SN 0660-1997Determination of propargite reduce in cereals for export (English PDF)

Foreword

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

This standard replaces SN 0660-1997 "export grain mite residue test method." this standard compared with SN 0660-1997, the main technical changes are as follows.

--- The standard name was revised from "Method for the determination of propargite residues in cereals for export" to "Determination of residues of propargite in cereals for export";

--- To expand the scope of application of standard testing;

--- Cut down the sampling part;

--- Improved sample preparation technology;

--- Added LC-MS confirmation method;

--- Reduce the detection limit, and for different test objects, given the different matrix to add different reference substance concentration recovery range.

Please note that some of this document may be patentable. The issuing agencies of this document do not bear the responsibility of identifying these patents.

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

1 Scope

This standard specifies the export of cereal residues in the amount of propargite gas chromatography and liquid chromatography/mass spectrometry/mass spectrometry method.

This standard applies to the determination of the export of wheat, barley, rice, soybeans, corn residues in mites.

2 Normative references

The following documents for the application of this document is essential. For dated references, only the dated version applies to this article Pieces. For undated references, the latest edition (including all amendments) applies to this document.

GB/T 6682 analytical laboratory water specifications and test methods the first method of gas chromatography

3 Method summary

Samples were soaked in water, extracted with acetonitrile by ultrasonic extraction, sodium chloride was added for liquid-liquid extraction, the acetonitrile layer was dried over anhydrous sodium sulfate and concentrated C18 cartridge purification, evaporated and evaporated to dryness with n-hexane 5mL dissolved, and then Fuli silica column purification, the eluent was concentrated to near dry, with acetone Solve the volume, microporous membrane, flame photometric detector (sulfur filter) test.

4 Reagents and materials

Unless otherwise specified, all reagents are analytical reagents, water GB/T 6682 provides a water.

4.1 Acetonitrile. Chromatographic purity.

4.2 n-hexane. Chromatographic purity.

4.3 Ethyl acetate. Chromatographic purity.

4.4 acetone. Chromatography pure.

4.5 sodium chloride.

4.6 anhydrous sodium sulfate, burning at 620 °C 4h, cooled and stored in a glass dryer spare.

4.7 Florisil. Chromatography, 150µm ~ 250µm (60 mesh ~ 100 mesh), burning at 620 °C 4h, after cooling was added 5% water Activation, stored in a glass dryer spare.

4.8 n-hexane - ethyl acetate solution (95 5) were measured 950mL n-hexane and 50mL ethyl acetate, and mix well.

4.9 C18 SPE column. LC-C18 column (2000 mg/12 mL), or equivalent. Before use need to activate with 10mL acetonitrile, keep the cylinder moist.

4.10 Standard. Propargite, CAS No. 2312-35-8, molecular formula. C19H26O4S, standard substance purity >= 99.9%.

4.11 standard stock solution accurately weighed 50.0mg propargite standard (accurate to 0.1mg) in 50mL volumetric flask, with acetonitrile Made of 1.0mg/mL standard stock solution, 0 °C ~ 4 °C preservation, can be used for 1 year.

4.12 standard working solution.After dilution with acetone according to the need to prepare the appropriate concentration of standard working solution, is now available with.