气相色谱-质谱联用法检测动物源性食品中的敌鼠

Determination of diphacinone in animal-origin food by gas chromatography-mass spectrometry

目的建立气相色谱-质谱联用法(gas chromatography-mass spectrometry,GC-MS)测定动物源性食品中敌鼠的方法。方法本研究考察了提取溶剂、萃取参数及净化小柱对检测结果的影响,样品用丙酮-正己烷(1:1,V:V)为提取溶剂进行微波萃取,采用C18小柱进行净化,以GC-MS进行检测。结果加标水平为0.001、0.002、0.01 mg/kg时,平均回收率为62%~90%,相对标准偏差为0.98%~9.04%,敌鼠的方法检出限为0.0008 mg/kg.结论该方法快速、简单,且灵敏度高,适用于动物源性食品中的敌鼠的检测。

Objective To establish a method for determination of diphacinone in animal-origin food by gas chromatography-mass spectrometry（GC-MS）. Methods The effects of extraction solvents, extraction parameters and purification column on the detection results were investigated. Samples were extracted with acetone n-hexane（1：1, V：V） as solvent and microwave-assisted extraction. Then they were purified by C18 column, and detected by GC-MS. Results At spiked levels of 0.001, 0.002 and 0.01 mg/kg, the average recoveries were in the range of 62%-90%, and relative standard deviations were 0.98%-9.04%. The limit of quantification was 0.0008 mg/kg. Conclusion The method is rapid, simple and highly sensitive, which is suitable for detection of diphacinone in animal-origin food.