凝胶渗透色谱-高效液相色谱串联质谱法测定咸鱼中7种有机磷农药

Determination of seven organophosphate pesticide residues in salted fish by high performance liquid chromatography-tandem mass spectrometry with gel permeation chromatography

目的建立咸鱼中丙溴磷、毒死蜱、马拉硫磷、亚胺硫磷、三唑磷、敌百虫和乐果等7种有机磷农药的凝胶渗透色谱-高效液相色谱串联质谱测定法。方法咸鱼样品经环己烷.乙酸乙酯（l:l,v:v）提取后,经凝胶渗透色谱仪净化,再使用Extend-C18色谱柱分离,采用电喷雾离子化源,以多反应监测（MRM）方式分析,正离子化模式进行检测。结果 7种有机磷农药在2.5100μg/kg线性范围内的相关系数良好,其检出限在0.050.20μg/kg之间。该方法加标回收率为70.9%116.6%,相对标准偏差为2.7%13.8%（n=6）。结论本方法具有提取效率高,净化效果好,准确灵敏和快速等优点,适用于咸鱼中有机磷农药残留检测,符合实际工作需要。

Objective A tandem mass spectrometry-liquid chromatography separation systems (HPLC-MS-MS) method was developed for the determination of 7 organophosphate pesticide residues (profenofos, chlorpyrifos, malathion, phosmet, triazophos, trichlorphon, and dimethoate) in salted fish. Methods Homogenized samples were extracted with cyclohexane-ethylacetate(1:1, v:v), purified by gel permeation chromatography, separated by Extend-C18 column, and determined by electrospray ionization in positive mode under multiple reactions monitoring (MRM). Results The calibration curve showed a good linearity in the range of 2.5~100 μg/kg, the detection limits for 7 pesticides were 0.05~0.20μg/kg, the recoveries at 3 spiked levels were 70.9%~116.6%, and RSDs were between 2.7%~13.8% (n=6). Conclusion This method is simple, effective, and sensitive, which is suitable for the determination and confirmation of the 7 organophosphate pesticide residues in salted fish.