分散液液微萃取-反萃取-接受相固化-高效液相色谱法测定减肥茶中的西布曲明  

Determination of Sibutramine in Dietic Teas by Dispersive Liquid-Liquid Microextraction-Back Extraction-Solidification of Acceptor PhaseHigh Performance Liquid Chromatography

作　　者：石慧[1] 夏丹[1] 邓晓庆[1] 谭月明[1] 苏孝礼[1] 谢青季[1] 马铭[1] 

机构地区：[1]化学生物学及中药分析教育部重点实验室,湖南师范大学,长沙410081

出　　处：《分析化学》2013年第9期1444-1448,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(Nos.21275052;21175042);湖南省高校科技创新团队支持计划资助项目

摘　　要：建立了分散液液微萃取-反萃取-接受相固化与高效液相色谱联用测定减肥茶中西布曲明的方法。优化的条件为:400"L石油醚为萃取剂、120"L甲醇为分散剂、14"L 0.2 mol/L HCl溶液和1"L甲醇的混合溶液为接受相,萃取2 min。在优化条件下西布曲明的富集因子可达130倍。方法的线性范围为0.6～200"g/L,检测出限为0.2"g/L,定量限为0.6"g/L。样品加标回收率介于91.9%～108.4%,日间相对标准偏差小于14%。A novel method for the determination of sibutramine in dietic teas by dispersive liquid-liquid microextraction-back extraction-solidification of acceptor phase（DLLME-BE-SAP）-high performance liquid chromatography was developed.The optimal experimental conditions were as follows： 400 μL petroleum ether as the organic phase,120 μL methanol as the dispersive solvent,the mixture of 14 μL of 0.2 mol/L HCl and 1 μL methanol as the acceptor phase.The extraction time was 2 min.High enrichment factor（130-fold） of sibutramine was obtained under the optimal experimental conditions.The linear range was 0.6-200 μg/L.The limit of detection（S/N=3） was 0.2 μg/L and the limit of quantitation（S/N=10） was 0.6 μg/L.The recoveries of the spiked samples were from 91.9% to 108.4%,and the inter-day relative standard deviations were lower than 14.0%.

关 键 词：分散液液微萃取-反萃取-接受相固化 高效液相色谱 西布曲明 

分 类 号：TS272.7[农业科学—茶叶生产加工] O657.72[轻工技术与工程—农产品加工及贮藏工程]