黄文军, 高丽荣, 弓爱君, 李 成, 王 璞,付 珊, 肖 珂, 张 兵, 刘文彬

(1.中国科学院生态环境研究中心,北京100085;2.北京科技大学应用科学学院化学系,北京100083)

同位素稀释高分辨气相色谱-高分辨质谱法测定土壤中痕量有机氯农药残留

黄文军1,2, 高丽荣1＊, 弓爱君2, 李 成1, 王 璞1,付 珊1, 肖 珂1, 张 兵1, 刘文彬1

(1.中国科学院生态环境研究中心,北京100085;2.北京科技大学应用科学学院化学系,北京100083)

建立了同位素稀释高分辨气相色谱-高分辨质谱测定土壤中痕量有机氯农药残留的分析方法。采用加速溶剂法萃取土壤样品,以正己烷/丙酮(体积比为1∶1)为提取溶剂,提取液经过Florisil硅土固相萃取小柱净化后,采用高分辨DB-5MS毛细管色谱柱(30m×0.25mm×0.25μm)分离,以保留时间和同位素特征离子丰度比定性,同位素峰面积比定量。实验结果表明,方法的回收率为77.3%～114.5%,相对标准偏差(RSD)≤10.81%(n=5),检出限均小于0.04pg/g。应用该方法检测某地区表层土壤中的有机氯农药,结果表明该方法适合测定环境土壤背景中痕量有机氯残留。

高分辨气相色谱-高分辨质谱;同位素稀释;有机氯农药;土壤

Abstract:A method for the determination of trace organochlorine pesticides(OCPs)in soil using isotope dilution and high resolution gas Chromatography-high resolution mass spectrometry(ID-HRGC-HRMS)was developed.The sam p le was extracted by accelerated solvent extractor(ASE)and cleaned-up by a Florisil solid phase extraction(SPE)cartridge.The analytes were separated by HRGC on a DB-5MS column(30m×0.25mm×0.25μm)and determined by HRMS.The identifications of OCPs were based on the retention time of13C-labelled standard and the abundance ratio of the two exact mass-to-charge ratios.The quantitative analysis was perform ed using the ratios of the integrated areas of the13C-labelled standards.This method has the recoveries ranging from77.3%to114.5%and the relative standard deviations(RSD)less than10.81%(n=5).The limits of detection(LOD s)of this method for all OCPs were lower than0.04pg/g.The results indicated that the method is rap id,selective and sensitive for precise determination requirements of organochlorine pesticides at trace level in soil.

Key words:high resolution gas Chromatography-high resolution mass spectrometry(HRGCHRMS);isotope dilution;organochlorine pesticide;soil

持久性有机污染物(PO Ps)具有高毒性和难降解等特点,并易于在人体和生物体内富集,从而给人类和生态环境带来危害。《关于持久性有机污染物的斯德哥尔摩公约》于2004年11月对我国正式生效。认识我国PO Ps环境污染现状,提出适合我国国情的PO Ps环境污染控制战略是我国作为缔约方履约的重要内容。

首批列入斯德哥尔摩公约的12种持久性有机污染物包括六氯苯、滴滴涕、艾氏剂、狄氏剂、异狄氏剂、毒杀芬、七氯、氯丹、灭蚁灵类等9种有机氯农药(OCPs)。……