SN 0707-1997Determination of dinitrocresol residues in foods for export. LC-MS/MS method (English PDF)

Foreword

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

This standard replaces SN 0707-1997 "export of meat and meat products dinitro-p-cresol residues in." this standard compared with SN 0707-1997 main changes are as follows.

--- Modify the standard Chinese name;

--- Original standard configuration has been modified;

--- By the scope of the standard increase of chicken meat, liver, beef, beef liver, beef kidney, rice, corn, wheat, soybeans, apples and Cabbage;

--- According to the major trading countries Dinitromethylene cresol limited demand re-enacted the lower limit of detection;

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

--- Increased confirmatory method.

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

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

1 Scope

This standard specifies the sample preparation HPLC food for export Dinitromethylene cresol and - mass spectrometry/mass spectrometry.

This standard applies to chicken, pork, liver, beef, beef liver, beef kidney, rice, corn, wheat, soybeans, apples and cabbage dinitro-p-cresol residues Determination of the amount of the stay and confirmed.

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

Dinitro-cresol in the sample residue with methanol - TCA extraction solution homogenized, after OasisHLB solid phase extraction (SPE), with liquid Chromatography - mass spectrometry/mass spectrometer, external standard.

4 Reagents and materials

Unless otherwise specified, the reagents were of analytical grade water as a water GB/T 6682 regulations.

4.1 acetonitrile. chromatography.

4.2 Methanol. chromatographically pure.

4.3 TCA.

4.4 trichloroacetic acid solution (10%). weigh 100.0g TCA, dissolved in water, and dilute to 1L.

4.5 -10% trichloroacetic acid solution in methanol (19 volume). amount of 900mL10% trichloroacetic acid solution (4.4), was added 100mL A Alcohol, and mix.

4.6 acetonitrile - water (28 volume). Measure 20mL of acetonitrile, was added 80mL of water, and mix.

4.7 Methanol - water (28 volume). Measure 20mL of methanol, was added 80mL of water, and mix.

4.8 dinitro-p-cresol standard substance. C7H6N2O5, CASN o.543-52-1, purity of greater than or equal to 99.0%.

4.9 standard stock solution. accurately weighed amount of reference material dinitro-p-cresol, preparation of standard stock with acetonitrile to a concentration of 1000µg/mL of Preparation of the solution, 0 °C ~ 4 °C stored in a refrigerator for a period of six months.

4.10 standard solution. Standard stock solution Pipette a volume of accurate, if necessary with acetonitrile - a dilute aqueous solution (4.6) to the appropriate concentration Standard working solution degrees, 0 °C ~ 4 °C stored in a refrigerator for a period of one month.

4.11 OasisHLB solid phase extraction (SPE) columns. 60mg, 3mL or performance are quite. Before using successively with methanol and 1mL, 3mL water activation.

4.12 microporous membrane. 0.22µm, organic.