GC Determination of 12 Pesticides in Drinking Water with Solid Phase Extraction
摘 要
提出了固相萃取-气相色谱法测定饮用水中12种农药残留量的方法。取水样250 mL过固相萃取柱,用乙酸乙酯、正己烷各5 mL洗脱,经无水硫酸钠脱水,采用DB-5MS毛细管色谱柱分离,电子捕获检测器检测。溴氢菊酯的线性范围为0.05~0.5 mg·L-1,其他农药的线性范围均在0.01~0.1 mg·L-1。溴氰菊酯的检出限为24.2 ng·L-1,其他农药的检出限均低于10 ng·L-1。12种农药的加标回收率在70.0%~110%之间,相对标准偏差(n=6)均小于10%。
Abstract
GC with solid-phase extraction was applied to the determination of 12 pesticides in drinking water. Water sample (250 mL) was extracted on C18 solid phase extraction column (SPE). The pesticides on SPE column were eluted with ethyl acetate (5 mL) and n-hexane (5 mL) successvely. Anhydrous Na2SO4 was used for dehydration. The analytes were separated on DB-5MS capillary column and detected by ECD. Linearity range of decamethrin was 0.05-0.5 mg·L-1, and all the other pesticides′ were found between of 0.01-0.1 mg·L-1. Detection limit of the method for decamethrin was 24.2 ng·L-1 and other pesticides′ were below 10 ng·L-1. Values of average recovery of 12 pesticides in water ranged from 70.0% to 110%, and RSD (n=6) were less than 10%.
中图分类号 O657.7
所属栏目 工作简报
基金项目 上海市浦东新区卫生系统学科带头人培养计划资助(PWRd2011-09)
收稿日期 2013/11/13
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联系人作者詹铭(zhanm@163.net)
备注李宏亮(1981-),男,山西宁武人,主管技师,硕士,主要从事理化检验。
引用该论文: LI Hong-liang,ZHAN Ming,JIANG Zhi-hua,XI Ye,HAO Li-Peng. GC Determination of 12 Pesticides in Drinking Water with Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(12): 1513~1516
李宏亮,詹铭,蒋志华,奚晔,郝莉鹏. 固相萃取-气相色谱法测定饮用水中12种农药[J]. 理化检验-化学分册, 2014, 50(12): 1513~1516
被引情况:
【1】王姗姗,李 刚,高丽娜,谭鑫易, "液液萃取分离-气相色谱-串联质谱法同时测定水中12种有机氯农药",理化检验-化学分册 52, 384-387(2016)
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参考文献
【1】CEREJEIRA M J, VIANA P, BATISTA S, et al. Pesticides in portuguese surface and ground Waters[J]. Water Research, 2003,37(1):1055-1063.
【2】GB 5749-2006生活饮用水卫生标准[S].
【3】GB/T 5750.9-2006生活饮用水标准检验方法 农药指标[S].
【4】李俊玲.全自动固相萃取-三重串联四极杆气相色谱/质谱联用测定食用菌中49种农药残留[J].中国卫生检验杂志, 2014(8):1068-1072.
【5】李斌,解启来,刘昕宇,等.自动固相萃取-GC/MS测定水中多环芳烃和有机氯农药[J].环境科学与技术, 2012(5):102-106.
【6】JUNK G A, RICHARD J J. Organics in water: solid phase extraction on a small scale[J]. Anal Chem, 1988,60:451.
【7】EPA Method 3535 5Solid-phase extraction (SPE)6[S].
【2】GB 5749-2006生活饮用水卫生标准[S].
【3】GB/T 5750.9-2006生活饮用水标准检验方法 农药指标[S].
【4】李俊玲.全自动固相萃取-三重串联四极杆气相色谱/质谱联用测定食用菌中49种农药残留[J].中国卫生检验杂志, 2014(8):1068-1072.
【5】李斌,解启来,刘昕宇,等.自动固相萃取-GC/MS测定水中多环芳烃和有机氯农药[J].环境科学与技术, 2012(5):102-106.
【6】JUNK G A, RICHARD J J. Organics in water: solid phase extraction on a small scale[J]. Anal Chem, 1988,60:451.
【7】EPA Method 3535 5Solid-phase extraction (SPE)6[S].
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