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About This Manual Analytical methods for food safety are used to screen and confirm positive pesticides results and they must be granted at least four identification points. For LC/MS and GC/MS detection methods using either electron ionization (EI) or chemical ionization (CI), two derivatives or the powerful MSMS or HRMS are available. For maximum productivity, the highly specific MSMS and HRMS methods are the preferred methods. Multi-residue pesticide methods are analytically challenging because of the diverse number of chemical structures and physical properties of the target analytes. Thermo Fisher Scientific provides methods and mass spectrometry instrumentation that complies with the strict international rules for screening and confirmatory analyses on either LC or GC separation for polar or less polar compounds using ion trap, triple quad or high resolution accurate mass MS instrumentation. The information and methodology in this document will show you how to analyze large numbers of pesticides using the TSQ Quantum GC mass spectrometer. About This Manual Pesticide analysis is a chromatographic challenge because there is a large variety of chemical compound groups that require high sample throughput and short run times. Sample preparation and clean-up is an integral step in pesticide analysis because there is a significant amount of sample matrix involved. Setting up the analytical method in a particular way can cut down on instrument maintenance and increase the robustness of the method. In this manual, we will describe how to set up a generic method for the multi-component GC-MS/MS analysis of over 500 pesticides. This method includes information about implementing the widely distributed QuEChERS sample preparation procedure, which is suitable for non- and low-fat sample material and can be employed for GCMS and LCMS. For GCMS extractions, an additional solvent exchange step is included in the method, which provides the extract in a GC-compatible solvent. For LCMS, the intermediate acetonitrile extract can be used directly. The GCMS method of choice for a multi-component pesticide analysis in matrix samples is the MS/MS technique using either ion trap or triple quadrupole mass spectrometers. The sample preparation, GC configuration and analytical method setup information is valid for ion trap detection with PolarisQ or ITQ. The MS part of this manual focuses on the use of the TSQ Quantum GC triple quadrupole mass spectrometer for creating a multiple reaction monitoring (MRM) analysis method. Thermo Scientific Pesticide Analyzer Reference 3
About This Manual This manual also describes the recommended GC configuration with either split/splitless (SSL) or the temperature programmed inlet (PTV). For increased method robustness and easier maintenance, we recommend the use of a pre-column for matrix samples. The GC and autosampler analytical method parameters are provided with the analytical column of choice. The analytical method is described in detail for easy implementation. For easy setup of the pesticide method, a dedicated start-up kit is recommended. High sample throughput applications will require additional GC consumables. The TSQ Quantum GC mass spectrometer is operated in H-SRM mode, which provides the required high selectivity for a multi-component pesticide method. The SRM acquisition parameters for all pesticides are provided in the required precision with two digits prepared for exploiting the high H-SRM matrix selectivity. All pesticides are listed with precursor and product ions, as well as collision energy. All given transitions have been proven in Thermo Scientific application labs for use with different matrices. At least two independent SRM transitions are listed for each pesticide and they are compliant with international regulations and for reaching highest ranking with the European identification point system. Several pesticide compounds are listed with more than two SRM transitions. This flexibility in data acquisition allows for additional result confirmation and verification with unexpected matrix interferences of unknown sample matrices. QuanLab Forms is a workflow software suite for manual and full automatic data processing. peak integration, calibration and quantitation, QA/QC with qualifier checks and reporting provide a seamless data analysis for the multi component pesticide method. A special feature in QuanLab Forms data processing (called a local method) offers easy checking and optimization. 4 Pesticide Analyzer Reference Thermo Scientific
Page 1 and 2: Pesticide Analyzer Reference
Page 3 and 4: © 2009 Thermo Fisher Scientific In
Page 5 and 6: Contents 4 Pesticide Analyzer Refer
Page 7: Introduction Modern analytical meth
Page 11 and 12: What is a Pesticide? Pesticide Chem
Page 13 and 14: What is a Pesticide? Table 2. Pesti
Page 23 and 24: Preparing Samples Preparing Samples
Page 25 and 26: Preparing Samples Extracting Sample
Page 27 and 28: Preparing Samples 5. Place the tube
Page 29 and 30: Preparing Samples Exchanging Solven
Page 31 and 32: Preparing Samples 5. Centrifuge the
Page 33 and 34: Setting Up a Method 9. Now you can
Page 35 and 36: Configuring the GC/MS System for Pe
Page 53 and 54: List of Pesticide Compounds Table 2
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List of Pesticide Compounds Table 2
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SRM Method Library Table 27. Compou
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References References 1. Anastassia
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