SN/T 0527-2012Determination of methiocarb and its metabolite residues in cereals 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 0527-1996 "methiocarb residues in cereals for export." this standard compared with SN 0527-1996, the main technical changes are as follows.

--- Standard Scope extended to the brown rice, corn, rice, barley and wheat;

--- The methiocarb metabolites. methylthio Wia sulfone, methiocarb sulfoxide were measured;

--- Extracts to acetonitrile;

--- Omitted sampling procedure.

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, Shanghai Institute of Technical Supervision quality inspection.

1 Scope

This standard specifies the cereals for export methiocarb and metabolites (methylthio Avia methiocarb sulfoxide and sulfone) residual amount of liquid chromatography - mass spectrometry/mass spectrometry test methods.

This standard is applicable to the export of rice, corn, rice, barley and wheat methiocarb, sulfide sulfone and sulfoxide Avia Residues qualitative set Determination.

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

The sample was extracted with acetonitrile and residual methiocarb metabolite extract was dried over anhydrous magnesium sulfate and carbon graphite purified, concentrated, Liquid chromatography - mass spectrometry/mass spectrometry, external standard and quantitative.

4 Reagent material

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

4.1 acetonitrile. chromatography.

4.2 formic acid. Chromatographic pure.

4.3 Methanol. chromatographically pure.

4.4 ammonium formate. chromatography.

4.5 anhydrous magnesium. pure class distinctions.

4.6 acetonitrile solution (11 volume). Measure 50mL of water and 50mL of acetonitrile and mixed well.

4.7 20mmol/L ammonium formate solution (containing 0.1% formic acid). Accurately weigh 1.2612g ammonium formate, formic acid is added 1mL with water-soluble Solutions and transferred to 1000mL volumetric flask, dilute to the mark.

4.8 0.1% formic acid solution. 1mL acid is dissolved in water and dilute to 1L.

4.9 Pesticide Standards. methiocarb (Methiocarb, CAS number. 2032-65-1), methylthio Wia sulfone (Methiocarbsulfoxid, CAS no. 2635-10-1), methiocarb sulfoxide (Methiocarbsulfone, CAS number. 2179-25-1) were greater than 98% purity.

4.10 formulated standard stock solution. Weigh appropriate amount of reference material, respectively, prepared in methanol at a concentration of 100mg/L standard stock Solution. The solution was stored at -18 °C refrigerator. Valid for one month.

4.11 intermediate mixed standard solution preparation. accurately Pipette a certain volume of standard stock solutions were diluted to 10.0mg/L of methanol the intermediate mixed standard working solution. The solution should be formulated in a brown flask below -18 °C in the dark to save 5d.

4.12 preparation mixed standard working solution. Pipette appropriate amount of each intermediate mixed standard working solution, the solution was diluted with a blank sample matrix, so