CAJ | 학술논문

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(1：1, 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2.5~100μg/kg线性范围内的相关系数良好,其检出限在0.05~0.20μg/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。
목적：건립함어중병추린、독사비、마랍류린、아알류린、삼서린、활백충화악과등7충유궤린농약적응효삼투색보-고효액상색보천련질보측정법。방법함어양품경배기완-을산을지(1：1, v：v)제취후,경응효삼투색보의정화,재사용 Extend-C18색보주분리,채용전분무리자화원,이다반응감측(MRM)방식분석,정리자화모식진행검측。결과7충유궤린농약재2.5~100μg/kg선성범위내적상관계수량호,기검출한재0.05~0.20μg/kg지간。해방법가표회수솔위70.9%~116.6%,상대표준편차위2.7%~13.8%(n=6)。결론본방법구유제취효솔고,정화효과호,준학령민화쾌속등우점,괄용우함어중유궤린농약잔류검측,부합실제공작수요。
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.