液液萃取—固相萃取气相色谱法测定火腿中有机磷农药残留量

时间：2021-02-06 08:00:56　来源：雅意学习网本文已影响人

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　　摘要 [目的]建立火腿中多种有机磷农药残留量同时测定的方法。[方法]火腿中有机磷农药经乙腈提取后，用乙腈-正己烷液液萃取除去脂类和色素，再经石墨碳黑固相萃取小柱净化，气相色谱-火焰光度检测器（GC-FPD）测定。[结果]16种有机磷农药在DB-17、DB-1色谱柱上均获得良好分离，在0.05～1.00 μg/mL范围内，农药残留量色谱分析的线性关系良好，满足定量分析要求，加标水平为0.08和0.20 mg/kg时，农药的平均回收率在71.96%～117.21%，变异系数为1.73%～12.84%。方法的检出限为0.005 3～0.011 8 mg/kg。[结论]该方法具有前处理简单、净化效果好、方法准确、灵敏度高、杂质干扰少的特点，适合火腿中有机磷农药残留量的分析。
　　关键词火腿；液液萃取；固相萃取；气相色谱；有机磷农药
　　中图分类号 TS207.5+3 文献标识码 A 文章编号 0517-6611（2017）13-0092-04
　　Determination of Organophosphate Pesticide Residues in Ham Using Liquid-liquid Extraction / Solid-Phase Extraction with Gas Chromatography
　　JIANG Lu1， MEI Wen-quan2， SHAO Jin-liang2 et al
　　（1. The Agricultural-food Quality and Safety Center of Kunming， Kunming， Yunnan 650118； 2. Quality Standardizing and Testing Technology Institute， Yunnan Academy of Agricultural Sciences， Kunming， Yunnan 650223）
　　Abstract [Objective] A novel method for the determination of organophosphate pesticide residues in ham at the same time was established. [Method] Organophosphate pesticide residues in ham were extracted by acetonitrile， the liquid-liquid extraction using acetonitrile and n-hexane as the extraction volvent was used to remove the grease and pigment and then， the solution was purified by carbon solid phase extraction column， detected by the flame photometry detector of gas chromatograph. [Result] Experimental results showed that 16 species of organophosphate pesticides were well separated in DB-17 and DB-1. Within the scope of 0.05 to 1.00 μg/mL， pesticide residues chromatography analysis of the linear relationship was good to meet quantitative analysis requirements. The average recoveries of organic phosphorus pesticides were 7196%-117.21%， spiked at 0.08 and 0.20 mg/kg level. The relative standard deviations for all the compounds were 1.73%-12.84%. The detection limit of the method varied between 0.005 3-0.011 8 mg/kg. [Conclusion] The method is simple， precise， sensitive， and has a good separation effect， it can be applied to the routine analysis for organophosphate pesticide residues in ham.
　　Key words Ham；Liquid-liquid extraction；Solid-phase extraction；Gas chromatography；Organophosphate pesticide
　　火腿即腌制或熏制的豬肉，味美且营养丰富，历来被看作是席上佳肴、馈赠珍品，深受国人喜爱，每年消费数万吨。然而，一些不法厂商为了避免蚊虫叮咬和生蛆等问题，在制作过程中添加了剧毒农药，给火腿质量安全带来了极大隐患，严重威胁着消费者的身体健康。因此，建立一种快速、准确地测量火腿中农药残留量的分析方法对有效解决其质量安全问题具有重要意义。目前，检测有机磷农药的方法主要有分光光度法[1]、传感器法[2]、流动注射法[3]、气相色谱法[4-5]、液相色谱法[6]、气质联用法[7]、液质联用法[8]等，但对于火腿中有机磷农药残留量的报道还较少。其中部分方法[9]需要用到气质联用仪、凝胶渗透色谱等大型、高精密度仪器，成本较昂贵；一些方法又只能测试较少种类的农药或者操作方法较为繁琐[10-12]。笔者基于火腿基质复杂、农药残留萃取困难的特点，采用乙腈-正己烷液液萃取联合石墨碳黑固相萃取小柱净化，除去样品中油脂等杂质，利用气相色谱-火焰光度检测（GC-FPD）较准确地分析了敌敌畏等16种有机磷农药残留量。

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液液萃取—固相萃取气相色谱法测定火腿中有机磷农药残留量

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