1 Scope
This standard specifies a method used to determine and confirm the residues of 10 aminoglycosides in animal tissues, such as spectinomycin, hygromycin B, dihydrostreptomycin, streptomycin, amikacin, kanamycin, apramycin, tobramycin, gentamicin and neomycin - High performance liquid chromatography - tandem mass spectrometry (HPLC-MS/MS).
This standard is applicable to the determination of residues of 10 aminoglycosides in animal innards, muscles and aquatic products.
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of this standard. For dated references, subsequent amendments (excluding corrections), or revisions, of any of these publications do not apply to this standard. However parties to agreements based on this standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative 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
Aminoglycosides residues in specimen are first extracted with phosphate buffer and then purified with a C18 solid phase extraction column, and after concentration, by using the heptafluorobutyric acid as the ion-pairing reagent, they are determined and quantified with HPLC-MS/MS method and external standard method respectively.
4 Reagents and materials
Unless otherwise specified, analytically-pure reagents and Grade-I water defined in GB/T 6682 shall be adopted.
4.1 Methanol: HPLC grade.
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents and materials
5 Instruments
6 Preparation and preservation of specimens
7 Determination procedures
8 Limit of quantitation (LOQ)
9 Recovery rate and precision
Annex A (Informative) Reference mass spectrometry conditions for MS/MS determination
Annex B (Informative) Reconstructed ion chromatogram of quantitative ion pairs of standard samples