液相色谱-串联质谱同时检测水稻样品中乙基多杀菌素及其代谢物残留  

Simultaneous determination of spinetoram and its metabolites in rice using liquid chromatography-tandem mass spectrometry

作　　者：傅强[1] 黄颖婕 付启明[1] 梁骥[1] 马婧 冯雪 李双双 

机构地区：[1]湖南化工研究院国家农药创制工程技术研究中心湖南加法检测有限公司,长沙410014 [2]湖南师范大学附属中学,长沙410006 [3]湖南人文科技学院,湖南娄底417000

出　　处：《农药学学报》2017年第5期631-637,共7页Chinese Journal of Pesticide Science

基　　金：农业部农药残留安全评价项目(2014P043)

摘　　要：采用液相色谱-串联质谱(LC-MS/MS)技术建立了同时检测水稻植株、谷壳、糙米中乙基多杀菌素及其代谢物N-demethyl-175-J和N-formyl-175-J残留的分析方法。样品采用乙腈提取,经分散固相萃取(PSA)净化,LC-MS/MS检测。结果表明:在0.02、0.2和2 mg/kg添加水平下,乙基多杀菌素及其代谢物的平均回收率在73%~105%之间,相对标准偏差(RSD)在0.9%~10%之间。乙基多杀菌素-J和-L的定量限(LOQ)分别0.016和0.004 mg/kg,代谢物的定量限(LOQ)为0.02 mg/kg。该方法操作简便、稳定和快速,可以满足水稻样品中乙基多杀菌素及其代谢物的定性与定量分析要求。A method was developed for simultaneous determination of spinetoram and its metabolites residues in rice samples using liquid chromatography-tandem mass spectrometry （LC-MS/MS）. Samples were extracted with acetonitrile. After clean up with PSA, the analyte was analyzed using LC- MS/MS. The results showed that the average recoveries varied from 73% to 105% at spiked levels of 0.02, 0.2 and 2 mg/kg for all the analyte. The relative standard deviations （RSD） varied from 0.9% to 10%. The limits of quantification （LOQ） （based on the recovery test） of spinetoram-J and spinetoram-L were 0.016 mg/kg and 0.004 mg/kg, respectively. The LOQ of spinetoram＇s metabolites were 0.02 mg/kg. As the method developed in this work is convenient, rapid and reliable, it can be applied in the qualitative and quantitative analyses of residues of spinetoram and its metabolite in rice samples.

关 键 词：液相色谱-串联质谱 水稻 乙基多杀菌素 代谢物 残留 

分 类 号：S482.2[农业科学—农药学] TQ450.263[农业科学—植物保护]