摘要
基于增强型脂质去除(Captiva EMR-Lipid)技术,建立一种超高效液相色谱-串联质谱(UP-LC-MS/MS)同时测定植物油脂中15种香料类物质的方法。样品采用体积分数80%乙腈水溶液提取,Captiva EMR-Lipid柱净化,以HSS T_(3)柱为分离柱,用体积分数0.1%甲酸水-乙腈为流动相进行梯度洗脱,使用电喷雾离子源多反应监测模式(MRM),外标法定量。结果表明:15种化合物标准工作曲线的相关系数(r)均大于0.995,方法的检出限为2.5~10.0μg/kg,定量限为8.0~30.0μg/kg,加标回收率为72.2%~96.7%,相对标准偏差(n=6)为1.7%~7.5%。建立的方法重现性好、灵敏准确,适用于植物油脂中15种香料类物质的同时测定。
A method for the simultaneous determination of 15 spice substances in vegetable oils was established based on the enhanced matrix removal-lipid(Captiva EMR-Lipid)technology using ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were extracted with volume fraction 80%acetonitrile aqueous solution and purified by Captiva EMR-Lipid column.Separation was achieved by HSS T_(3) column using a gradient elution with volume fraction 0.1%formic acid aqueous solution and acetonitrile as the mobile phase,and quantified by electrospray ionization source multiple reaction monitoring mode(MRM)and external standard method.The results showed that the correlation coefficients(r)of the standard working curves for all 15 substances were greater than 0.995.The limits of detection ranged from 2.5 to 10μg/kg,and the limits of quantification ranged from 8.0 to 30.0μg/kg.The spiked recoveries were between 72.2%and 96.7%,with relative standard deviations(n=6)of 1.7%-7.5%.The established method had good reproducibility,sensitivity,and accuracy,and was suitable for the simultaneous determination of 15 spice substances in vegetable oils.
作者
孟鹏
MENG Peng(Fujian Inspection and Research Institute for Product Quality,Fuzhou 350002,Fujian,China;National Quality Supervision and Testing Center for Processed Food(Fuzhou),Fuzhou 350002,Fujian,China)
出处
《粮食与油脂》
北大核心
2025年第12期149-156,共8页
Cereals & Oils
基金
国家市场监管总局科技计划项目(2021MK054)
福建省市场监督管理局科技项目(FJMS2022005)。
