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SN/T 3149-2012: Determination of fentin and fenbutatin oxide residues and food for export. Gas chromatography-mass spectrometry method
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SN/T 3149-2012: Determination of fentin and fenbutatin oxide residues and food for export. Gas chromatography-mass spectrometry method

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Determination of fentin and fenbutatin oxide residues and food for export.Gas chromatography-mass spectrometry method People's Republic of China Entry-Exit Inspection and Quarantine Standards Triphenyltin food for export, fenbutatin Residue Detection Gas chromatography - mass spectrometry Issued on. 2012-05-07 2012-11-16 implementation People's Republic of China The State Administration of Quality Supervision, Inspection and Quarantine released

Foreword

This standard was drafted in accordance with GB/T 1.1-2009 given rules. Please note that some of the content of this document may involve patents. Distribution of this document Institutions do not assume the responsibility to identify these patents. This standard is proposed and managed by the National Certification and Accreditation Administration Committee. This standard was drafted. Tianjin People's Republic of China Exit Inspection and Quarantine. The main drafters of this standard. He Jia, Gao Jian will, Zhao Kung, Xiaoya Bing, Lin Anqing, Zhang Man, Xu Hong, Wu Yanhui, Zhang Jun. Triphenyltin food for export, fenbutatin Residue Detection Gas chromatography - mass spectrometry

1 Scope

This standard specifies the triphenyltin food for export and fenbutatin gas chromatography - mass spectrometry method. This standard applies to export apples, cabbage, green onions, tea, rice, soybeans, fish, pork, kidney, milk, eggs and triphenyltin phenylbutyrate Determination of tin residues and confirmation.

2 Method summary

Sample remaining triphenyltin and tributyltin in benzene under acidic extraction with acetone, and then the n-hexane liquid - liquid distribution, ethyl bromide derivative reagent , Generating ethyl triphenyl tin and tris (2-methyl-2-phenyl-propyl) ethyl tin, and then Florisil SPE column purification, eluent was concentrated After constant volume, gas chromatography - mass spectrometer and validation, external standard.

3 Reagents and materials

Unless otherwise specified, the reagents were of analytical grade, water is deionized water. 3.1 hydrobromide. 3.2 acetone. 3.3 n-hexane. Ethyl acetate 3.4. HPLC grade. 3.5 Cyclohexane. HPLC grade. 3.6 ethyl acetate - cyclohexane (11, volume ratio). exact amount of 500mL of ethyl acetate and 500mL of cyclohexane, after mixing for gel Chromatographic mobile phase. 3.7 anhydrous sodium sulfate. After burning 650 ℃ 4h, stored in a sealed container in the back. 3.8 sodium chloride. 3.9 3mol/L ethyl magnesium bromide solution in ether. 3.10 1mol/L hydrochloric acid solution. Take 20.8mL of concentrated hydrochloric acid, diluted with water to a 250mL volumetric flask. 3.11 acetone - n-hexane (12, volume ratio) solution. 3.12 hexane - diethyl ether (991 volume) was added. 3.13 triphenyltin standard (triphenyl tin, triphenyltinchloride, C18H15ClSn, CAS number. 639-58-7; triphenyl acetate Tin triphenyltinacetate C20H18O2Sn, CAS number. 900-95-8; triphenyltin hydroxide triphenyltinhydroxide, C18H16OSn, CAS number. 76-87-9). purity of greater than or equal to 98%. 3.14 fenbutatin standards (fenbutatinoxide, C60H78OSn2, CAS Number. 13356-08-6). purity of greater than or equal to 98%. 3.15 standard stock solution. accurately weigh the right amount of triphenyltin and fenbutatin standards were formulated with acetone to 100μg/mL standard Stock solution. Standard stock solution can be stored for 6 months at -18 ℃ condition. 3.16 standard working solution. Dilute into the corresponding standard working solution according to testing requirements with acetone. Standard liquid can be 0 ℃ ~ 4 ℃ 3 months under the conditions of storage. 3.17 Florisil SPE. 1g, 6mL or equivalent who filled in the column of about 1cm anhydrous sodium sulfate, previously living with 5mL n-hexane ...