超声提取-气相色谱法测定保健品中15种有机氯农药残留量
GC Determination of Residual Amounts of 15 Organochlorine Pesticides in Health Care Products with Ultrasonic Extraction
摘 要
保健品样品经丙酮、二氯甲烷、石油醚超声提取,提取液过弗罗里硅藻土层析柱净化,所得经净化的淋出液中15种有机氯农药残留量用于气相色谱法测定。采用OV-1701石英毛细管色谱柱分离,用电子捕获检测器测定。15种化合物的检出限(3S/N)在0.091~0.621 ng·kg-1之间。在3个浓度水平下加入标准溶液进行了回收和精密度试验,所得回收率在80.5%~126%之间;测定值的相对标准偏差(n=6)在1.2%~13%之间。
气相色谱法
保健品
有机氯农药
Ultrasonic extraction
GC
Health care products
Organochlorine pesticides
Abstract
The sample of health care products was extracted ultrasonically with acetone, dichloromethane and petroleum ether in succession, and the extracts were combined and purified by passing through Florida diatomite column. The contents of 15 organochlorine pesticides obtained in the eluate were determined by GC. OV-1701 capillary column was used for separation and electron capture detector was adopted in the determination. Values of detection limits (3S/N) of the 15 compounds were found in the range of 0.091-0.621 ng·kg-1. Tests for recovery and precision were made by standard addition method at 3 different concentration levels, values of recovery found were in the range of 80.5%-126% and values of RSD′s (n=8) found were in the range of 1.2%-13%.
中图分类号 O657.7
所属栏目 工作简报
基金项目 贵州省科技厅科学技术基金(黔科合J字LKS［2011］30号);贵州省教育厅自然科学基金(黔教科2010017);贵阳市科技局医疗卫生科技计划项目(［2008］筑科科农合同字第14号);贵州省教育厅招标项目(黔教科(2011)018号)
收稿日期 2012/5/17
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备注张勇(1980-),男,安徽巢湖人,讲师,主要从事水环境和大气环境化学研究。
引用该论文: ZHANG Yong,LIU Yu-bo,CHEN Li-li,XIA Pin-hua,LI Cun-xiong,ZHANG Ming-shi. GC Determination of Residual Amounts of 15 Organochlorine Pesticides in Health Care Products with Ultrasonic Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(3): 337～340
张勇,刘玉波,陈丽丽,夏品华,李存雄,张明时. 超声提取-气相色谱法测定保健品中15种有机氯农药残留量[J]. 理化检验－化学分册, 2013, 49(3): 337～340
被引情况:
【1】张莉,徐万邦,蒋忠军, "毛细管气相色谱法测定沉香中20种有机氯农药残留量",理化检验－化学分册 50, 987-990(2014)
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参考文献
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【5】纪淑娟,刘长江,佐藤元昭,等.用气-质联用技术检测葱、蒜、韭菜中多种农药残留量时试样预处理方法［J］.理化检验-化学分册, 2006,42(11):914-917.
【6】SUCHAN P, PULKRABOV J, HAJLOV J, et al. Pressurized liquid extraction in determination of polychlorinated biphenyls and organochlorine pesticides in fish samples［J］. Anal Chim Acta, 2004,520:193-200.
【7】阎正,封棣,李申杰,等.固相萃取-毛细管气相色谱法测定中草药中13种有机氯农药的残留量［J］.色谱, 2005,23(3):308-311.
【8】张潜,赖发伟.气相色谱法同时测定大米中的37种农药残留［J］.理化检验-化学分册, 2010,46(11):1289-1292.
【9】饶小思,邵丽华,王淑娥,等.毛细管气相色谱法测定药物保健品中六六六、滴滴涕残留量［J］.药物分析杂志, 2007,27(10):1663-1666.
【10】宋家玉,周景洋,陈金东,等.毛细管气相色谱法测定保健食品、中药材中的五氯硝基苯残留［J］.化学分析计量, 2011,20(2):55-57.
【11】潘玉香,董静,孙军,等.气相色谱法测定复杂基质蔬菜中11种农药的残留量［J］.化学分析计量, 2009,45(7):98-100.
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