GPC-UPLC-MS/MS测定食用油脂中5种辣椒素类物质

Determination of five kinds of capsaicins in edible oil by GPC-UPLC-MS/MS

建立了凝胶渗透色谱-超高效液相色谱-串联质谱法(GPC-UPLC-MS/MS)测定食用油脂中天然辣椒素、二氢辣椒素、合成辣椒素、降二氢辣椒素、高二氢辣椒素含量的方法。样品经凝胶渗透色谱在线净化后,采用超高效液相色谱-串联质谱法分析,动态多反应监测模式(dMRM),同位素内标法定量。结果表明:方法在0.05~10μg/L范围内线性良好,线性相关系数均大于等于0.998;检出限为0.02~0.05μg/kg,定量限为0.10μg/kg;在0.20、1.00、5.00μg/kg添加水平下,平均加标回收率为90.6%~101.5%,相对标准偏差(RSD)为2.5%~9.7%。该方法前处理过程简便快捷,定量准确,可满足实验室准确测定食用油脂中5种辣椒素类物质的需求。

A new analytical method was developed for the simultaneous determination of capsaicin, dihydrocapsaicin, nonivamide, nordihydrocapsaicin and homodihydrocapsaicin in edible oil by gel permeation chromatography(GPC) coupled with ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The sample was cleaned by GPC online, then analyzed by UPLC-MS/MS based on dynamic multiple reaction monitoring(dMRM) mode, and quantified using isotope internal standard technique. The results showed that the method was linear in the range of 0.05-10 μg/L with linear correlation coefficients not less than 0.998, and the limits of detection and quantitation were 0.02-0.05 μg/kg and 0.10 μg/kg respectively. The average recoveries were in the range of 90.6%-101.5% at 0.20,1.00,5.00 μg/kg spiked levels with relative standards deviation(RSD) between 2.5% and 9.7%. The method had the items of simple, rapidness, and accuracy, and could be used to accurately quantify the five kinds of capsaicins in edible oil.