1 Scope
This standard specifies the sample preparation method, the high-performance liquid chromatography (HPLC) method for testing and the liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS) method for confirmation for the determination of tetracyclines residues in food of animal origin.
This standard is applicable to the determination of 7 tetracyclines residues, namely minocycline, oxytetracycline, tetracycline, demeclocycline, chlortetracycline, methacycline and doxycycline, by the HPLC method, and that of 10 tetracyclines residues, namely minocycline, 4-epioxytetracycline, oxytetracycline, 4-epitetracycline, tetracycline, demeclocycline, 4-epichlortetracyc-line, chlortetracycline, methacycline and doxycycline, by the LC-MS/MS method, in food of animal origin such as animal muscle and offal, aquatic products and milk.
2 Normative reference
The following normative documents contain provisions which, through reference in this text, constitute provisions of this standard. For dated references, 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 latest editions of the standards indicated below. For undated references, the latest edition of the document referred to applies.
GB/T 6682 Water for analytical laboratory use - Specification and test methods (GB/T 6682-1992, neq ISO 3696:1987)
3 Principle
The residues of tetracycline antibiotics in the specimen are first extracted with 0.1mol/L Na2EDTA-Mcllvaine buffer solution (pH=4.0±0.05), and then filtered and centrifuged to obtain the supernatant which is purified by HLB solid phase extraction column, and determined by HPLC or liquid chromatography-electrospray-mass spectrometry (LC-ES-MS), and quantified by external standard peak area method.
1 Scope
2 Normative reference
3 Principle
4 Reagents and materials
5 Apparatus
6 Sample preparation and storage
7 Determination procedures
8 Blank test
9 Calculation and expression of results
10 Lower determination limit, recovery rate and precision
Annex A (Informative) Reference MS conditions
Annex B (Informative) Multi-reaction monitoring (MRM) chromatograms and liquid chromatograms
Annex C (Informative) Test data on recovery rate and precision of the methods
