液液萃取-全碳同位素标记-液质联用法测定酱油中玉米赤霉烯酮Determination of Zearalenone in Soy Sauce by Liquid-Liquid Extraction-Full 13C Isotope Labelling-Liquid Chromatography-Tandem Mass Spectrometry
阳曦,刘玮,向世杰
摘要(Abstract):
建立一种快速测定酱油中玉米赤霉烯酮的方法。采用液液萃取-液相色谱-串联质谱法对液相色谱条件、质谱分析条件、提取溶剂、净化方式等影响因素进行了优化。通过试验确定样品经乙腈提取,三氯甲烷萃取净化,采用乙腈、水作为流动相,电喷雾离子源在负离子模式下进行多反应监测(multiple reaction monitoring, MRM),对玉米赤霉烯酮的含量进行测定。在此条件下,5~100 ng/mL浓度范围内玉米赤霉烯酮的线性关系良好,相关系数(r)为0.9997,检出限为0.1μg/kg,定量限为0.3μg/kg,方法回收率为92.7%~96.0%,相对标准偏差小于3.0%。该方法前处理简单、灵敏度高、重复性好,可有效满足酱油中玉米赤霉烯酮的测定。
关键词(KeyWords): 液液萃取;同位素;高效液相色谱-串联质谱法;酱油;玉米赤霉烯酮
基金项目(Foundation):
作者(Author): 阳曦,刘玮,向世杰
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