SN/T 1751.3-2011Determination of quinolone residues in foodstuffs of animal origin for import and export. Part 3: HPLC method (English PDF)

Foreword

SN/T 1751 "Determination of the import and export food of animal origin quinolones residues" is divided into three parts.

--- Part 1. Microbiological inhibition assay;

--- Part 2. liquid chromatography - mass spectrometry/mass spectrometry;

--- Part 3. High Performance Liquid Chromatography.

This section SN/T 1751 Part 3.

This section drafted in accordance with GB/T 1.1-2009 given rules.

Please note that some of the content of this document may involve patents. Release mechanism of the present document does not assume responsibility for the identification of these patents.

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

This section drafted by. China Inspection and Quarantine Science Research Institute, People's Republic of China and East Nanjing Exit Inspection and Quarantine of the People's co Exit Inspection and Quarantine and the Mongolia.

1 Scope

SN/T 1751 This section provides the high performance liquid chromatographic method foods of animal origin of 15 quinolone residues.

This section applies to shrimp, fish, chicken and milk powder ciprofloxacin, Dan Nuosha star, enrofloxacin, sarafloxacin, flumequine, promise fluorine sand Xing, Difloxacin, marbofloxacin, quinoline acid, nalidixic acid, pefloxacin, sparfloxacin, Orbifloxacin, fleroxacin and lomefloxacin Residues Determination.

2 Normative references

The following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein Member. For undated references, the latest edition (including any amendments) applies to this document.

Laboratory use specifications and test methods GB/T 6682 Analysis

3 Method summary

Sample extraction residues quinolone with phosphate buffer, and acetonitrile, dried hexane to remove grease, C18 solid phase extraction and MAX After the column purification by high performance liquid chromatography - fluorescence detector and ultraviolet detector and quantified by external standard.

4 Reagents and materials

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

4.1 acetonitrile. chromatography.

4.2 Methanol. chromatographically pure.

4.3 hexane. chromatographically pure.

4.4 sodium phosphate dodecahydrate.

4.5 sodium hydroxide.

4.6 phosphoric acid.

4.7 25% aqueous ammonia.

4.8 formic acid.

4.9 acetonitrile saturated n-hexane solution. 100mL acetonitrile (4.1) was added to 100mL of n-hexane (4.3), followed by sufficient shaking, standing stratification, Supernatant liquid.

4.10 0.02mol/L phosphate solution. accurately measure 1.4mL phosphoric acid (4.6) in 1L flask, water volume to 1L.

4.11 5mol/L sodium hydroxide solution. Weigh 200g of sodium hydroxide (4.5) dissolved in water and dilute to 1L.

4.12 sodium phosphate buffer solution (50mmol/L, pH7.4 ± 0.2). Weigh 19g sodium phosphate dodecahydrate (4.4), dissolved in water and constant volume to 1L, add phosphoric acid to adjust the pH to 7.4 ± 0.2.

4.13 Sample extracts. 180mL phosphate buffer solution (4.12) was added to 20mL of acetonitrile.

4.14 eluent 1. Take 25mL25% aqueous ammonia (4.7), was added 75mL of methanol (4.2).