摘要
利用高效液相色谱-电感耦合等离子体质谱（HPLC-ICP/MS）联用技术对5种有机锡[三甲基氯化锡（TMT）、二丁基氯化锡（DBT）、三丁基氯化锡（TBT）、二苯基氯化锡（DPhT）和三苯基氯化锡（TPhT）]进行了分离,采用Agilent TC-C18柱进行有机锡的形态分析,流动相为V（乙腈）∶V（H2O）∶V（乙酸）=65∶23∶12,0.05%的三乙胺,pH=3.0,流速为0.4mL/min,测定了0.5～100μg/L范围内5种有机锡化合物的混合标准工作曲线,其相关系数优于0.998（R2）,方法的检出限均小于0.5μg/L。采用流动相对菲律宾蛤（Ruditapes Philippi-narum,R.P.）及毛蛤（Ark Shell,A.S.）样品进行超声萃取及高速离心后,用上述方法进行了分析。结果表明,海产品含有4种有机锡,其中TBT和TPhT的含量最高,为14.38～104.7μg/L（干重）。TMT、TBT和TPhT的加标回收率均优于80%。DPhT和DBT可能存在吸附或降解问题,因而回收率仅为37.3%～75.2%。
The hyphenated technique of high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry （HPLC-ICP-MS） was applied to the simultaneous determination of five organotin compounds in the shellfish samples. Agilent TC-C18 column was selected , mobile phase of the HPLC was CH3CN： H2O： CH3COOH = 65： 23：12 （V/V） , 0.05% TEA, pH = 3.0 at flow rate 0. 4 mL/min. Five mixed organotin standards from 100 μg/L to 0. 5 μg/L was used for the method evaluation. The experimental results indicate that the linearity （R2） for each compound was over 0. 998. The shellfish samples were treated by supersonic extraction with mobile phase for 30min. Four organotin compounds including dibutyltin （DBT） , tributyltin （TBT）, diphenyltin （DPhT） and triphenyltin （TPhT） in shellfish samples were detected with method mentioned above. It was found that the domain compounds in the samples were tributyltin （TBT） and triphenyltin （TPhT）. The recoveries test from the standard addition for trimethyhin （TMT）, tributyltin （TBT）, and triphenyltin （TPhT） were over 80% . However, the recoveries for diphenyltin （DPhT） and dibutyltin （DBT） were relatively low, 37, 3% and 75.2% respectively. The reason might be attributed to the decomposition of those compounds during the extraction procedure. The further study on this subject is under the progress. ood
出处
《分析化学》
SCIE
CAS
CSCD
北大核心
2008年第8期1035-1039,共5页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金(No.20675021)
中内级公益科研院所基本科研业务费专项基金(No.2007G19)资助项目
关键词
高效液相色谱-电感耦合等离子体质谱法
有机锡
形态分析
海产品
High performance liquid chromatography-inductively coupled plasma mass spectrometry, organotin comoounds, soeciation analvsis, seaf
