液相色谱-串联质谱法测定紫菜中三种三取代有机锡化合物  

Determination of Trimethyltin,Triphenyltin and Tributyltin in Seaweed by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：毛雪金[1] 程丽华[2] 万益群[1,2] 

机构地区：[1]南昌大学食品科学与技术国家重点实验室,江西南昌330047 [2]南昌大学分析测试中心,江西南昌330047

出　　处：《分析科学学报》2014年第4期462-466,共5页Journal of Analytical Science

基　　金：国家科技支撑计划(No.2012BAK17B02);国家自然科学基金(No.20965005);食品科学与技术国家重点实验室自由探索课题(No.SKLF-ZZB-201304);食品科学与技术国家重点实验室目标导向项目(No.SKLF-ZZA-201302)

摘　　要：建立了液相色谱-串联质谱（LC-MS/MS）同时测定紫菜中三甲基锡（TMT）、三苯基锡（TPhT）和三丁基锡（TBT）的分析新方法。样品用二氯甲烷-乙酸乙酯（1∶1,V/V）混合溶剂进行超声提取,提取液经氮吹至近干,并用甲醇和水混合溶液（7∶3,V/V）定容,经活性炭净化。采用ZORBAX Eclipse plus C18色谱柱分离,流动相为甲醇-0.1%甲酸溶液（55∶45,V/V）,流速为0.3mL/min。在正离子模式下采用多重反应模式（MRM）进行监测。有机锡化合物在1-100ng/mL浓度范围内线性良好,相关系数在0.9902-0.9918之间,TMT、TPhT和TBT的检测限分别为0.2ng/mL、0.4ng/mL和0.2ng/mL。在25、75ng/mL两个添加水平下回收率在72.3%-98.0%之间,其相对标准偏差均小于8.1%。该方法可用于紫菜中三种三取代有机锡化合物的同时测定。A reliable, simple and accurate analytical method was proposed for the simultaneous determination of trimethyltin（TMT）, triphenyltin（TPhT） and tributyltin（TBT） in seaweed by liquid chromatography-tandem mass spectrometry. The three organotin compounds（OTCs） were extracted by 20 mL of the mixed solvent of dichloromethane-ethyl acetate（1：1,V/V） for 15 min with ultrasonicassisted extraction（UAE）. The upper layer was transferred into 20 mL glass centrifuge tube, and concentrated to dryness,then 1 mL mixture solution of methanol and water（70： 30,V/V） was added and cleanuped with active carbon. ZORBAX Eclipse plus C18 column was used for the separation of the three OTCs. The mobile phase of HPLC was methanol -0. 1%methanoic acid（55： 45,V/V ） with the flow rate of 0.3 mL/min. The mass detection was operated in the positive ion mode using multiple reaction monitoring（MRM）. It showed the good linearities when the analyte concentrations were in the range of 1-100 ng/mL, with the correlation coefficients（R^2） in the range of 0. 9902-0. 9918. For TMT, TPhT and TBT,the detection limits were 0.2,0.4 and 0.2 ng/mL, respectively. In the two spiked levels, the average recoveries of TMT,TPhT and TBT were ranged from 72.3% to 98.0%, with relative standard derivations（RSDs） less than 8.1%. The results indicate this method is suitable for detecting TMT, TPhT and TBT in seaweed.

关 键 词：液相色谱-串联质谱法 紫菜 三甲基锡 三丁基锡 三苯基锡 

分 类 号：O657.63[理学—分析化学]