1 Scope
This standard specifies LC-MS-MS method for determination of 486 pesticides and related chemicals (see Appendices A and E) residues in barley, wheat, oats, rice and corn.
This standard is applicable to qualitative identification of 486 pesticides and related chemicals residues and quantitative determination of 376 pesticides and related chemicals residues in barley, wheat, oats, rice and corn.
For quantitative determination of 376 pesticides and related chemicals, method detection limit of this standard is 0.02μg/kg~0.96 mg/kg (see Appendix A).
2 Normative References
The following standards contain provisions which, through reference in this text, constitute provisions of this standard. For dated reference, subsequent amendments to (excluding correction to), or revisions of, any of these publications do not apply. However, the parties to agreements based on this standard are encouraged to investigate the possibility of applying the most recent editions of the standards. For undated references, the latest edition of the normative document referred to applies.
GB 549l Inspection of Grain and Oilseeds - Methods for Sampling and Sample Reduction
GB/T 6379.1 Accuracy (Trueness and Precision) of Measurement Methods and Results - Part 1: General Principles and Definitions
(GB/T 6379.1-2004, ISO 5725-1:1994,IDT)
GB/T 6379.2 Accuracy (Trueness and Precision) of Measurement Methods and Results - Part 2: Basic Method for the Determination of Repeatability and Reproducibility of a Standard Measurement Method (GB/T 6379.2-2004, ISO 5725-2:1994, IDT)
GB/T 6682 Water for Analytical Laboratory Use-Specification and Test Methods (GB/T 6682-2008, ISO 3696:1987, MOD)
3 Principles
Pesticides and related chemicals in the specimen is extracted by acetonitrile homogenization, purified by gel permeation chromatography, determined with LC-MS-MS, and quantified by external standard method.
Foreword I
1 Scope 1
2 Normative References 1
3 Principles 2
4 Reagents and Materials 2
5 Apparatus 3
6 Specimen Preparation and Storage 3
7 Determination Procedures 3
8 Calculation of Results 6
9 Precision 6
Appendix A (Informative) Table on English and Chinese Names, Method Detection Limit, Grouping, Solvent Selection and Concentration of Mixed Standard Solution for 486 Pesticides and Related Chemicals 7
Appendix B (Informative) Monitoring Ion Pair, Collision Gas Energy, Fragmentor in Source and Retention Time of 486 Pesticides and Related Chemicals 20
Appendix C (Informative) Multi-response Monitoring (MRM) Chromatogram of 486 Pesticides and Related Chemicals 35
Appendix D (Informative) Data Table on Precision of 486 Pesticides and Related Chemicals 36
Appendix E (Informative) Bilingual References of 486 Pesticides and Related Chemicals (in Alphabetical Order) 46