超高效液相色谱-串联质谱法同时检测回收油脂中的3种辣椒素类化合物  

Simultaneous Determination of Three Capsaicinoids in Recovery Oil by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：梁瑞 赵静 孙悦 高晖 海艳 LIANG Rui;ZHAO Jing;SUN Yue;GAO Hui;HAI Yan(Ningxia Grain and Oil Product Quality Inspection Center,Yinchuan 750002,China)

机构地区：[1]宁夏回族自治区粮油产品质量检测中心,宁夏银川750002

出　　处：《食品科技》2021年第5期285-289,共5页Food Science and Technology

基　　金：2018年度宁夏回族自治区重点研发计划项目(2018BEG03071)。

摘　　要：建立了超高效液相色谱-串联质谱法(UHPLC-MS/MS)同时测定回收油脂中辣椒素、合成辣椒素和二氢辣椒素的方法。样品经氢氧化钠溶液提取,酸化后采用C_(18)固相萃取柱净化,经ZORBAX Eclipse plus C_(18)色谱柱(2.1 mm×100 mm,3.5 μm)以乙腈–0.1%甲酸水溶液为流动相进行梯度洗脱,以电喷雾离子源正离子多反应监测(MRM)模式进行质谱监测。结果表明:辣椒素、合成辣椒素、二氢辣椒素在0.50-100 ng/mL的线性范围内线性关系良好,R^(2)≥0.999,检出限和定量限分别为0.03-0.06 μg/kg和0.1-0.2 μg/kg。低、中、高3个水平下的加标回收率在87.8%-100.4%,相对标准偏差(RSD)为1.1%-8.8%(n=6)。该方法高效、准确、可靠,可有效地应用于回收油脂中辣椒素、合成辣椒素和二氢辣椒素的同时检测。A comprehensive analytical method was developed and validated for the simultaneous determination of capsaicin,nonivamide and dihydrocapsaicin in recovery oil by using ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS).The target analytes in samples were extracted with hydroxide sodium and acidified with sulfuric acid.The extract cleaned up on a C_(18) solid phase extraction column.The analytes were separated on a ZORBAX Eclipse plus C_(18) column (2.1 mm×100 mm,3.5 μm) using acetonitrile-0.1% (v/v) formic acid as a mobile phase for gradient elution,and then determined by tandem mass spectrometry in positive ESI modes under multiple reaction monitoring (MRM).The results showed that good linearity was observed in the concentration range from 0.50 ng/mL to 100 ng/mL for the three capsaicinoids,with absolute coefficients (R^(2)) greater than 0.999.The limits of detection (LODs) ranged from 0.03 μg/kg to 0.06 μg/kg and limits of quantitation (LOQs) between 0.1 μg/kg to 0.2 μg/kg.The recoveries varied from 87.8% to 100.4% at three spiked levels,with relative standard deviations (RSDs) between 1.1% and 8.8% (n=6).The developed method is efficient,accurate,reliable and is effective for the simultaneous determination of capsaicin,nonivamide and dihydrocapsaicin in recovery oil.

关 键 词：超高效液相色谱-串联质谱 回收油脂 辣椒素类化合物 固相萃取 

分 类 号：TS207.5[轻工技术与工程—食品科学] O657.63[轻工技术与工程—食品科学与工程]