固相萃取-液相色谱-串联质谱法同时检测动物源性食品中的可乐定和赛庚啶

Simultaneous determination of clonidine and cyproheptadine residues in animal-derived food by solid phase extraction-liquid chromatography-tandem mass spectrometry

目的建立固相萃取-液相色谱-串联质谱法同时检测动物源性食品中的可乐定和赛庚啶残留的分析方法。方法试样经乙腈提取,过混合型阳离子交换固相萃取柱净化,采用T3色谱柱,多反应监测正离子扫描方式,分离分析,基质外标法定量。结果目标物在1.0~100 ng/mL范围内线性关系良好,相关系数(r2)大于0.999;方法的检出限为1μg/kg,定量限为5μg/kg。在5、10、50μg/kg添加水平下不同基质(猪肉、鸡肉、牛肉、猪肝、猪脂肪、牛奶、鸡蛋和肠衣)中可乐定和赛庚啶的加标回收率范围为67.2%~102.0%,相对标准偏差为5.37%~12.3%。结论该方法选择性好、抗干扰能力强,能满足国内外法规的要求,可以为动物源食品中可乐定和赛庚啶残留的监测提供技术支持。

Objective To establish a method for the simultaneous determination of clonidine and cyproheptadine residues in animal-derived food by solid phase extraction-liquid chromatography-tandem mass spectrometry.Methods The samples were extracted with acetonitrile,and purified by a mixed cation exchange solid-phase extraction column.A T3 chromatographic column was used with multi-reaction monitoring positive ion scanning mode for separation and analysis,and the matrix was quantified by external standard method.Results The linearity of the target compound was good within the range of 1.0-100 ng/mL,and the correlation coefficient(r2)was greater than 0.999.The limit of detection was 1μg/kg,and the limit of quantitation was 5μg/kg.The recoveries of clonidine and cyproheptadine in different matrices(pork,chicken,beef,pork liver,pig fat,milk,eggs,and casing)at the addition levels of 5,10,and 50μg/kg were in the range of 67.2%-102.0%,with the relative standard deviations of5.37%-12.3%.Conclusion This method has good selectivity and strong anti-interference ability,which can meet the requirements of laws and regulations at home and abroad and provide technical support for the monitoring of clonidine and cyproheptadine residues in animal-derived food.