同位素稀釋高分辨氣相色譜-高分辨質譜法測定土壤中痕量有機氯農藥殘留

黃文軍, 高麗榮, 弓愛君, 李 成, 王 璞,付 珊, 肖 珂, 張 兵, 劉文彬

(1.中國科學院生態環境研究中心,北京100085;2.北京科技大學應用科學學院化學系,北京100083)

同位素稀釋高分辨氣相色譜-高分辨質譜法測定土壤中痕量有機氯農藥殘留

黃文軍1,2, 高麗榮1＊, 弓愛君2, 李 成1, 王 璞1,付 珊1, 肖 珂1, 張 兵1, 劉文彬1

(1.中國科學院生態環境研究中心,北京100085;2.北京科技大學應用科學學院化學系,北京100083)

建立了同位素稀釋高分辨氣相色譜-高分辨質譜測定土壤中痕量有機氯農藥殘留的分析方法。采用加速溶劑法萃取土壤樣品,以正己烷/丙酮(體積比為1∶1)為提取溶劑,提取液經過Florisil硅土固相萃取小柱凈化后,采用高分辨DB-5MS毛細管色譜柱(30m×0.25mm×0.25μm)分離,以保留時間和同位素特征離子豐度比定性,同位素峰面積比定量。實驗結果表明,方法的回收率為77.3%～114.5%,相對標準偏差(RSD)≤10.81%(n=5),檢出限均小于0.04pg/g。應用該方法檢測某地區表層土壤中的有機氯農藥,結果表明該方法適合測定環境土壤背景中痕量有機氯殘留。

高分辨氣相色譜-高分辨質譜;同位素稀釋;有機氯農藥;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

持久性有機污染物(PO Ps)具有高毒性和難降解等特點,并易于在人體和生物體內富集,從而給人類和生態環境帶來危害。《關于持久性有機污染物的斯德哥爾摩公約》于2004年11月對我國正式生效。認識我國PO Ps環境污染現狀,提出適合我國國情的PO Ps環境污染控制戰略是我國作為締約方履約的重要內容。

首批列入斯德哥爾摩公約的12種持久性有機污染物包括六氯苯、滴滴涕、艾氏劑、狄氏劑、異狄氏劑、毒殺芬、七氯、氯丹、滅蟻靈類等9種有機氯農藥(OCPs)。……