加速溶剂萃取-多层硅胶柱净化-气相色谱串联三重四级杆质谱法测定土壤和沉积物中的多氯萘  

Determination of Polychlorinated Naphthalenes in Soil and Sediment Samples by Accelerated Solvent Extraction-Multilayer Silica Gel Column Cleanup Coupled with Gas Chromatography-Triple Quadrupole Mass Spectrometry

作　　者：张利飞[1,2] 张秀蓝[1,2] 张辉[1] 李玲玲[1,2] 张琳利 董亮[1,2] 

机构地区：[1]国家环境分析测试中心,北京100029 [2]国家环境保护二嗯英污染控制重点实验室,北京100029 [3]首都师范大学资源环境与旅游学院,北京100048

出　　处：《分析化学》2014年第2期258-266,共9页Chinese Journal of Analytical Chemistry

基　　金：国家重大科学仪器设备开发专项项目(No.2011YQ060084)资助~~

摘　　要：通过制作多氯萘（PCNs）在商品多层硅胶柱上的流出曲线、优化气相色谱质谱参数和利用三重四级杆质谱的多重反应监测模式,应用氘代一氯萘#2作为一氯和二氯代萘的定量内标,建立了基于DB-5MS和Rt-βDEXcst两根色谱柱的同位素稀释测定土壤和沉积物中多氯萘的分析方法,实现了两种高毒性六氯代萘#66和#67的基线分离。18种多氯萘同类物校正曲线在1.0~240μg/L浓度范围的相对响应因子为0.70~5.45,相对标准偏差小于18.5%。方法检出限在0.014~0.858μg/L之间,定量限在0.048~2.862μg/L之间。30 m的Rt-βDEXcst色谱柱方法效果优于60 m的DB-5MS色谱柱,但前者耗时较长。实际样品分析表明,7种PCNs回收率标记物,除一氯代萘约为6%外,其余均大于28%。测试土壤和沉积物样品中以低氯代萘为主。A method for determining polychlorinated naphthalenes （PCNs） in soil and sediment samples has been developed by using accelerated solvent extraction-muhilayer silica gel column cleanup coupled with gas chromatography-triple quadrupole mass spectrometry （GC-QqQ-MS/MS）. The cleanup condition based on commercial multilayer silica gel column was optimized. 150 mL hexane was finalized and used as eluent. D7- mono chlorinated naphthalene （CN） （#2） was used as internal standard for monoCN and diCN. Main parameters of GC and MS/MS were optimized as well to improve the conditions of separation and resolution of target compounds. Baseline separation of hexaCN （#66） and hexaCN （#67） was accomplished by GC-QqQ- MS/MS using a Rt43DEXcst capillary column in multiple reaction monitoring mode. The relative standard deviations of the average relative response factors for the 18 PCN congeners were below 18.5% in the range of 1.0-240μg/L. The limits of detection and limits of quantitation of PCNs were in the range of 0.014-0. 858μg/L and 0. 048-2. 862μg/L, respectively. The overall performance of the 30 meters Rt-~DEXcst capillary column was better than the traditional 60 meters DB-SMS column. However, it was time-consuming to use the former column. The present method was applied for the determination of PCNs in soil and sediment samples from the Southern Jiangsu Province. The recoveries of the seven labeled PCNs were higher than 28% , except for monoCN （ about 6% ） in the real samples. The results showed that lower chlorinated naphthalenes were the predominant congeners in the test samples.

关 键 词：三重四级杆质谱 多氯萘 多层硅胶柱 

分 类 号：X830.2[环境科学与工程—环境工程] O657.63[理学—分析化学]