Determination of Residual Organophosphorus Pesticides in Ham by Gas Chromatography with Purification on Gel Permeable Column
摘 要
用乙腈萃取火腿试样中的残留农药,所得萃取液经凝胶渗透色谱柱净化后用气相色谱法(带火焰光度法检测器)测定了9种农药的残留量,用外标法定量.HP-1701型毛细管色谱柱(30 m×0.53 mm,1.0 μm)用于气相色谱分离,采用柱温250 ℃和检测器温度230 ℃,载气为氮气,流速为10 mL·min-1,测得三唑膦农药的测定限为2.8 μg·kg-1,其它8种有机膦农药的测定限均为5 μg·kg-1.用标准加入法测定回收率,9种农药的回收率均在70%以上.
Abstract
Ham sample was extracted with acetonitrile,and the organophosphorus pesticides in the extract were purified by passing through the gel permeable column (GPC).Elution was carried out with cyclohexane-ethyl acetate (1+1) mixture as eluant,and the eluate collected from the 100th-165th mL was taken for GC determination of 9 pesticides.Flame photometric detection (FPD) and external standard method were adopted in the quantitative analysis.DB-1701 capillary chromatographic column (30 m×0.53 mm,i.d.1.0 μm) was used in the GC-separation,with the column temperature at 250 ℃,and the detector temperature at 230 ℃.Flow-rate of the carrying gas (N2) taken was 10 mL·min-1.Limit of quantification of triazophos was found to be 2.8 μg·kg-1,while for the other 8 pesticides,the values found were all 5 μg·kg-1.Recovery test of all these pesticides were done and results obtained were above 70%.
中图分类号 O653.37
所属栏目 工作简报
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收稿日期 2006/3/9
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备注谢文(1966-),女,吉林省梨树人,硕士研究生,高级工程师,主要从事食品中农药、兽药的残留分析.
引用该论文: XIE Wen,DING Hui-ying,ZHANG Xiao-dong,HUANG Lei-fang. Determination of Residual Organophosphorus Pesticides in Ham by Gas Chromatography with Purification on Gel Permeable Column[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2007, 43(5): 383~385
量谢文,丁慧瑛,章晓氡,黄雷芳. 凝胶柱前处理-气相色谱法测定火腿中多种有机膦农药残留[J]. 理化检验-化学分册, 2007, 43(5): 383~385
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参考文献
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【3】SN 0123-1992出口肉及肉制品中敌敌畏、二嗪膦、倍硫膦、马拉硫膦残留量检验方法[S].
【4】SN 0214-1993出口肉及肉制品中敌敌畏、二嗪膦、皮蝇膦、毒死蜱、杀螟硫膦、对硫膦、乙硫膦、蝇毒膦残留量检验方法[S].
【5】SN 0125-1992出口肉及肉制品中敌百虫残留量的检验方法[S].
【6】邵俊杰.食品分析大全:第1卷[M].北京:高等教育出版社,1977:31-43.
【7】EN 12393-2:1998Enropean standard[S].
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