GC Determination of 16 Organochlorine Pesticides in Water with Headspace Solid Phase Microextraction
摘 要
取水样(8.00 mL)置于20 mL顶空瓶中,加入3 g氯化钠至饱和。采用聚二甲基硅氧烷/二乙烯基苯(PDMS/DVB)萃取纤维头,在振动速率250 r·min-1下于70℃萃取60 min。萃取后将PDMS/DVB萃取纤维头插入气相色谱仪,解吸4 min,采用HP-5色谱柱为固定相进行色谱分离。16种有机氯农药的质量浓度在一定范围内与其峰面积呈线性关系,检出限(3.143s)为0.001~0.005 μg·L-1。按标准加入法进行回收试验,回收率在70.6%~132%之间,测定值的相对标准偏差(n=6)在3.7%~30%之间。利用上述方法开展了水中有机氯农药的保存试验研究。
Abstract
Water sample (8.00 mL) was placed in 20 mL headspace flask and saturated with 3 g of sodium chloride. The solution was extracted for 60 min at 70℃ at a vibration rate of 250 r·min-1, using the extract fiber of poly (dimethylsiloxane)/divinylbenzene (PDMS/DVB). After extraction, the PDMS/DVB extract fiber was inserted into GC and desorbed for 4 min. The extract was separated by GC using HP-5 chromatographic column as stationary phase. Linear relationships between values of peak area and mass concentration of 16 organochlorine pesticides were found in definite ranges, with detection limits (3.143s) in the range of 0.001-0.005 μg·L-1. Test for recovery was made by standard addition method, giving results in the range of 70.6%-132%, with RSDs (n=6) ranged from 3.7% to 30%. The preservation of organochlorine pesticides in water was studied by the above method.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201710011
所属栏目 工作简报
基金项目 国家高技术研究发展“八六三”计划基金资助项目(2013AA06A308)
收稿日期 2016/10/19
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联系人作者陈烨(chenye@cnemc.cn)
备注许秀艳(1977-),女,山东乳山人,高级工程师,主要研究方向为环境监测
引用该论文: XU Xiuyan,CAO Fangfang,DING Xining,CHEN Ye. GC Determination of 16 Organochlorine Pesticides in Water with Headspace Solid Phase Microextraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(10): 1171~1176
许秀艳,曹方方,丁曦宁,陈烨. 顶空固相微萃取-气相色谱法测定水中16种有机氯农药的含量[J]. 理化检验-化学分册, 2017, 53(10): 1171~1176
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【5】LORD H, PAWLISZYN J. Evolution of solid-phase microextraction technology[J]. Journal of Chromatography A, 2000,885(1/2):153-193.
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【7】JUNIOR J L R, POPPI N R. Detemination of organochlorine pesticides in ground water samples using solid-phase microextration by gas chromatography-electron capture detection[J]. Talanta, 2007,72(5):1833-1841.
【8】ZHAO R S, WANG X, YUAN J P, et al. A novel headspace solid-phase microextraction method for the exact determination of organochlorine pesticides in environmental soil samples[J]. Analytical & Bioanalytical Chemistry, 2006,384(7/8):1584-1589.
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