分析化学2011，Vol.39Issue(4)：544-547,4.DOI:10.3724/SP.J.1096.2011.00544
高效液相色谱-电感耦合等离子体质谱联用测定沉积物中的多种有机锡
Speciation Analysis of Organotin Compounds in Sediment by Hyphenated Technique of High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry
摘要
Abstract
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 sediment samples. Agilent TC-C18 column was selected,mobile phase of the HPLC was CH3CN ∶H2O ∶CH3COOH =65∶23∶12 (V/V), 0.05％ triethylamine (TEA), pH=3.0 at flow rate 0f 0.6 mL/min. 30％ O2/Ar mixed gas was added to the make-up gas,which not only reduced the carbon build-up on the cones, but also protected the cones. To reduce solvent loading on the plasma, the double-pass spray-chamber was peltier cooled to-5 ℃. The high RF power (1500 W) helped the samples to decompose completely. A mix standard solution of five mixed organotin compounds from 100 μg/L to 1 μg/L was used for the method assessment. The experimental results indicate that the correlation coefficient of calibration curves (R2) for each organotin compound was over 0. 998. The international standard reference PACS-2 samples were treated by supersonic extraction with mobile phase added 0.2％ tropolone. Two organotin compounds including dibutyltin chloride (DBT) and tributyltin chloride (TBT) were detected with method mentioned above.The values of dibutyltin chloride (DBT) and tributyltin chloride (TBT) were 0.99 and 0.83 mg/kg,respectively. The results showed good accordance with the certified values. The recoveries from the standard addition for five organtins were over 80％.关键词
高效液相色谱-电感耦合等离子体质谱/有机锡/形态分析/海洋沉积物Key words
High performance liquid chromatography-inductively coupled plasma mass spectrometry/Organotin compounds/ Speciation/ Sediment引用本文复制引用
于振花,张杰,王小如..高效液相色谱-电感耦合等离子体质谱联用测定沉积物中的多种有机锡[J].分析化学,2011,39(4):544-547,4.基金项目
本文系国家自然科学基金(Nos.20675021,41006054)资助项目 （Nos.20675021,41006054）
