低温高压萃取-气相色谱质谱法同时测定水样中多种有机锡化合物  

Determination of organotin compounds in water by gas chromatography-mass spectrometry after low-temperature high-pressure extraction

作　　者：马冰峰 马雅倩[2] 万益群[2] 

机构地区：[1]江西省产品质量监督检测院,江西南昌330029 [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）》2013年第5期452-456,共5页Journal of Nanchang University(Natural Science)

基　　金：国家科技支撑计划项目(2012BAK17B02);国家自然科学基金资助项目(20965005);食品科学与技术国家重点实验室自由探索课题(SKLF-ZZB-201304);食品科学与技术国家重点实验室目标导向课题(SKLF-ZZA-201302)

摘　　要：应用高压低温萃取技术对目标物进行萃取,采用NaBEt4衍生,结合气相色谱-质谱分析技术,研究建立了水样中多种有机锡化合物（二丁基锡,三丁基锡和三苯基锡）同时检测的新方法。实验采用高压冷冻萃取釜进行萃取,对水样的萃取方式,有机萃取溶剂种类以及水相和有机相的比例等参数进行了优化。在优化的实验条件下,二丁基锡,三丁基锡和三苯基锡3种化合物在0.01-1.0μg·mL-1的浓度范围内线性关系良好,线性相关系数分别为0.997 7,0.999 7和0.999 7,检测限分别为0.34,0.41和0.20μg·L-1。3个加标水平的平均回收率在74.1%-100.5%之间,相对标准偏差在4.7%-9.1%之间。该方法快速、简便、经济环保,适合于水样的分析检测。A method based on low-temperature high-pressure extraction device with gas chromatographymass spectrometry（GC-MS）has been developed for the simultaneous determination of three organotin compounds（OTCs）including dibutyltin（DBT）,tributyltin（TBT）,and triphenyltin（TPhT）.With the application of low-temperature high-pressure extraction device,the critical parameters including the way of pretreatment,type of extraction solvent,the ration of water sample and extraction solvent were optimized.Under the optimized conditions,the developed analytical procedure was sensitive with good linearity,the detection limits of three OTCs were 0.34,0.41and 0.20g·L-1,respectively.The obtained recoveries of the analytes at three different addition levels ranged from 74.1%to 100.5%,providing the precision of between 4.7%and 9.1%.Due to its simplicity,reliability and low-cost,the method is appropriate to be used in routine laboratories for monitoring of OTC in water samples.

关 键 词：有机锡化合物 气相色谱-质谱 低温高压萃取 水样 

分 类 号：O657.63[理学—分析化学]