超声波提取-气相色谱-质谱法测定紫菜中甲基锡及乙基锡  

Simultaneous determination of three organotin compounds in laver by gas chromatography-mass spectrometry

作　　者：周慧云[1] 柳英霞[2] 鄢爱平[2] 谭婷[2] 

机构地区：[1]南昌广播电视大学,江西南昌330003 [2]南昌大学分析测试中心,江西南昌330047

出　　处：《南昌大学学报（理科版）》2014年第6期585-589,共5页Journal of Nanchang University(Natural Science)

基　　金：国家自然科学基金资助项目(20965005);江西省科技支撑计划基金资助项目(2008BB22400);南昌大学食品科学与技术国家重点实验室目标导向基金资助项目(SKLF-MB-201002);南昌大学食品科学与技术国家重点实验室自由探索基金资助项目(SKLF-TS-200918)

摘　　要：建立了紫菜中二甲基锡、三甲基锡和三乙基锡的同时检测新方法。紫菜样品经过超声波辅助提取,采用四乙基硼酸钠对紫菜样品提取液中的有机锡化合物进行衍生后,经活性炭净化,运用气相色谱-质谱法（GC-MS）进行分析。在优化条件下,3种有机锡化合物在0.02-2.5 mg·L^-1的范围内得获得了较好的线性,检测限分别为0.004 3、0.003 8和0.002 6mg·L^-1,其相关系数分别为0.998 0、0.999 1和0.998 5。二甲基锡、三甲基锡和三乙基锡在0.05、0.50和2.0 mg·L^-1 3个添加水平的平均回收率为72.6%-95.7%,相对标准偏差为5.14%-9.26%。该方法可以用于紫菜样品中多种有机锡化合物的同时检测。The protocol for simultaneous determination and quantification of 3organotins in laver samples was established by using gas chromatography-mass spectrometry（GC-MS）techniques.The laver samples were extracted by ultrasonic assisted extraction,and derivatized with sodium tetraethylborate（NaBEt4）.The extracts were analyzed by GC-MS after being purified with graphitized carbon black.Under the optimized conditions,good accuracy and specificity were achieved.The average recovery rate obtained for the analytes was in the range of 72.6%-95.7%,with the relative standard deviations（RSDs）lower than 9.26%.The limits of detection for each OTC were 0.0043,0.003 8mg·L^-1 and 0.0026mg·L^-1,respectively.Some different laver samples were also detected using this developed method.It is expected that this method could be used for the OTCs determination in the future.

关 键 词：二甲基锡 三甲基锡 三乙基锡 气相色谱-质谱 紫菜 

分 类 号：O657[理学—分析化学]