SN 0639-1997Determination of linuron and its metabolite residues in meat and meat products for export. HPLC-MS/MS method (English PDF)

Foreword

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

This standard replaces SN 0639-1997 "export of meat and meat products linuron residues in." this standard compared with SN 0639-1997, the main technical changes are as follows.

--- Change the standard name, increasing the measured metabolites;

--- Expanding the scope of application of the matrix;

--- Remove the sampling part;

--- Change to gas chromatography liquid chromatography - mass spectrometry/mass spectrometry, lower detection limit.

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 Shanghai Entry-Exit Inspection and Quarantine Bureau.

1 Scope

This standard specifies the method for determination of export meat and meat products linuron and its metabolites (3,4-dichloro-aniline) residues.

This standard applies to exports of pork, kidney, liver, pork sausage, luncheon meat, sausages, meat and meat products linuron and its metabolite (3,4-dichloro-aniline) residual amount of liquid chromatography - mass spectrometry/mass spectrometry 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 linuron and its metabolite with acetone - acetonitrile extract, fat frozen at -18 °C refrigerator, extract mining with Florisil column purification, liquid chromatography - mass spectrometry/mass spectrometry and validation, internal standard.

4 Reagents and materials

Unless otherwise specified, use the analytical reagent, the water is deionized water.

4.1 acetonitrile. HPLC fractions.

4.2 acetone. HPLC fractions.

4.3 hexane. HPLC fractions.

4.4 ether. HPLC fractions.

4.5 formic acid. pure class distinctions, >=99%.

4.6 ammonium acetate.

4.7 acetone, acetonitrile (595, volume ratio). Measure 50mL and 950mL acetonitrile, acetone, and mix.

4.8 diethyl ether-hexane (19. volume ratio). Measure 100mL ether and 900mL hexane, and mix.

4.9 acetone and n-hexane (19. volume ratio). Measure 100mL acetone and 900mL hexane, and mix.

4.10 aqueous acetonitrile (11 volume). amount of 100mL of acetonitrile and 100mL of water, and mix.

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

4.12 containing 5mmol L ammonium acetate and water/0.1% formic acid. Weigh 385.4mg of ammonium acetate and 1mL acid dissolved in pure water and the volume to 1L.

4.13 Standard substances. linuron (Linuron, CAS number. 330-55-2), linuron isotope internal standard (Linuron-D6), 3,4- dichloro-aniline (3,4-Dichloroaniline, CAS number. 95-76-1); 3,4-dichloroaniline isotope internal standard (3,4-Dichloroaniline-2,6-D2), purity