加速溶剂萃取-硅胶萃取净化-气相色谱/质谱法检测地表水中有机氯农药和多氯联苯  

Determination of Organochlorine Pesticides and Polychlorinated Biphenyls in Surface Water Using Accelerate Solvent Extraction Coupling with Gas Chromatography-Mass Spectrometry

作　　者：邵阳[1,2] 杨国胜[1,2] 韩深[3] 马玲玲[1,2] 罗敏[1,2] 刘韦华[3] 徐殿斗[1,2] 

机构地区：[1]中国科学院高能物理研究所核技术应用研究中心,北京100049 [2]北京市射线成像技术与装备工程技术研究中心,北京100049 [3]北京出入境检验检疫局技术中心,北京100026

出　　处：《分析化学》2016年第5期698-706,共9页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(Nos.11275216;11575210;11435002和21407149)资助~~

摘　　要：建立了加速溶剂萃取-硅胶固相萃取净化-气相色谱/质谱同时检测地表水中15种有机氯农药(OCPs)和82种多氯联苯(PCBs)的方法。对影响OCPs和PCBs回收率的主要因素进行优化,得出最优的萃取条件:3次静态萃取循环,100℃的萃取温度,丙酮/正己烷(1∶1,V/V)为萃取液,静态萃取10 min。在最优条件下,15种OCPs和82种PCBs在加标水溶液中的回收率分别为70.9%~130%和52.5%~89.1%。日内和日间相对标准偏差分别为1.7%~16.1%和2.4%~33.3%。OCPs和PCBs混合标样在10~800μg/L范围内线性相关系数(R^2)均大于0.995。OCPs和PCBs方法检测限分别为0.13~0.38 ng/L和0.10~0.32 ng/L。相比于传统萃取方法,本方法回收率高、萃取时间短、试剂用量少。应用本方法测得北京城区地表水中OCPs和PCBs的含量范围分别为n.d.~3.45 ng/L和n.d.~4.88 ng/L。A rapid and sensitive analytical method for the simultaneous determination of 15 organochlorine pesticides （OCPs） and 82 polychlorinated biphenyls （PCBs） in water using accelerate solvent extraction （ASE） and silica gel solid phase extraction （SPE） cleanup followed by gas chromatography-mass spectrometry （GC-MS） analysis was developed. The main potential influence parameters which affected the recoveries of OCPs and PCBs were investigated for the optimum ASE efficiency. Finally, 3 static extraction cycles, 100℃ of extraction temperature, mixture of acetone and hexane （ 1 ： 1, V/V） as extraction solvent, and l0 min of static extraction time were used. Under the optimized conditions, the recoveries of 15 OCPs and 82 PCBs in spiked water were 70.9% -130% and 52.5% -89.1% , respectively. The intra-day and inter-day relative standard deviation was 1.7% -16.1% and 2.4% -33.3% , respectively. The correlation coefficients （ RE ） for OCPs and PCBs were above 0. 995 in the range of 10-800 I.Lg/L. And the method detection limits were characterized as 0.13-0.38 ng/L for OCPs and 0. 10-0.32 ng/L for PCBs. Compared to the traditional methods, the developed method had the advantages of higher recoveries and less consumption of extraction time and toxic solvent. Subsequently, the developed method was applied to measure the concentrations of OCPs and PCBs in the surface water of Beijing. The concentrations of OCPs and PCBs were in the range of not detected （n. d. ） -3.45 ng/L and n. d. -4.88 ng/L, respectively.

关 键 词：加速溶剂萃取 有机氯农药 多氯联苯 地表水 北京 气相色谱/质谱联用 

分 类 号：X839.2[环境科学与工程—环境工程] O657.63[理学—分析化学]