SN 0663-1997Determination of heptachlor, heptachlor epoxide residues in meats and meat products for export (English PDF)

Foreword

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

This standard replaces SN 0663-1997 "heptachlor and heptachlor epoxide residues in meat and meat products for export." this standard compared with SN 0663-1997 main changes are as follows.

--- Modify the standard name. the "export of meat and meat products for heptachlor and heptachlor epoxide residues in" to "export meat and meat Products in the heptachlor and heptachlor epoxide residues in the determination ";

--- Standard Scope increased beef, chicken, ham, sausage;

--- Original standard "2 sampling and sample preparation" to "6 Sample preparation and preservation";

--- Modify the original standard sample preparation method. the chromatography column to the commercialization of solid-phase extraction column, an increase of gel permeation chromatography (GPC) Purification;

--- Increased by Gas Chromatography - Mass Spectrometry.

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

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

1 Scope

This standard specifies the method for determination of export meat and meat products heptachlor and heptachlor epoxide residues.

This standard applies to pork, beef, chicken, ham, sausage of heptachlor and heptachlor epoxide measured residues.

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 of heptachlor and heptachlor epoxide residues with acetone - hexane extract, the extract by gel permeation chromatography (GPC) to remove the oil, then by After the solid-phase extraction (SPE), gas phase chromatography and gas chromatography - mass spectrometry confirmed, external standard.

4 Reagents and materials

Except where noted, all reagents were of analytical grade water as a water GB/T 6682 regulations.

4.1 acetone. HPLC grade.

4.2 hexane. HPLC grade.

4.3 Cyclohexane. HPLC grade.

Ethyl acetate 4.4. HPLC grade.

4.5 anhydrous sodium. 650 °C burning 4h, store in a sealed container in the back.

4.6 acetone - n-hexane (28 volume). Measure 20mL acetone and 80mL hexane, and mix.

4.7 ethyl acetate - cyclohexane (11 volume). amount of 500mL ethyl acetate and 500mL of cyclohexane, and mix.

4.8 ethyl acetate - n-hexane (19 volume). the amount of 10mL and 90mL ethyl acetate, n-hexane, and mix.

4.9 Standard. heptachlor, epoxide A and B were heptachlor epoxide purity not less than 98.0%, see Appendix A in Table A.1.

4.10 standard stock solution. 100mg/L, respectively accurately weighed take 10mg heptachlor standard substance, heptachlor epoxide A, B heptachlor epoxide in 100mL Flask, and were dissolved with n-hexane to volume. The following 4 °C dark preservation, valid for one year.

4.11 standard mixed solution. Pipette appropriate amount of each stock standard solution (4.10) and diluted with n-hexane for the component concentration of 1mg mixed/L of Intermediate standard solution. 4 °C stored.

4.12 SPE. Florisil column (1000mg, 6mL), or equivalent person. 5mL n-hexane before use activation.

4.13 microporous membrane. 0.45µm, organic.

5 Apparatus

5.1 Gas chromatograph. with electron capture detector (ECD).