SN/T 0212.2-2017Determination of clopidol residues in poultry meat for export (English PDF)

Foreword

This part is the second part of SN/T 0212.

This part is drafted in accordance with the rules given in GB/T 1.1-2009.

This part replaces SN/T 0212.2-1993 "Test Method for Residue of Dichloropyridinol in Exported Poultry Meat (Gas Chromatography)".

The main changes in this section compared with SN/T 0212.2-1993 are as follows.

--- Modified the name of the standard;

--- Sampling steps are omitted;

--- Expanded the scope of detection of the original standard, adding chicken liver in addition to chicken;

--- Improve the derivatization method;

--- Replacement of gas chromatography by gas chromatography-mass spectrometry and gas chromatography tandem mass spectrometry.

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

This section drafted by. Shanghai Entry-Exit Inspection and Quarantine Bureau of the People's Republic of China.

1 Scope

This part of SN/T 0212 specifies gas chromatography-mass spectrometry and gas chromatography strings for diclofenac residues in poultry and liver.

Mass spectrometry.

This section applies to the determination of diclofenac residues in poultry and liver.

2 Method summary

The sample is extracted with dichloropyridinol from methanol, and the extract is purified by a neutral alumina column and catalyzed by pyridine under alkaline conditions.

Derived from propionic anhydride. It was determined by gas chromatography-mass spectrometry and gas chromatography tandem mass spectrometry and quantified by external standard method.

3 Reagents and materials

All reagents were of analytical grade and water was distilled water unless otherwise stated.

3.1 Methanol. Pure by liquid chromatography.

3.2 Hexane. Residual grade.

3.3 Pyridine.

3.4 Propionic anhydride. purity >= 98.0%.

3.5 sodium tetraborate.

3.6 0.1mol/L sodium tetraborate solution. Weigh 38.0g sodium tetraborate (3.5), dissolve it with water and dilute to 1000mL.

3.7 Alumina. neutral, for chromatography, particle size 100 mesh ~.200 mesh, burning at 300 ° C for 3 h, and baking in an oven at 130 ° C for 1 h, put Put it into the desiccator for use.

3.8 Dichloropyridinol standard substance. (Clopidol, C7H7Cl2NO, CAS No.. 2971-90-6), purity > 98%.

3.9 Dichloropyridinol standard stock solution. accurately weigh the appropriate amount of dichloropyridinol standard substance, and make 0.10mg/mL with methanol.

The standard stock solution was stored in the refrigerator at 4 ° C in the dark. The shelf life is 12 months.

3.10 Dichloropyridinol standard working solution. Dilute the standard solution of diclofenac (3.9) to a suitable concentration with methanol as needed.

The standard working solution is stored in a refrigerator at 4 ° C in the dark. The shelf life is 6 months.

4 Instruments and equipment

4.1 Gas Chromatography-Mass Spectrometer with EI source.

4.2 Gas Chromatography Tandem Mass Spectrometer with EI source.

4.3 Organize the mincer.

4.4 Homogenizer.

4.5 Centrifuge, 4000r/mim.

4.6 Vortex mixer.

4.7 Rotate the evaporator.

4.8 Nitrogen blowing instrument.