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[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。
[Objective] To establish a gas chromatographic analysis system for rapid determination of seven kinds of water-soluble organophosphorus pesticides (trichlorfon, dichlorvos, methamidophos, acephate, omethoate, monocrotophos, dimethoate) in aquatic products method. [Method] The samples were extracted with pure water by ultrasonic wave and the soluble protein was precipitated by lead acetate. The filtrate was extracted by acetonitrile liquid-liquid extraction, and the interference substances were purified by solid phase adsorption on N-propyl ethylenediamine solid phase adsorbent (PSA) matrix. Flame photometric detector (GC-FPD) to detect the target pesticide. [Result] The results showed that there was a good linear relationship between the seven pesticides in the range of 0.040 ~ 10.000 mg / kg, the correlation coefficient was between 0.998 8 and 0.999 6, the detection limit was between 0.008 and 0.015 mg / kg (S / N = 3 ). The recoveries of the methods were between 77.0% and 109.0% with relative standard deviations between 1.4% and 7.1%. [Conclusion] The method has been successfully applied to the analysis of organophosphorus pesticide residues in aquatic products with simple, rapid, environmental and high sensitivity.