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

为了快速有效的检测沉积物中的多种有机锡,利用高效液相色谱-电感耦合等离子体质谱(HPLC-ICP/MS)联用技术对沉积物中的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))的形态进行了分离,采用Agilent TC-C18柱进行有机锡的形态分析,流动相为乙腈-水-乙酸(65∶23∶12,V/V),0.05%三乙胺,pH=3.0,流速为0.6 mL/min,方法的检出限均小于0.5 mg/L。采用添加0.2%环庚三烯酚酮的流动相对国际标准物质PACS-2样品进行超声萃取及高速离心后,用上述方法进行分析。结果表明,PACS-2中二丁基锡的含量为0.99 mg/kg,三丁基锡的含量为0.83 mg/kg,测定值与标准值吻合。对PACS-2的5种有机锡的加标回收率均大于80%。本方法前处理简单快速,可用于沉积物中有机锡的形态分析。

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 mg/L to 1 mg/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%.