高效萃取吸管-在线凝胶色谱-气相色谱-质谱法测定淡水鱼中的农药残留量

Determination of pesticide residues in freshwater fish by disposable pipette extraction-online gel chromatography gas chromatography coupled with mass spectrometry

中文关键词:  高效萃取吸管  在线凝胶色谱-气相色谱-质谱  淡水鱼  农药残留

英文关键词:disposable pipette extraction  online gel permeation chromatography coupled with gas chromatography-mass spectrometry  freshwater fish  pesticide residues

中文摘要:

      目的 建立一种在线凝胶色谱-气相色谱-质谱(gel permeation chromatography coupled with gas chromatography-mass spectrometry, GPC-GC/MS)联用法测定淡水鱼中农药残留的检测方法。方法 采用超声辅助技术和高效萃取吸管法对南昌地区淡水鱼样品净化处理, 以乙腈为提取液, 采用氯化钠去除水分后, 经在线GPC-GC-MS系统进样分析, 选择离子检测方式定量检测。结果 25种化合物的质量浓度在一定范围内与其对应的峰面积有良好的线性关系, 相关系数大于0.996, 方法的检出限为9.1×10?5~3.1×10?1 mg/kg。以空白样品为基体进行加标回收实验, 回收率为71.4%~103.2%, 相对标准偏差小于9%。结论 该方法前处理简单快速, 灵敏度高, 有机溶剂使用量少, 适用于淡水鱼中农药残留的检测。

英文摘要:

      Objective To establish a method for the determination of pesticide residues in freshwater fish by online gel permeation chromatography coupled with gas chromatography-mass spectrometry(GPC-GC/MS). Methods The samples in Nanchang area were purified by ultrasonic assisted technology and high efficiency extraction pipette, extracted with acetonitrile, removed water by sodium chloride, then analyzed by online GPC- GC-MS, quantitated by selected ion monitoring. Results The mass concentration of 25 compounds has a good linear relationship with its corresponding peak area within a certain range, and the correlation coefficient was greater than 0.996. The limits of the detection method were 9.1×10?5?3.1×10?1 mg/kg. The blank sample was used as the matrix for the standard recovery experiment. The recovery rates were 71.4%?103.2%, and the relative standard deviation was less than 9%. Conclusion The method is simple and rapid in pretreatment, sensitive, less organic solvent used and is suitable for the detection of pesticide residues in freshwater fish can be used.