OALib Journal期刊
ISSN: 2333-9721
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分散液-液微萃取-气相色谱-质谱法同时测定中毒样品中有毒生物碱和鼠药
DOI: 10.11895/j.issn.0253-3820.140815, PP. 282-287
Keywords: 分散液-液微萃取,生物碱,鼠药,气相色谱-质谱,同时测定
Abstract:
建立了分散液-液微萃取(Dispersiveliquid-liquidmicro-extraction,DLLME)与气相色谱-质谱(GC-MS)联用同时测定中毒样品中3种鼠药(毒鼠强、溴鼠灵、溴敌隆)和5种有毒生物碱(莨菪碱、东莨菪碱碱、钩吻碱、士的宁、马钱子碱)的方法.100μL萃取剂氯仿与600μL分散剂甲醇混合后,迅速注入样品,萃取过程在乳化体系中完成;以8000r/min离心5min,使两相分层,取下层有机相进行GC-MS分析.考察了萃取剂、分散剂的种类和体积、萃取时间、pH值及盐浓度对萃取效率的影响.在优化条件下,各目标物在水样、尿样、黄酒样的检出限为0.003~1.0μg/L,在米饭样品检出限为0.002~0.2μg/kg;各目标物低、中、高加标回收率为81.0%~110%,精密度均小于7%.本方法灵敏度高,快捷高效,适用于中毒样品中有毒生物碱和鼠药的同时测定.
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