SN/T 2113-2008Determination of residues of tranquillizer drugs in animal-origin foodstuffs for import and export. LC-MS/MS method (English PDF)

Foreword

The Standard Appendix A and Appendix B are informative.

This standard is proposed and managed by the National Certification and Accreditation Administration Committee.

This standard by the People's Republic of China Shanghai Exit Inspection and Quarantine is responsible for drafting.

1 Scope

This standard specifies the import and export of animal-derived foods chlorpromazine and diazepam two kinds of sedative drugs residues in sample preparation and liquid Chromatography - mass spectrometry/mass spectrometry method for the quantitative determination and qualitative confirmation.

This standard applies to meat, chlorpromazine and diazepam determination of drug residues in the kidneys.

2 Normative references

The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard.

GB/T 6682 analytical laboratory use specifications and test methods (GB/T 6682-2008, ISO 3696. 1987, MOD)

3 Preparation and Storage of samples

3.1 meat samples. Remove all the samples taken from a representative sample of about 500g, crushed with a grinder, mixed, were divided into two, respectively as a sample into a clean container, sealed and marked with tags, the specimen was stored at -18 °C refrigerator.

3.2 Kidney. Remove all the samples taken from a representative sample of about 100g, remove the medulla, crushed with a grinder, mixed, were divided Two, respectively, into a clean container as a sample, and sealed and labeled, the specimen was stored at -18 °C refrigerator.

3.3 In the sample preparation procedure, it should be protected from light as much as possible and to prevent sample contamination or the occurrence of the change of residue content.

4 Method summary

After the sample is added D6- chlorpromazine as an internal standard and extracted with acetonitrile extract was diluted with 20% sodium chloride solution, aqueous sulfuric acid tone to pH 4.8 ~ 5.0, OASISHLB SPE column purification, after concentrating by high performance liquid chromatography/tandem mass spectrometry, within Standard method.

5 Reagents and materials

Unless otherwise specified, all reagents were of analytical grade water as a water GB/T 6682 regulations.

5.1 acetonitrile. HPLC fractions.

5.2 Methanol. HPLC fractions.

5.3 formic acid. HPLC fractions.

5.4 ammonium acetate.

5.5 sodium chloride.

5.6 aqueous sulfuric acid solution. 0.05mol/L and 0.01mol/L.

5.7 acidic acetonitrile. Join 5mL0.05mol/L sulfuric acid solution in 100mL acetonitrile.

5.8 20% aqueous sodium chloride solution. 20g in 100mL of water was added sodium chloride.

5.9 Mobile phase A. 1000mL Acetonitrile taken, formic acid was added 1.0mL, ultrasonic mixing.

5.10 Mobile phase B. Weigh 0.154g of ammonium acetate was added 1.0mL of formic acid, dissolved in water and dilute to 1000mL, ultrasonic mixing.

5.11 SPE cartridges. OASISHLB, 500mg, 6mL, or equivalent person.