Ionization Mass Spectrometry and LiveID Software.............................................................................132 Automated 2-Dimensional Fingerprint Analysis for Routine Botanical Authentication Using the ACQUITY QDa Mass Detector ......................................................................................................................................139 Improving Quantitative Analysis of Red Wine Using the Xevo G2-XS QTof with SONAR Data Independent Acquisition (DIA) .....................................................................................................................145 FOOD INGREDIENTS Determination of Vitamin D and Previtamin D in Food Products ..........................................................................................151 Soft Drink Analysis Using the ACQUITY UPLC H-Class PLUS System ...............................................................................159 [ 2 ] SINGLE RESIDUE METHODS [ 3 ] SINGLE RESIDUE METHODS [ 4 ] [ APPLICATION NOTE ] Determination of Highly Polar Cationic Pesticides and Plant Growth Regulators in Food Using UPLC-MS/MS Benjamin Wuyts,1 Janitha De-Alwis,2 Euan Ross,2 and Simon Hird2 1Waters Corporation, Zellik, Belgium 2Waters Corporation, Wilmslow, UK APPLICATION BENEFITS INTRODUCTION Provides a direct, single extraction The European Union Reference Laboratory for Pesticides Single Residue LC-MS/MS method for the analysis of Methods (EURL-SRM) published the QuPPe (Quick Polar Pesticides)1 various highly polar cationic pesticides methods for the simultaneous analysis of a number of highly polar and plant growth regulators in cereals, pesticides. To meet the needs of analyzing highly polar pesticides by fruit, and vegetable commodities. LC-MS/MS, details on a number of chromatographic methods have been provided including one based upon hydrophilic interaction liquid chromatography (HILIC)1-2 for the determination of a series of cationic and polar basic analytes. Although several compounds included in this application note are approved for use in Europe (maximum residue limits (MRLs) are listed in Table 1), other pesticide/crop combinations are not and default MRLs apply.3 As well as being a separate contaminant of interest, melamine4 is also a metabolite of cyromazine, although it is not yet part of the residue definition used for enforcement purposes. In this application note, example performance data is provided from Waters™ ACQUITY UPLC I-Class System and Xevo TQ-S micro on three commodities which represent high water content and high starch, low water content sample types. Organic wheat flour, cucumber, and apple, were extracted following the QuPPe method,1 to assess various performance factors of the UPLC-MS/MS method such as calibration linearity, retention time stability, method precision, and trueness. Table 1. Current MRLs2-3 in the three representative matrices for the compounds included in this application note. WATERS SOLUTIONS Compound MRL (mg/kg) ACQUITY™ UPLC™ I-Class System Apple Cucumber Wheat Xevo™ TQ-S micro Difenzoquat Herbicide 0.01 0.01 0.01 Propamocarb Fungicide 0.01 5.0 0.01 MassLynx™ MS Software Cyromazine Growth regulator 0.05 2.0 0.05 TargetLynx™ XS Application Manager Nereistoxin Insecticide 0.01 0.01 0.01 ACQUITY UPLC BEH Amide Column Melamine Contaminant 2.5 2.5 2.5 Chlormequat Growth regulator 0.01 0.01 4.0 Mepiquat Growth regulator 0.02 0.02 3.0 Trimethylsulfonium Organic cation 0.05 0.05 5.0 KEYWORDS LC-MS/MS, HILIC, pesticides, plant growth regulators, residue analysis, MRL, QuPPe, SANTE guidelines Determination of Highly Polar Cationic Pesticides and Plant Growth Regulators in Food Using UPLC-MS/MS [ 5 ] [ APPLICATION NOTE ] EXPERIMENTAL Sample preparation and extraction Homogenized organic apple and cucumber were extracted using the QuPPe method1 as shown in Figure 1. For wheat flour only 5 g of sample was taken and 10 mL of LCMS grade water was added to this before extraction with the acidified methanol. Before the centrifugation step, the wheat flour was placed in a freezer at -20 °C for 2 hrs. The supernatant from the QuPPe extracts were then filtered using a 0.45 µm PVDF filter, spiked with the pesticide mix and analyzed using the liquid chromatography, mass spectrometry method highlighted below. Method performance information for analyte recovery can be found in the QuPPe document.1 The performance of the LC-MS/MS step of the method was assessed using SANTE guidelines.5 Solutions of matrix-matched standards were prepared over the range 0.002 to 0.200 mg/kg (1.0 to 100.0 ng/mL in vial concentration) in apple and cucumber, 0.004 to 0.400 mg/kg (1.0 to 100.0 ng/mL in vial concentration) in wheat flour. Replicate injections at two concentration levels were run between bracketed calibration curves to assess the performance of the method. No isotopically labelled standards were used for this analysis. UPLC conditions UPLC system: ACQUITY UPLC I-Class with Weigh homogenized