SN 0692-1997Determination of strobane residues in meats and meat products for export. CC-MS method (English PDF)

Foreword

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

This standard replaces SN 0692-1997 "turpentine chloride residues in meat and meat products for export." this standard compared with SN 0692-1997, the main changes are as follows.

--- Abolition of the "sampling and sample preparation," adds "Sample Preparation and Storage" (see Chapter 5, Chapter 2, 1997 edition);

--- Sample extraction by the Soxhlet extraction method to extract high-speed vortex (see 61, 1997 version 3.4.1.);

--- Sample purification method consists of two sulfonated gel permeation purification to purify (see 62, 1997 edition of 3.4.2 and 3.4.4.);

--- Canceled the step of sample extract in methanol was added a solution of potassium hydroxide dehydrochlorination (see the 1997 version 3.4.3);

--- Determination by gas chromatography to gas chromatography - mass spectrometry (see 63, 1997 edition of 3.4.5.);

--- Quantitative methods limit the 0.2mg/kg amended to 0.01mg/kg (see 7.1, 4.1, 1997).

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

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

1 Scope

This standard specifies the export of meat and meat products turpentine chloride gas chromatography - mass spectrometry method.

This standard applies to pork, beef, lamb, chicken, bacon and floss in determining the amount of residual chloride, turpentine and confirmation.

2 Method summary

Sample chlorination residual turpentine using n-hexane-speed vortex extraction, gel permeation purification eluate was concentrated and volume for Gas chromatography - mass spectrometer and validation, external standard.

3 Reagents and materials

Unless otherwise specified, all reagents were of analytical grade, water is distilled water.

3.1 hexane. redistilled.

3.2 sodium chloride.

3.3 anhydrous sodium sulfate. After burning 650 °C 4h, the dryer use.

3.4 ethyl acetate.

3.5 cyclohexane.

3.6 cyclohexane - ethyl acetate solution (11 volume). Ethyl acetate (3.4), and cyclohexane (3.5) mixed in equal volumes.

3.7 turpentine chloride pesticide standards (Strobane, C10H9Cl7, CAS. 8001-50-1). 99.5% purity.

3.8 standard stock solution. Weigh accurately 50mg turpentine chloride pesticide standards (accurate to 0.1mg) in 50mL brown volumetric flask with N-hexane (3.1) and dissolve to volume, shake, formulated to a concentration of 1000µg/mL standard stock solution. Standard stock solution at 0 °C ~ 4 °C stored.

3.9 standard intermediate solution. Imbibe 1.0mL standard stock solution in 100mL brown volumetric flask, dissolve and n-hexane (3.1) to volume, formulated at a concentration of 10µg/mL standard intermediate solution. Intermediate standard solution was stored at 0 °C ~ 4 °C in the dark.

3.10 standard solution. intermediate standard solution Pipette a volume of serially diluted to the appropriate concentration of the working standard solution based on testing needs liquid. Standard working solution should be now with the current.

4 Instruments and equipment

4.1 Gas chromatography - mass spectrometry with chemical ionization (CI source).

4.2 Organization mashed machines.

4.3 Vortex device.

4.4 gel permeation chromatography.

4.5 nitrogen blowing instrument.

4.6 rotary evaporator.

4.7 high-speed centrifuge. 10000r/min.