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化学学报
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化学学报 ›› 2011, Vol. 69 ›› Issue (20): 2505-2510. 上一篇    下一篇

研究论文

有机磷药物在水产品中的存在状态研究及其分析应用

王雪荣，刘振波，贾风燕，张强，殷军港，刘永明*   

  1. (烟台大学化学生物理工学院 烟台 264005)
  • 投稿日期:2011-03-02 修回日期:2011-05-04 发布日期:2011-06-20
  • 通讯作者: 刘永明 E-mail:yongming_liu@163.com
  • 基金资助:

    山东省科技攻关项目

Study on the Form of Organic Phosphorus in Aquatic Products and Its Analytical Application

WANG Xue-Rong, LIU Zhen-Bo, JIA Feng-Yan, ZHANG Qiang, YIN Jun-Gang, LIU Yong-Ming   

  1. (School of Chemical and Biological Science and Engineering, Yantai University, Yantai 264005)
  • Received:2011-03-02 Revised:2011-05-04 Published:2011-06-20
  • Contact: Yongming LIU E-mail:yongming_liu@163.com

PDF

944

被引次数

14

用分子荧光法、气相色谱法探讨了有机磷药物在以蛋白质为主要基质的水产品中的存在状态, 并研究了蛋白质对有机磷药物提取的影响. 结果表明, 有机磷药物与蛋白质有较强结合作用. 体积分数为70%～90%乙腈水溶液可引起蛋白质变性伸展, 利于释放结合的药物, 从而提高蛋白质基质中的有机磷提取回收率. 以体积比乙腈∶乙酸∶水＝90∶1∶9的溶液提取鱼肉样品中的有机磷药物, 以PSA, GDX-103为混合颗粒吸附剂, 以无水硫酸镁、无水醋酸钠为混合无机盐除水剂, 经离心分离去除基质后萃取液直接进样测定了鱼肉中5种有机磷药物(敌敌畏、甲胺磷、乐果、甲基对硫磷和乙基对硫磷), 测定回收率为72.97%～107.21%, 检出限为0.002～0.045 mg•kg－1. 方法操作步骤简单、快速、高效.

关键词: 蛋白质, 结合作用, 有机磷药物, 基质去除, 气相色谱, 水产品, 直接进样

Molecular fluorescence spectrometry and gas chromatography were applied to study the form of organic phosphorus in protein matrix of aquatic products. The influence of proteins on extraction of organic phosphorus from aquatic products samples was also discussed. The results showed that there was a strong binding effect between organic phosphorus and proteins. In the volume fraction of acetonitrile (ACN) between 70% and 90% aqueous solution protein denaturation could occur and the organic phosphorus binding with the protein could be released, which resulted in a higher recovery rate of the extraction of organic phosphorus from protein matrix samples. The method involved the following steps: extracted the fish sample by using the solution of V(acetonitrile)∶V(acetic acid)∶V(water)＝90∶1∶9, eliminated the moisture by adding anhydrous magnesium sulfate (MgSO4) plus sodium acetate (NaAc), purified the samples by using primary secondary amine (PSA) and GDX-103. The extract was then centrifuged and transferred to vials for direct analysis by gas chromatography (GC). The method was used to the determination of five organic phosphorus residues (dichlorvos, methamidophos, dimethoate, methyl-parathion and ethyl-parathion) in fish. The recovery ranges and the detection limits were 72.97%～107.21% and 0.002～0.045 mg•kg－1, respectively. The method was simple, quick and sensitive.

Key words: protein, binding effect, organic phosphorus, matrix eliminating, gas chromatography, aquatic product, direct analysis

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