SN/T 0212.1-2014Determination of clopidol residues in foodstuffs of animal origin for export (English PDF)

Foreword

SN/T 0212 is divided into 3 parts.

--- Part 1. Determination of residual amount of dichloropyridinol in foods for export of animals;

--- Part 2. Method for the determination of dichloropyridinol residues in poultry meat - methyl - gas chromatography;

--- Part 3. Determination of dichloropyridinol residues in poultry meat - Propionylation - gas chromatography.

This part is the first 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 0212.1-1993 "Liquid chromatography method for the determination of diclofenac in export poultry meat", and Compared with SN/T 0212.1-1993, the main changes are as follows.

---Modified the name of the standard;

--- The scope of application is increased from frozen chicken to chicken, pork, beef, fish, chicken liver, chicken kidney, chicken feet, eggs and milk;

--- The original standard liquid chromatography was determined as the first method of this standard;

--- Added second method liquid chromatography-mass spectrometry/mass spectrometry;

--- Added Appendix A (informative appendix) "High Performance Liquid Chromatogram of Dichloropyridinol Standard Solution".

1 Scope

This part of SN/T 0212 specifies the method for determining the amount of diclofenac residue in animal-derived foods.

This part of the first method of liquid chromatography is suitable for the determination of residual amount of dichloropyridinol in frozen chicken, the second method liquid chromatography-mass spectrometry the method is applicable to the determination of dichloropyridinol residues in chicken, pork, beef, fish, chicken liver, chicken kidney, chicken feet, eggs and milk.

2 Normative references

The following documents are indispensable for the application of this document. For dated references, only dated versions apply to this article.

Pieces. For undated references, the latest edition (including all amendments) applies to this document.

GB/T 6682 Analytical laboratory water specifications and test methods First method liquid chromatography

3 Method summary

The dichloropyridinol in the sample is extracted with acetonitrile, purified by alumina column and anion exchange column, and dichloroform is determined by liquid chromatography.

The residual amount of pyridinol was quantified by external standard method.

4 Reagents and materials

Reagents and materials Unless otherwise specified, all reagents are of analytical grade and water is the first grade water in accordance with GB/T 6682.

4.1 Acetonitrile. liquid chromatography grade.

4.2 Methanol. liquid chromatography grade.

4.3 Sodium acetate aqueous solution (100g/L). Weigh 100.0g of sodium acetate in a 1000mL volumetric flask, dissolve it in water and dilute to volume, mix After mixing, spare.

4.4 acetic acid methanol solution (0.25%). accurately transfer 0.25mL of acetic acid in a 100mL volumetric flask, dissolve it with methanol and dilute to volume.

Mix and reserve.

4.5 acetic acid methanol solution (0.5%). accurately transfer 0.5mL of acetic acid in a 100mL volumetric flask, dissolve it with methanol and dilute to volume, mix After mixing, spare.

4.6 Saturated silver nitrate acetone solution.

4.7 anhydrous sodium sulfate. 650 ° C burning for 4h, stored in a sealed bottle.

4.8 Alumina. For chromatography, neutral, 70 mesh to 230 mesh.

4.9 Anion exchange resin. Dowex 1-X8, 100 mesh ~.200 mesh, chloride ion type. Conversion to the acetate form was carried out as follows before use.

Immerse 100g of Dowex1-X8 resin in 100g/L sodium acetate aqueous solution, stir it from time to time, soak for 2h, then pour into the Buchner funnel, use 500mL 100g/L sodium acetate aqueous solution (4.3) was rinsed to only trace amounts of chloride ions (tested with saturated silver nitrate acetone solution, slightly turbid)