色谱 ›› 2018, Vol. 36 ›› Issue (10): 1038-1044.DOI: 10.3724/SP.J.1123.2018.05012

• 研究论文 • 上一篇    下一篇

快速溶剂萃取-气相色谱-串联质谱法同时测定土壤中有机氯及有机磷农药

宋晓娟1, 贺心然1,2, 尹明明1, 万延延1   

  1. 1. 连云港市环境监测中心站, 江苏 连云港 222001;
    2. 河海大学环境学院, 江苏 南京 210098
  • 收稿日期:2018-05-12 出版日期:2018-10-08 发布日期:2014-08-22
  • 通讯作者: 贺心然,E-mail:xinranhejs@163.com
  • 基金资助:

    国家重大环境问题决策支持项目(2023004017);江苏省"333工程"培养资金资助项目(BRA2017311).

Determination of organochlorine and organophosphorus pesticides in soil by gas chromatography-tandem mass spectrometry with accelerated solvent extraction

SONG Xiaojuan1, HE Xinran1,2, YIN Mingming1, WAN Yanyan1   

  1. 1. Lianyungang Municipal Environmental Monitoring Center Station, Lianyungang 222001, China;
    2. College of Environment, Hohai University, Nanjing 210098, China
  • Received:2018-05-12 Online:2018-10-08 Published:2014-08-22
  • Supported by:

    Decision Support Project on National Major Environmental Issues (No. 2023004017); Training Funds by "333 Project" of Jiangsu Province (No. BRA2017311).

摘要:

建立了快速溶剂萃取(ASE)-气相色谱-串联质谱(GC-MS/MS)同时分析土壤中8种有机氯农药(OCPs)和5种有机磷农药(OPPs)的方法。样品由正己烷-丙酮(1:1,v/v)溶液萃取,经无水硫酸钠脱水、氮吹仪浓缩后,采用硅胶(Si)固相萃取小柱进行净化,正己烷-丙酮(1:1,v/v)溶液进行洗脱,然后经HP-5MS色谱柱(30 m×0.25 mm×0.25 μm)分离,在电子轰击电离源下以多反应监测(MRM)模式进行检测,内标法定量。分析结果表明,13种目标物在1.00~100 μg/L范围内线性关系良好,相关系数(R)大于0.995;加标回收率为66.8%~88.4%,能够实现准确定量;日内精密度与日间精密度均小于10%。当取样量为10.0 g时,8种OCPs的方法检出限为0.02~0.04 μg/kg,5种OPPs的方法检出限为0.06~0.12 μg/kg,能够满足土壤农药残留的检测要求。

关键词: 快速溶剂萃取, 气相色谱-串联质谱, 土壤, 有机磷, 有机氯

Abstract:

A method based on gas chromatography-tandem mass spectrometry (GC-MS/MS) coupled with accelerated solvent extraction (ASE) was developed for the determination of eight organochlorine pesticides (OCPs) and five organophosphorus pesticides (OPPs) in soils. The soil samples were grinded after freeze-drying. Particles with diameters lower than 250 μm were chosen by ion-sieving. After this, 10.0 g soil mixed with 2.0 g diaomite was extracted with hexane-acetone (1:1, v/v). The extracts were dehydrated with anhydrous sodium sulfate and concentrated with a termovap sample concentrator. The concentrated solutions were further cleaned up with Si SPE columns and eluted with hexane-acetone (1:1, v/v). The purified solutions were then isolated by HP-5MS column (30 m×0.25 mm×0.25 μm) and detected using the multiple reaction monitoring mode at the electron impact source. It is observed that this method has good linearities in the range of 1.00-100 μg/L for the 13 compounds, and the correlation coefficients (R) were greater than 0.995. The spiked recoveries of the 13 compounds were in the range of 66.8%-88.4%, and the relative standard deviations were less than 10%. With 10.0 g of sampling weight, the method detection limits ranged from 0.02 to 0.04 μg/kg for the eight OCPs and from 0.06 to 0.12 μg/kg for the five OPPs. This method is suitable for the determination of trace OCPs and OPPs in soils.

Key words: accelerated solvent extraction (ASE), gas chromatography-tandem mass spectrometry (GC-MS/MS), organochlorine pesticides (OCPs), organophosphorus pesticides (OPPs), soil

中图分类号: