黄会秋, 黄逊. 气相色谱法测定水产品中7种水溶性有机磷农药[J]. 环境与职业医学, 2015, 32(10): 979-982. DOI: 10.13213/j.cnki.jeom.2015.15154
引用本文: 黄会秋, 黄逊. 气相色谱法测定水产品中7种水溶性有机磷农药[J]. 环境与职业医学, 2015, 32(10): 979-982. DOI: 10.13213/j.cnki.jeom.2015.15154
HUANG Hui-qiu , HUANG Xun . Determination of Seven Water-Soluble Organophosphorus Pesticides in Fishery Products by Gas Chromatography[J]. Journal of Environmental and Occupational Medicine, 2015, 32(10): 979-982. DOI: 10.13213/j.cnki.jeom.2015.15154
Citation: HUANG Hui-qiu , HUANG Xun . Determination of Seven Water-Soluble Organophosphorus Pesticides in Fishery Products by Gas Chromatography[J]. Journal of Environmental and Occupational Medicine, 2015, 32(10): 979-982. DOI: 10.13213/j.cnki.jeom.2015.15154

气相色谱法测定水产品中7种水溶性有机磷农药

Determination of Seven Water-Soluble Organophosphorus Pesticides in Fishery Products by Gas Chromatography

  • 摘要: 目的 建立一种快速测定水产品中7 种水溶性有机磷农药(敌百虫、敌敌畏、甲胺磷、乙酰甲胺磷、氧化乐果、久效磷、乐果)残留的气相色谱分析方法。

    方法 将样品用纯水超声提取, 乙酸铅沉淀可溶性蛋白质, 滤液经乙腈液液萃取, N-丙基乙二胺固相吸附剂(PSA)基质固相吸附净化干扰物质, 最后采用气相色谱火焰光度检测器(GC-FPD)检测目标农药。

    结果 在0.040~10.000 mg/kg范围内, 7种农药具有良好的线性关系, 相关系数在0.998 8~0.999 6之间, 检出限为0.008~0.015 mg/kg 范围(S/N=3)。方法加标回收率在77.0%~109.0%之间, 相对标准偏差在1.4%~7.1%之间。

    结论 方法已成功应用于水产品中有机磷农药残留分析, 操作简单、快速、环保, 灵敏度高。

     

    Abstract: Objective To develop a method for quick determination of residues of seven water-soluble organophosphorus pesticides (trichlorphon, dichlorvos, methamidophos, acephate, omethoate, azodrin, and dimethoate) in fishery products by gas chromatography.

    Methods The samples were extracted with purified water by ultrasonic extraction and the soluble proteins were precipitated by lead acetate, then the filtrate was re-extracted by acetonitrile liquid-liquid extraction and primary secondary amine (PSA) solid sorbent for further cleanup of interferences, and finally the targeted pesticides were determined by gas chromatography with flame photometric detection (GC-FPD).

    Results Good linear relationships were obtained for the seven pesticides in the range of 0.040-10.000 mg/kg of the analytes with correlation coefficients of 0.998 8-0.999 6 and detection limits of 0.008-0.015 mg/kg (S/N=3). The recoveries for standard addition fell in the range from 77.0% to 109.5% and the relative standard deviations were between 1.4% and 7.1%.

    Conclusion This method has been successfully applied to the determination of organophosphorus pesticide residues in real fishery product samples. The method is proven to be simple, rapid, environmental friendly, and satisfied with high sensitivity.

     

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