水浴皂化-气相色谱-质谱法测定杏仁油中的角鲨烯

Determination of Squalene in Almond Oil by Water Bath Saponification Combined with Gas Chromatography-mass Spectrometry

基于水浴皂化,建立了测定杏仁油中角鲨烯的气相色谱-质谱法(GC-MS)。样品经氢氧化钠-乙醇皂化后,环己烷提取,GC-MS测定。采用电子轰击离子源(EI)进行电离,选择离子对模式进行测定。角鲨烯在0.1~10 mg/L范围内,相关系数r^(2)为0.9992。加标回收实验的回收率结果为92.8%~98.6%之间,相对标准偏差(RSD)为2.70%~5.31%。方法检出限为2.0 mg/kg,方法定量限为5.0 mg/kg。方法学实验结果及灵敏度能满足一般杏仁油样品的测定。

A gas chromatography-mass spectrometry(GC-MS)method for the determination of squalene in almond oil was established based on water bath saponification.The samples were saponified with sodium hydroxide-ethanol,then extracted with cyclohexane and determined by GC-MS.Electron impact ionization(EI)was used for ionization and the measurement was performed in selected ion pair mode.The correlation coefficient r^(2) of squalene was 0.9992 in the range of 0.1~10 mg/L.The recovery results of the spiked recovery experiment were between 92.8%and 98.6%,while the relative standard deviation(RSD)was 2.70%to 5.31%.The method detection limit was 2.0 mg/kg and the method quantification limit was 5.0 mg/kg.The experimental results and sensitivity of the methodology could meet the determination of general almond oil samples.