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目的建立简单、准确测定水果中7种有机磷农药残留的分析方法。方法取水果样品以丙酮为提取剂经加速溶剂萃取装置(ASE)萃取,提取液无水硫酸钠除水后,在线定量浓缩(EVA),再经全自动凝胶渗透色谱仪(GPC)净化,净化液在线浓缩定容后采用气相色谱-质谱法同时进行分离和定性,外标法定量检测。结果该实验条件下,7种有机磷化合物的线性关系良好,相关系数均>0.999;样品加标的平均回收率为80%~118%,相对标准偏差均<5.0%,该方法的检测限为0.012μg/L~0.084μg/L。结论该方法的提取效率高,稳定性好,准确灵敏,大量实际样品的检测结果表明,此方法适于水果中农药残留检测实际工作的需要。
Objective To establish a simple and accurate method for the determination of 7 organophosphorus pesticide residues in fruits. Methods The samples of fruits were extracted with acetone as accelerant by accelerated solvent extraction (ASE). After the extract was extracted with anhydrous sodium sulfate, the samples were quantitatively concentrated (EVA) by water and purified by GPC (Automated Gel Permeation Chromatography) After the purification solution was concentrated on-line, the gas chromatography-mass spectrometry was used for separation and qualitative analysis simultaneously. Results Under the experimental conditions, the linear relationships of the seven organophosphorus compounds were good with correlation coefficients> 0.999. The average recoveries of spiked samples were 80% -118% with relative standard deviations <5.0%. The detection limit was 0.012 μg / L to 0.084 μg / L. Conclusion The method has high extraction efficiency, good stability, accurate and sensitive. The detection results of a large number of actual samples show that this method is suitable for the practical work of pesticide residue detection in fruits.