1 Scope
This Standard specifies determination for the residues of furaltadon metabolite (5-morpholine methyl-3-amino-2-oxazole alkyl ketone, abbreviated to AMOZ), nitrofurazone metabolite (semicarbazide, abbreviated to SEM), nitrofurantoin metabolite (1-amino-2-glydant, abbreviated to AHD) and furazolidone metabolite (3-amino-2-oxazole alkyl ketone, abbreviated to AOZ) in milk and milk powder-LC-MS-MS method.
This Standard applies to the determination of residues of AMOZ, SEM, AHD and AOZ in milk and milk powder.
Detection limits in the methods of this Standard: 0.2 μg/kg for AMOZ, SEM, AHD and AOZ in milk while 1.6 μg/kg for those in milk powder.
Note: the English and Chinese names as well as the English abbreviations of furaltadon, nitrofurazone, nitrofurantoin and furazolidone refer to Appendix A in Table A .1 of this Standard.
2 Normative References
The following documents contain provisions which, through reference in this text, constitute provisions of this Standard. For dated reference, subsequent amendments to (excluding any corrigendum), or revisions of, any of these publications do not apply. However, parties to agreements based on this Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. For any undated references, the latest edition of the document referred to applies.
GB/T 6379.1 Accuracy (Trueness and Precision) of Measurement Methods and Results - Part 1: General Principles and Definition(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, IS0 3696:1987, MOD)
3 Principle
The specimen of milk or milk powder is hydrolyzed with trichloroacetic acid and removed of protein, and the nitrofurans metabolite is subjected to derivatization with 2-nitrobenzaldehyde and purification with Oasis HLB or solid-phase extraction column with equivalent property in acidic condition. Detected by means of LC-MS-MS(ESI +) and quantified via internal or external standard method.
1 Scope
2 Normative References
3 Principle
4 Reagents and Materials
5 Apparatus
6 Preparation and Preservation of Specimen
7 Determination Procedures
8 Result Calculation
9 Precision
Appendix A (Informative) English/Chinese Names and English Abbreviations for Four Species of Nitrofurans and Metabolites
Appendix B (Informative) Multi-response Monitoring (MRM) Chromatogram
Appendix C (Informative) Recovery Rate
