色谱

色谱 ›› 2012, Vol. 30 ›› Issue (03): 318-326.DOI: 10.3724/SP.J.1123.2011.11010

• 技术与应用 • 上一篇    下一篇

固相萃取-气相色谱-质谱联用同时测定河水和海水中87种农药

宋伟, 林姗姗, 孙广大, 陈猛*, 袁东星   

  1. 厦门大学环境与生态学院, 福建 厦门 361005
  • 收稿日期:2011-11-06 修回日期:2011-12-12 出版日期:2012-03-28 发布日期:2012-05-02
  • 通讯作者: 陈猛,博士,副教授,主要研究方向为农药、兽药等有机污染物的分析技术和环境行为. Tel: (0592)2183127
  • 基金资助:

    厦门市重大科技平台项目(3502Z20091005)

Simultaneous determination of 87 pesticides in river water and seawater using solid phase extraction-gas chromatography-mass spectrometry

SONG Wei, LIN Shanshan, SUN Guangda, CHEN Meng*, YUAN Dongxing   

  1. College of Environment and Ecology, Xiamen University, Xiamen 361005, China
  • Received:2011-11-06 Revised:2011-12-12 Online:2012-03-28 Published:2012-05-02

PDF

501

被引次数

56

摘要：

采用固相萃取-气相色谱-质谱联用技术,建立了河水和海水中87种农药(24种有机磷、15种有机氯、12种唑类、9种拟除虫菊酯类、5种氨基甲酸酯类、7种酰胺类及15种其他新型农药)的多残留同时分析方法。优化了影响分离效果和灵敏度的仪器参数,考察了固相萃取柱柱型及水样体积、pH、盐度的影响,采用NH2柱优化了净化效果,内标法和替代物法用于数据的质量控制。结果表明: 在最佳条件下,各目标农药的方法检出限为0.1～6.6 ng/L;以实际河水和海水为基底,在5 ng/L和20 ng/L的加标水平下,绝大多数目标农药的回收率为60%～120%,相对标准偏差(n=4)为0.01%～9.7%。该法灵敏、准确,已成功地应用于福建九龙江河口区表层水样中多种类农药的复合污染监测,检出包括5种有机磷类、3种酰胺类、4种唑类、3种氨基甲酸酯类、2种拟除虫菊酯类等农药20种。

关键词: 多残留分析;复合污染, 固相萃取, 海水, 河水, 农药, 气相色谱-质谱

Abstract:

A method for the simultaneous determination of 87 commonly used pesticides in China including 24 organophosphorous pesticides, 15 organochlorine pesticides, 12 azoles, 9 pyrethroids, 7 amides and anilines, 5 carbamates and other 15 pesticides in river water and seawater was established using solid phase extraction (SPE)-gas chromatography-mass spectrometry (GC-MS). GC-MS parameters influencing separation and sensitivity were optimized, and the effects of sample volume, pH and salinity on SPE were investigated. The purification was performed using NH2 SPE cartridge. An internal standard and 5 surrogates were used for data analysis and quality control. The results indicated that under the optimized conditions the limits of detection were in the range of 0.1~6.6 ng/L. For most target pesticides, recoveries were between 60% and 120% with relative standard deviations (RSDs, n=4) of 0.01%~9.7% at the spiked levels of 5 ng/L and 20 ng/L in real river water and sea water matrices. The method was successfully applied to monitor multi-class pesticides in surface water in Fujian Jiulong estuary, and 20 pesticides including 5 organophosphorous pesticides, 3 amides, 4 azoles, 3 carbamates, 2 pyrethroids and 3 other pesticides were detected in the mass concentration range of 1.18~660.93 ng/L. The proposed method can meet the requirement for the determination of trace pesticide residues in water samples.

Key words: combined pollution, gas chromatography-mass spectrometry (GC-MS), multi-residue analysis, pesticides, river water, seawater, solid phase extraction (SPE)