气相色谱-串联质谱法测定植物油中角鲨烯的含量
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.
标题：气相色谱-串联质谱法测定植物油中角鲨烯的含量
英文标题：Determination of squalene in vegetable oil by gas chromatography-tandem mass spectrometry
作者：
黎斌 绿城农科检测技术有限公司
刘小羽 绿城农科检测技术有限公司
俞璐萍 绿城农科检测技术有限公司
刘亚楠 绿城农科检测技术有限公司
王卢燕 绿城农科检测技术有限公司
桑力青 绿城农科检测技术有限公司
杨婷婷 南京市产品质量监督检验院,国家农副产品质量监督检验中心
朱萌萌 绿城农科检测技术有限公司
中文关键词:角鲨烯,净化,稳定性,气相色谱-串联质谱法,
英文关键词:squalene,purification,stability,gas chromatography-tandem mass spectrometry,
发表日期：2020-02-22
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