气相色谱-质谱法测定土壤中有机氯农药及多氯联苯
GC-MS Determination of Organochlorine Pesticides and Polychlorobiphenyls in Soil
摘 要
提出了土壤中有机氯农药及多氯联苯的测定方法.土壤样品中22种以污染物存在的农药以丙酮-正己烷(1+1)混合溶剂,用加速溶剂萃取仪进行提取,所得萃取液浓缩至1 mL,通过固相萃取柱进行纯化.用正己烷-乙酸乙酯(8+2)混合溶剂将农药从柱上洗脱,洗脱液浓缩至1 mL后供气相色谱-质谱法测定,采用选择离子(SIM)模式.在两个浓度水平上加入各农药的标准进行了回收试验,测得回收率在68%~130%之间,测定值的相对标准偏差(n=6)均小于25.5%.测得22种农药的检出限(3s/b)在0.25~0.72 ng·g-1之间.
有机氯农药
多氯联苯
土壤
GC-MS in hyphenation
Organochlorine pesticides
Polychlorobiphenyls
Soil
Abstract
Twenty two organochlorine pesticides (OCP′s),including polychlorobiphenyls (PCBP′s),present in soil as pollutants,were extracted from soil sample with mixed solvent of acetone and n-hexane (1+1) by accelerated solvent extraction. The extract was concentrated to 1 mL,which was then purified on the solid phase extraction column and eluted from the column with mixed solvent of n-hexane and ethylacetate (8+2). The eluate was concentrated to 1 mL and used for GC-MS determination,with SIM mode. Recovery was tested by addition of standards of the 22 pesticides at 2 different concentration levels,and the results of recovery were found in the range of 68%-130%. Values of RSD′s (n=6) found for all the 22 pesticides were less than 25.5%. Detection limits (3s/b) found were in the range of 0.25 to 0.72 ng·g-1.
中图分类号 O657.37
所属栏目 工作简报
基金项目 国土资源部地质大调查项目资助(1212010511218)
收稿日期 2008/4/15
修改稿日期
网络出版日期
作者单位点击查看
备注佟玲(1980-),女,北京人,助理研究员,硕士,主要从事有机污染物残留分析工作.
引用该论文: TONG Ling,HUANG Yuan-ying,ZHANG Ling-jin,WU Shu-qi. GC-MS Determination of Organochlorine Pesticides and Polychlorobiphenyls in Soil[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(7): 858～861
佟玲,黄园英,张玲金,吴淑琪. 气相色谱-质谱法测定土壤中有机氯农药及多氯联苯[J]. 理化检验－化学分册, 2009, 45(7): 858～861
被引情况:
【1】时磊,沈小明,胡璟珂,吕爱娟,蔡小虎,沈加林, "不同方法提取海岸带沉积物中多氯联苯及有机氯农药测定的比较",理化检验－化学分册 50, 1113-1116(2014)
【2】范磊,黄素华,田霆,何日安,周华俏,黄可尊, "气相色谱-串联质谱法测定水中多氯联苯",理化检验－化学分册 49, 1479-1482(2013)
【3】梁焱,陈盛,张鸣珊,李腾崖,何书海, "快速溶剂萃取-气相色谱-质谱法测定土壤中24种半挥发性有机物含量",理化检验－化学分册 52, 677-683(2016)
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【3】申中兰,蔡继宝,高芸.基质固相分散-加速溶剂萃取-气相色谱法测土壤中有机氯农药残留[J].分析化学,2005,33(9):1318-1320．
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【7】许行义,刘劲松,庞晓露.土壤中有机氯农药残留分析前处理方法研究[J].中国环境监测,2003,20(1):36-38．
【8】江奎,汪雨,支辛辛.加速溶剂萃取/GC ECD分析土壤中多氯联苯的研究[J].青岛大学学报,2006,21(1):18-22．
【9】李娟,丁曦宁,胡冠九.微波萃取-气相色谱-质谱法测定土壤中的有机氯农药[J].中国环境监测,2005,21(4):49-51．
【10】BRUCE A T,ANGELA R B. Determination of organochlorine pesticides in ground water using solid-phase microextraction followed by dual-column gas chromatography with electron-capture detection[J]. Journal of Chromatography A,2002,964:21-33．
【11】KOICHI S,ANDREAS S,COURTNEY D S. Development of a accelerated solvent extraction and gel permeation chromatography analytical method for measuring persistent organohalogen compounds in adipose and organ tissue analysis[J]. Chemosphere,2004,57:373-381．
【12】FATOKI O S,AWOFOLU R O. Methods for selective determination of persistent organochlorine pesticide residues in water and sediments by capillary gas chromatography and electron-capture detection[J]. Journal of Chromatography A,2003,983:225-236．
【13】ROQUE S,MERCEDES B,ELENA P. Determination of low concentrations of organochlorine pesticides and PCBs in fish feed and fish tissues from aquaculture activities by gas chromatography with tandem mass spectrometry[J]. J Sep Sci,2003,26:75-86．
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