GC Determination of Residual Endosulfan in Grains with Separation by Accelerated Solvent Extraction
摘 要
提出了粮食中α-硫丹、β-硫丹、硫丹乙酯、硫丹丙酯和硫丹硫酸盐5种硫丹类有机氯农药的气相色谱测定方法.样品粉碎后以丙酮为溶剂经快速溶剂萃取仪在加热(80 ℃)状态下静态提取5 min、氟罗里硅土固相萃取柱净化后注入毛细管气相色谱仪分离测定.5种硫丹类农药的测定下限(10S/N)分别为0.82~1.75 μg·kg-1,平均回收率为88.9%~99.1%,相对标准偏差(n=5)为6.80%~10.23%.
Abstract
Sample of grain was crushed and extracted with acetone under static condition at 80 ℃ for 5 min.The endosulfan pesticides (mainly the α-endosulfan,β-endosulfan,acetate of endosulfan,propyl ester of endosulfan and sulfate of endosulfan) were dissolved in the organic phase and separated from the grain matrix.The extract was evaporated to near dryness by rotary evaporator.The residue was dissolved with petroleum ether and purified by solid phase extraction.The SPE column was rinsed with mixed solvent of petroleum ether and acetone (9+1),and the eluate collected was evaporated to near dryness,and the residue was taken up with petroleum ether and used for GC analysis after separation on DB 1701 capillary column.The μ-ECD detector was used for the determination.Lower limit of determination (10S/N) for the 5 pesticides were found in the range of 0.82-1.75 μg·kg-1,and values of RSD′s (n=5) found were in the range of 6.80%-10.23%.Values of average recovery found by standard addition method were in the range of 88.9%-99.1%.
中图分类号 O657.31
所属栏目 工作简报
基金项目 塔里木大学校长基金重点项目(TDZKZD06002)
收稿日期 2008/11/29
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备注蒋卉(1972-),女,江苏人,实验师,主要从事环境和食品检测.
引用该论文: JIANG Hui,JIN Yu-xia,LIU Wen-jie. GC Determination of Residual Endosulfan in Grains with Separation by Accelerated Solvent Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(3): 251~253
蒋卉,晋玉霞,刘文杰. 溶剂萃取-气相色谱法测定粮食中硫丹类农药残留量[J]. 理化检验-化学分册, 2010, 46(3): 251~253
被引情况:
【1】崔艳华, "固相萃取-气相色谱法测定鱼塘投毒案件水样中硫丹的含量",理化检验-化学分册 51, 1199-1202(2015)
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参考文献
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【2】BHAVAN P S,GERALDINE P.Biochemical stress responses in tissues of the prawn macrobrachium malcolmsonii on exposure to endosulfan[J].Pesticide Biochemistry and Physiology,2001,70:27-41.
【3】WILLEY J B,KRONE P H.Effects of endosulfan and nonylphenol on the primordial germ cell population in pre-larval zebrafish embryos[J].Aquatic Toxicology,2001,54:113-123.
【4】杨新玲,蒋雨平,翁建英,等.硫丹对PC12细胞增殖的影响及诱导其凋亡的研究[J].中国临床神经科学,2004,12(1):5-9.
【5】张晓丹,周广红,陈少军.硫丹对小鼠睾丸生精细胞毒作用及其机制研究[J].环境与职业医学,2006,23(1):34-37.
【6】SIDDIQUE T,ZAHIR Z A,FRANKENBERGER W T.Reversed -phase liquid chromatographic method for analysis of endosulfan and its major metabolites[J].Journal of Liquid Chromatography & Related Technologies,2003,26:1069-1082.
【7】THOMAS K V,HURST M R,MATTHIESSEN P,et al.Toxicity characterisation of organic contaminants in stormwaters from an agricultural headwater stream in south east england[J].Water Research,2001,35:2411-2416.
【8】周延生,王涵文,关亚风.加压溶剂萃取法萃取大气颗粒物中的烷烃[J].分析化学,2004,32(8):983-987.
【9】曾雪灵,叶明立,陈永欣,等.加速溶剂萃取-离子色谱法测定肉制品中的硝酸根及亚硝酸根[J].分析测试学报,2006,25(13):92-94.
【10】喻凌寒,宋之光,陈江韩.快速溶剂萃取反相高效液相色谱法测定青蒿中的青蒿素[J].分析试验室,2006,25(8):68-71.
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