SN 0195-1993Determination of 2, 4-D residues in meat and meat products for export. LC-MS/MS (English PDF)

Foreword

Accordance with the standards GB/T 1.1-2009. Drafting Rules "Standardization Guide Part 1 standard structure and preparation of" given.

This standard is SN 0195-1993 "export meat and meat products for 2,4-D residues in" amendments. Standardized text format Formula, increasing the "Normative references" and other standards for coding and related content. Some of the original standard text wording and text content it has been revised. This standard compared with SN 0195-1993 main changes are as follows.

--- Modify the standard Chinese name, the standard Chinese name to "export meat and meat products 2,4 Residues party Method by liquid chromatography - mass spectrometry/mass spectrometry ";

--- Re-enacted the lower limit of detection;

--- Liquid chromatography - mass spectrometry/mass spectrometry instead of the original standard gas chromatography;

--- Increased confirmatory methods.

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

This standard was drafted. Tianjin People's Republic of China Exit Inspection and Quarantine.

1 Scope

This standard specifies the export of meat and meat products for 2,4-D residues in sample preparation and liquid chromatography - mass spectrometry/mass spectrometry and confirmation methods.

This standard is applicable to the export of meat and meat products for the detection of residues of 2,4-D.

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

Under acidic conditions, extracted with dichloromethane tissue residues 2,4 and its sodium salt, and transferred to the lye. Washed with an organic solvent Fandi then acidified, 2,4-extracted with dichloromethane. After removing the solvent volume was dissolved in methanol for liquid chromatography - tandem mass spectrometry.

External standard.

4 Reagents and materials

Unless otherwise specified, reagents were of analytical grade, water GB/T 6682 provisions of ultrapure water.

4.1 Methanol. chromatographically pure.

4.2 dichloromethane.

4.3 ethanol.

4.4 anhydrous ether.

4.5 sulfuric acid - water (19). In excellent pure concentrated sulfuric acid formulation. After water (19) extracted twice with 50mL methylene chloride - sulfuric acid per 500mL spare.

4.6 Sodium hydroxide solution (30g/L). In excellent pure sodium hydroxide formulated. Each 500mL sodium hydroxide solution (30g/L) with two 25mL Chloride extracted twice after use.

4.7 Sodium chloride. pure class distinctions, each 250g of sodium chloride 100mL dichloromethane ultrasonic extraction twice, evaporated to dryness, burning at 600 °C 4h, storage in a stoppered bottle.

4.8 saturated sodium chloride solution. formulated with excellent pure sodium chloride. Each 250mL 25mL saturated sodium chloride solution twice extracted with methylene chloride Reserve.

4.9 2,4-D (2,4-D; CAS Number. 94-75-7) Standard. Purity >=99%.

4.10 2,4-standard solution. Weigh accurately 10mg2,4- drop standard (4.9) was dissolved in methanol (4.1) and dilute to 100mL, preparation to a concentration of 0.100mg/mL standard stock solution. Then progressively diluted with methanol to a standard working solution of appropriate concentration.

4.11 matrix extract. blank sample, after other operations resulting solution was treated with 7.1.

4.12 matrix standard solution. A standard solution (4.10) in dry nitrogen blowing instrument in order to extract the matrix was dissolved, after the vortex 30s