气相色谱-串联质谱法测定植物油中角鲨烯的含量

Determination of squalene in vegetable oil by gas chromatography-tandem mass spectrometry

目的建立气相色谱-串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)测定植物油中角鲨烯化合物的方法。方法植物油样品经正己烷超声提取,中性氧化铝固相萃取柱(Alumina-N)净化,内标法定量。结果采用优化后的条件,角鲨烯在0.01~0.64 mg/kg的定量范围内,线性关系良好,相关系数在0.99以上。选取不同含量植物油样品(菜籽油、葵花籽油、花生油),在样品添加角鲨烯化合物浓度为10、100、200 mg/kg时,平均回收率为91.5%~106%,相对标准偏差小于4.6%。在正常的光照和室温条件下,角鲨烯在放置1、3、5 d后的浓度分别较0 d时降低了14.8%、20.7%和27.8%,在放置11、13、15 d后的浓度较0 d时降低了37.0%、39.0%和40.5%。结论该方法具有高效、快速、操作简单、实验成本低等优点,可以满足实验室内植物油中角鲨烯的快速、高通量检测。

Objective To establish a method for the determination of squalene compounds in vegetable oil by gas chromatography-tandem mass spectrometry(GC-MS/MS).Methods Samples of vegetable oil were extracted with hexane,and then a cleanup step using Alumina-N SPE cartridge was applied.The purified extract quantified by internal standard method.Results Under the optimized conditions,squalene had a good linear relationship in the quantitative range of 0.01–0.64 mg/kg,and the correlation coefficient was greater than 0.99.Selecting samples of vegetable oils with different contents(rapeseed oil,sunflower oil,peanut oil),when the concentration of squalene compound added to the samples was 10,100,200 mg/kg,the average recovery rates were 91.5%–106%,and the relative standard deviation was less than 4.6%.Under normal light and room temperature conditions,the concentrations of squalene after 1 d,3 d,and 5 d were decreased by 14.8%,20.7%,and 27.8%compared with 0 d,the concentrations of squalene after 11 d,13 d,and 15 d were decreased by 37.0%,39.0%and 40.5%compared with 0 d.Conclusion This method has the advantages of high efficiency,fast,simple operation and low experimental cost,and can meet the rapid and high-throughput detection of squalene in vegetable oil in the laboratory.