SN/T 0605-2012Determination of bitertanol 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 0605-1996 "cereals for export double oxacillin alcohol residues in bacteria." this standard compared with SN 0605-1996, the main technical changes are as follows.

--- Change the standard name;

--- Remove the sampling part;

Change --- Gas chromatography is liquid chromatography - mass spectrometry/mass spectrometry, lower detection limit;

--- Modify the pre-treatment 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 Shanghai Entry-Exit Inspection and Quarantine Bureau.

1 Scope

This standard specifies the method for determination of cereals for export bacteria double oxacillin alcohol residues.

This standard applies to exports of rice, corn, barley, wheat, buckwheat, rice, sorghum, oats bacteria double oxacillin alcohol residues LC -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

Samples were extracted with acetonitrile, the amino (NH2) solid phase extraction (SPE) for liquid chromatography - mass spectrometry/mass spectrometer, external standard.

4 Reagent material

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

4.1 acetonitrile. high performance liquid chromatography.

4.2 Methanol. HPLC grade.

4.3 acetone. HPLC fractions.

4.4 sodium chloride.

4.5 anhydrous magnesium sulfate.

4.6 formic acid, the purity of >=99%.

4.7 aqueous acetonitrile. water - acetonitrile (91, volume ratio).

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

4.9 pesticide standards materials. double oxacillin alcohol standard bacteria (bitertanol, CAS number. 55179-31-2, molecular formula. C20H23N3O2). Pure Degree >=98.0%.

4.10 Standard stock solution preparation. Accurately weigh an appropriate amount of bacteria double oxacillin alcohol standards, formulated with acetonitrile to a concentration of 1.0mg/mL standard Quasi stock solution. The solution was stored at -18 °C refrigerator for a period of 12 months.

4.11 intermediate standard solution preparation. diluted with acetonitrile standard stock solution to a final concentration of about 1.0µg/mL, less than 4 °C dark refrigerated Save for a period of six months.

4.12 matrix formulated standard working solution. If necessary, draw temporary use when a certain amount of standard intermediate solution, formulated with a matrix blank solution an appropriate concentration of the working standard solution. Refrigerated below 4 °C dark, using now.

4.13 amino (NH2) SPE column. SUPELCOLC-NH23mL (filler 500mg), or equivalent person. Before use with 10mL acetonitrile activation.