SN 0706-1997Determination of naled residue in foodstuffs of animal origin for export (English PDF)

Foreword

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

This standard replaces SN 0706-1997 "naled residues in meat and meat products for export." this standard compared with SN 0706-1997, the main technical changes are as follows.

--- Standard name changed to "export food of animal origin in naled residues determination";

--- Suitable matrix detection range extended to pork, liver, chicken, beef, fish, pork and eggs, canned;

--- Remove the sampling part of the contents;

--- Modify the sample pre-treatment methods;

--- Gas Chromatography - Mass Spectrometry changed to liquid chromatography - mass spectrometry/mass spectrometry;

--- Given the limit of quantification and recovery of different methods.

Please note that some of the content of this document may involve patents. Release mechanism of the present document does not assume responsibility for the identification of these patents.

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

This standard was drafted. People's Republic of China, Xiamen Entry-Exit Inspection and Quarantine Bureau Technology Center.

1 Scope

This standard specifies the export of food of animal origin by gas chromatographic method naled residues and liquid chromatography - mass spectrometry/mass spectrometry confirmation method.

This standard applies to pork, liver, chicken, beef, fish, pork and eggs, canned naled residues in the detection and confirmation.

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 remaining naled extracted by ethyl acetate, frozen in addition to fat, determined by gas chromatography (GC-ECD), external standard liquid Chromatography - mass spectrometry/mass spectrometry (LC-MS/MS) for confirmation.

4 Reagents and materials

Unless otherwise stated, all reagents HPLC grade water to a water GB/T 6682 regulations.

4.1 methanol.

4.2 acetonitrile.

4.3 ethyl acetate.

4.4 formic acid.

4.5 anhydrous sodium. AR.

4.6 0.1% (volume fraction) solution of formic acid. amount of 1.0mL of formic acid water volume to 1000mL.

4.7 0.1% formic acid - acetonitrile (1 by volume ratio). Equal volumes of 0.1% formic acid and acetonitrile miscible.

4.8 Standard substance. naled (naled, CAS number. 300-76-5), molecular formula. C4H7Br2Cl2O4P, purity >=96.6%.

4.9 standard stock solution. accurately weighed amount naled standard material with methanol formulated into 100µg/mL standard solution 0 °C ~ 4 °C dark preservation, valid for one month.

4.10 standard solution. if necessary, prepared in methanol standard solution of different concentrations, using now.

4.11 matrix-matched standard solution. if necessary, with a blank sample extract obtained in accordance with the sample preparation step, preparation of different concentrations the matrix standard solution, using now.

4.12 0.22µm filter. aqueous phase the organic phase.

5 Instruments and equipment

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