HPLC-ICP-MS联用技术测定水样中苯基锡  

Determination of the phenyltin compounds in water samples by HPLC-ICP-MS

作　　者：鄢爱平[1] 郭岚[1] 雷晓康[1] 柳英霞[1] 万益群[1,2] 

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

出　　处：《南昌大学学报（理科版）》2014年第2期132-136,共5页Journal of Nanchang University(Natural Science)

基　　金：国家自然科学基金(21105043);江西省科技支撑项目(2008BB22400);食品科学与技术国家重点实验室目标导向资助项目(SKLF-MB200807);食品科学与技术重点实验室自由探索资助项目(SKLF-TS-200918)

摘　　要：建立了水样中苯基锡化合物(二苯基锡、三苯基锡和四苯基锡)的高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)的分析方法。水样采用正己烷(含0.01%环庚三烯酚酮)液液萃取,VARIAN Pursuit 5μ-C18反相色谱柱分离,ICP-MS测定。流动相为V甲醇V乙酸(10%,用三乙胺调pH为3.0)=8515。3种化合物在0.5～40μg·L-1范围内均呈良好的线性关系,线性相关系数r>0.999;仪器检测限分别为0.16,0.11和0.18μg·L-1;加标回收率在85.3%～109%之间;相对标准偏差<8%。方法应用于实际水样中3种苯基锡化合物的分析,结果满意。In this study,a sensitive and accurate method for simultaneous determination of three phenyl-tin compounds （diphenyltin,triphenyltin and tetraphenyltin） in water samples with HPLC-ICP-MS was developed. The samples were treated by liquid-liquid extraction with n-hexane（containing 0.01% tropolone）, then were separated and detected by HPLC-ICP-MS. VARIAN Pursuit 5 μ-C18 was selected by a separate column,the composition of mobile phase was optimized as VCH3OH ：Vacetic acid（10% ,pH was adjusted to 3.0 with triethylamine）=85 ： 15. The linear calibration curves were conducted in the 0.5 μg · L-40 μg · L^-1 concentration range and the coefficients were found to be all over 0. 999. The instrument detection limits of diphenyltin （DPhT）, triphenyhin （TPhT） and tetraphenyltin （TePhT） were 0. 16,0. 11 and 0. 18 μg · L^-1 ,respectively. The average recoveries were in the range of 85.3% -109% with the R. S. D. 〈8% . This method was applied to the simultaneous determination of DPhT,TPhT and TePhT in Poyang lake samples with expected results.

关 键 词：高效液相色谱一电感耦合等离子体质谱 苯基锡 水样 

分 类 号：O657.63[理学—分析化学]