茶叶籽油中角鲨烯的定性与定量分析

Qualitative and Quantitative Analysis of Squalene in Tea Seed Oil

采用GC-MS分析茶叶籽油中不皂化物的成分,并采用高效液相色谱法对茶叶籽油中的角鲨烯进行定量分析。结果表明:茶叶籽油不皂化物的主要成分为角鲨烯、α-生育酚,另外还有合金欢醇、香叶里拉醇、羊毛甾醇、茉莉酮、D12齐墩果烯、2,4-二叔丁基苯酚及2,5-二叔丁基-1,4-苯醌等物质。通过C18柱分离样品中的角鲨烯,当流动相为甲醇/乙腈(60+40,V/V)、检测波长210 nm、流速2 m L/min、柱温30℃时,能有效分离茶叶籽油样品中的各组分,再经HPLC测得茶叶籽油中角鲨烯含量为4.1 mg/kg。当角鲨烯质量浓度在20~500 mg/L之间时,峰面积和质量浓度的线性关系较好,线性相关系数(R^2)为0.999 0;平均加标回收率为84.2%~90.1%,相对标准偏差(RSD)小于6.98%(n=4),此方法的测定低限(LOQ)为2.7 mg/kg。

The unsaponifiable matters of tea seed oil has been analyzed by GC -MS; squalene in tea seed oil has been determined by high performance liquid chromatography. The results showed that the main components of tea seed oil unsaponifiables were squalene and alpha tocopherol, In addition, there were small quantities of huisaehe alcohol, geranyl linalool, Lanosterin, cis - Jasmone, D12 oleanene, 2,4 - Di - tert - butylphenol and 2,5 - Di - tert -butyl-p -benzoquinone. The squalene in sample were separated from the other impurities by C18 column. On condition of that： the mobile phase of methanol/acetonitrile （60 ＋40, V/V）, the detection wavelength of 210 nm, the flow rate of 2 mL/min, the column temperature at 30℃, these should be chosed as determination conditions, the components in tea seed oil could be effectively separated. The squalene content in tea seed oil was 4.1 mg/kg measured by HPLC. The linear correlation between peak area and concentration of squalene was fine in concentration range of 20 - 500 mg/L with the linear correlation coefficient （R2 ） of 0.999 0. The average recoveries were 84.2% - 90.1%, relative standard deviation was less than 6.98% （n =4）, and the Limit of Quantity （LOQ） was 2.7 mg/kg.