Rapid GC-MS Determination of BHC and DDT Residues in Soil After Purification by On-line Gel Permeation Chromatography
摘 要
采用加速溶剂萃取(ASE)及凝胶色谱(GPC)在线净化,实现了土壤中六六六及滴滴涕的8种异构体或同系物残留量的气相色谱-质谱(GC-MS)联用快速测定.以二氯甲烷-丙酮(1+1)为溶剂,采用加速溶剂萃取土壤样品,萃取液经合并,蒸干后溶于10 mL丙酮中,通过GPC-GC-MS联用仪可实现净化后直接在线检测,检测模式为离子监测(SIM)模式,利用保留时间和特征离子进行定性,外标法定量.在此检测方法下,8种有机氯农药在0.02~0.4 mg·L-1范围内呈线性关系,检出限(3S/N)在0.014 7~0.078 3 μg·kg-1之间,加标回收率在101.4%~129.5%范围内.
Abstract
Rapid GC-MS determination of residual amounts of 8 isomers or homologues of BHC and DDT in soil was achieved by separation with accelerated solvent extraction (ASE) and purification with on-line gel permeation chromatography (GPC).Mixed solvent of dichloromethane and acetone (1 to 1 by vol.) was used as the extraction solvent in ASE,and the extracts obtained were combined and evaporated to near dryness.The residue was taken up with acetone,diluted to 10 mL and used for GC-MS analysis after purification by the on-line GPC.The mode of SIM was used in the MS-detection.Qualitative analysis was performed based on the retention time and characteristic ions,and quantitative analysis was carried out by the external standard method.Linear relationships between values of peak area and concentration of the 8 pesticides were obtained in the same range of 0.02 to 0.4 mg·L-1,with their detection limits (3S/N) in the range of 0.014 7-0.078 3 μg·kg-1.Results of recovery test were found in the range from 101.4% to 129.5%.
中图分类号 O657.63
所属栏目 工作简报
基金项目 北京市科技计划课题(Z080005032508023);国家863计划课题(2008AA100803);国家科技支撑计划课题(2008BADA7B03)
收稿日期 2009/5/1
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备注平华(1983- ),女,河北人,硕士,助理工程师,主要从事农产品质量检测和农田环境监测研究.
引用该论文: PING Hua,LU An-xiang,ZHAO Liu,MA Zhi-hong,PAN Li-gang. Rapid GC-MS Determination of BHC and DDT Residues in Soil After Purification by On-line Gel Permeation Chromatography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(7): 813~815
平华,陆安祥,赵柳,马智宏,潘立刚. 凝胶色谱在线净化-气相色谱-质谱联用快速测定土壤中六六六和滴滴涕残留[J]. 理化检验-化学分册, 2010, 46(7): 813~815
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参考文献
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【3】邹辉,王盛才,杜宁宁,等.气相色谱法测定土壤中有机氯杀虫剂[J].光谱实验室,2007,24(6):1084-1089.
【4】陈伟东,陈国雄,老倩群,等.程序升温毛细管气质联用法快速测定食品中12种有机氯农药[J].中国卫生检验杂志,2008,18(5):807-809.
【5】朱雪梅,崔艳红,郭丽青,等.用加速溶剂提取仪提取污染土壤中的有机氯农药[J].环境科学,2002,23(5):113-116.
【6】刘现明,徐学仁,张笑天,等.大连湾沉积物中的有机氯农药和多氯联苯[J].海洋环境科学,2001,20(4):40-44.
【7】胡贝贞,宋伟华,谢丽萍,等.加速溶剂萃取/凝胶渗透色谱-固相萃取净化/气相色谱-质谱法测定茶叶中残留的33种农药[J].色谱,2008,26(1):22-28.
【8】SANDRA R R,MARIO S G,VALDECIR F X,et al.Organochlorine pesticides and polychlorinated biphenyls in soil and water samples in the Northeastern part of Sāo Paulo State,Brazil[J].Chemosphere,2006,65:1949-1958.
【9】WANG Xue-jun,PIAO Xiu-ying,CHEN Jing,et al.Organochlorine pesticides in soil profiles from Tianjin,China[J].Chemosphere,2006,64:1514-152.
【10】TAO S,GUO L Q,WANG X J,et al.Use of sequential ASE extraction to evaluate the bioavailability of DDT and its metabolites to wheat roots in soils with various organic carbon contents [J].The Science of the Total Environment,2004,320:1-9.
【11】MORENO D V,FERRERA Z S,RODRIGUES J J S.Microwave assisted micellar extraction coupled with solid phase microextraction for the determination of organochlorine pesticides in soil samples[J].Anal Chim Acta,2006,571:51-57.
【12】WANG Wen-tao,MENG Bing-jun,LU Xiao-xia,et al.Extraction of polycyclic aromatic hydrocarbons and organochlorine pesticides from soils: A comparison between Soxhlet extraction,microwave-assisted extraction and accelerated solvent extraction techniques[J].Anal Chim Acta,2007,602:211-222.
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