| 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 |
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| 引用本文： | 傅强,黄颖婕,付启明,梁骥,马婧,冯雪,李双双.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[J].农药学学报,2017,19(5):631-637. |
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| 作者姓名： | 傅强 黄颖婕 付启明 梁骥 马婧 冯雪 李双双 |
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| 作者单位： | 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 |
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| 基金项目： | 农业部农药残留安全评价项目（2014P043） |
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| 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。
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| 关 键 词： | 液相色谱-串联质谱 水稻 乙基多杀菌素 代谢物 残留 |
| 收稿时间： | 2017/6/16 0:00:00 |
Simultaneous determination of spinetoram and its metabolites in rice using liquid chromatography-tandem mass spectrometry |
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| FU Qiang,HUANG Yingjie,FU Qiming,LIANG Ji,MA Jing,FENG Xue and LI Shuangshuang.Simultaneous determination of spinetoram and its metabolites in rice using liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Pesticide Science,2017,19(5):631-637. |
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| Authors: | FU Qiang HUANG Yingjie FU Qiming LIANG Ji MA Jing FENG Xue and LI Shuangshuang |
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| Institution: | 1.National Engineering Center for Agrochemicals, Hunan Research Institute of Chemical Industry, Hunan J & F Test Co., Ltd. Changsha 410014, Hunan Province, China2.The High School Attached to Hunan Normal University, Changsha 410006, Hunan Province, China3.Hunan University of Humanities, Science and Technology, Loudi 417000, Hunan Province, China |
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| Abstract: | 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. |
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| Keywords: | liquid chromatography-tandem mass spectrometry(LC-MS/MS) rice spinetoram metabolite residue |
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