超声波辅助提取植物油中甾醇和生育酚

Ultrasound-assisted extraction of sterols and tocopherol from edible oils

为优化食用植物油中主要营养物质的定量分析方法,建立了超声波辅助萃取LC-MS/MS测定食用油中植物甾醇和生育酚分析方法。在单因素实验的基础上,采取中心组合设计优化实验中超声时间和超声温度。通过优化分析得到食用油皂化提取豆甾醇、β-谷甾醇和δ-生育酚最优实验条件为：超声反应温度75℃,超声反应时间40min,功率100%。本方法中豆甾醇、β-谷甾醇、δ-生育酚的定量限分别为10.0ng/m L、10.0ng/m L和8.1ng/m L,相关系数均≥0.990 4,加标回收率在87.2%～97.8%之间,相对标准偏差为2.3%～8.6%。将建立的方法应用于茶籽油、紫苏子油、橄榄油、大豆油样品分析,结果表明本方法前处理操作简单且用时短、结果准确可靠,适用于食用植物油中主要甾醇和生育酚定量分析。

To optimize nutriment quantitative analysis in eadible oil,we developed an LC- MS / MS method coupled with ultrasonic extraction to analyze phytosterol and tocopherol. Central composite design was employed to optimize the extraction conditions including ultrasonic time and ultrasonic temperature. After systemic analysis,the optimized experimental conditions were obtained as follows： ultrasonic temperature at 75℃,ultrasonic time of 40 min and ultrasonic power of 100%. Validation indicated that the limits of detection（ LOQ） were 10. 0 ng / m L,10. 0 ng / m L and 8. 1 ng / m L for stigmasterol,β- sitosterol and δ- tocopherol respectively. Recoveries ranged from 87. 2% to 97. 8%. Correlation coefficients were higher than 0. 9904. And the relative standard deviations（ RSD） were 2. 3% to 8. 6%. Consequently the method was used to analyze stigmasterol,β- sitosterol and δ- tocopherol in camellia oil,petilla oil,olive oil and soybean oil. Results showed that this method was simple,rapid,accurate and reliable,which was a suitable method for quantitative analysis of main phytosterols and tocopherols in vegetable oil.