超高效液相色谱-串联质谱法测定食用油脂中辣椒素

Determination of capsaicin in edible oils by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  天然辣椒素  二氢辣椒素  合成辣椒素

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  natural capsaicin  dihydrocapsaicin  nonivamide

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定食用油脂中辣椒素的分析方法。方法 试样经正己烷溶解, 氢氧化钠水溶液提取, 碱性提取液经硫酸酸化后, 过PEP-2固相萃取小柱净化, 采用超高效液相色谱-串联质谱仪检测, 外标法定量。以ACQUITY UPLC BEH C18色谱柱(3.0 mm×100 mm, 1.7 μm)为固定相, 以0.1%甲酸水溶液和0.1%甲酸乙腈溶液为流动相进行梯度洗脱, 串联质谱分析中采用电喷雾离子源正离子模式和多反应监测模式。 结果 天然辣椒素、二氢辣椒素、合成辣椒素的质量浓度在0.1~100 μg/L内与其对应的峰面积呈线性关系, 检出限合成辣椒素为0.01 μg/kg, 天然辣椒素为0.006 μg/kg, 二氢辣椒素为0.005 μg/kg。以空白样品为基体进行加标回收实验, 回收率在80.3%~96.2%, 测定值的相对标准偏差(n=6)为4.48%~7.25%。结论 该方法快速、准确, 能满足食用油脂中辣椒素的快速筛查和检测要求。

英文摘要:

      Objective To establish a method for the determination of capsaicin in edible oils by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were dissolved in n-hexane, extracted with sodium hydroxide aqueous solution, and the basic extract was acidified by sulfuric acid and purified by PEP-2 solid-phase extraction column. The samples were detected by UPLC-MS/MS, and quantified by external standard method. ACQUITY UPLC BEH C18 column (3.0 mm×100 mm, 1.7 μm) was used as stationary phase, and 0.1% formic acid aqueous solution and 0.1% formic acid acetonitrile solution were used as mobile phase for gradient elution. Electrospray ion source positive ion mode and multi-reaction monitoring mode were used in tandem mass spectrometry. Results The mass concentrations of natural capsaicin, dihydrocapsaicin and nonivamide were in a linear relationship with their corresponding peak areas within the range of 0.1?100 μg/L. The limits of detection of nonivamide were 0.01 μg/kg, natural capsaicin 0.006 μg/kg and dihydrocapsaicin 0.005 μg/kg. The recovery experiments were carried out using the blank sample as the matrix. The recoveries were 80.3%?96.2%, and the relative standard deviations (n=6) of the measured values were 4.48%?7.25%. Conclusion This method is rapid and accurate, and can meet the requirements of rapid screening and detection of capsaicin in edible oils.