超高效液相色谱-串联质谱法测定水稻中咪鲜胺的残留总量

Determination of the total residue of prochloraz in rice by UPLC-MS/MS

建立超高效液相色谱-串联质谱检测水稻中咪鲜胺残留总量的方法。水稻糙米、稻壳、秸秆样品采用乙腈提取,基质分散固相萃取净化,高温条件下盐酸吡啶催化生成2,4,6-三氯苯酚,经XR-ODSⅢ C_(18)超高效液相色谱柱分离,基质外标法定量。试验结果表明,在添加水平为0.05~5 mg/kg时,咪鲜胺的添加回收率为70%~84%,相对标准偏差为0~4.6%。方法的定量限(LOQ)为0.05 mg/kg。方法操作简便、精确、高效,适用于水稻样品中咪鲜胺农药残留的快速筛查和定量检测。

A method to determinate the residues of prochloraz and its metabolites in rice were established by UPLC-MS/MS.The samples of brown rice,rice husk and straw were extracted with acetonitrile,purified by matrix dispersion solid phase extraction.Then at the high temperture,prochloraz reacted with pyridine hydrochloride to generate 2,4,6-trichlorophenol,the analytes were separated on XR-ODSⅢ C_(18) column,and quantified by an external standard method.The results indicated that the recoveries of prochloraz were 70%-84%,the relative standard deviations were 0-4.6%,at the adding level of 0.05-5 mg/kg.The limit of quantitation(LOQ)of prochloraz was 0.05 mg/kg.The method was simple,accurate,and suitable for quantitative detection of prochloraz and its metabolites in rice.