加速溶剂萃取结合亲水交互色谱法同时测定油料种子中多种生育酚及生育三烯酚

Simultaneous determination of various tocopherols and tocotrienols in oil seeds by accelerated solvent extraction combined with hydrophilic interaction chromatography

该研究建立了一种加速溶剂萃取结合亲水交互作用色谱法同时测定油料种子中4种生育酚及4种生育三烯酚的方法。样品在110℃条件下经正己烷萃取180 s后,采用90%正己烷/10%叔丁基甲基醚-四氢呋喃-甲醇(20∶1∶0.1,V/V)流动相体系,经BEH Amide HILIC色谱柱分离,由荧光检测器外标法定量。结果表明,4种生育酚及4种生育三烯酚分别在0.5~80.0μg/mL、0.5~30.0μg/mL质量浓度范围内线性关系良好,相关系数R^(2)为0.995~0.999,检出限为32~70μg/kg,定量限为96~210μg/kg,加标回收率为86.3%~99.2%,相对标准偏差(RSD)为2.5%~6.1%。该方法具有操作简单、灵敏度高、回收率和重现性好、结果准确可靠的特点,可以满足油料种子中多种生育酚异构体定性和定量检测的需求。

A method for the determination of 4 tocopherols and 4 tocotrienols in oil seeds by accelerated solvent extraction combined with hydrophilic interaction chromatography was established.The sample was extracted with n-hexane at 110℃for 180 s,separated by BEH Amide HILIC column using 90%n-hexane/10%tert butyl methyl ether-tetrahydrofuran-methanol(20∶1∶0.1,V/V)as mobile phase,and quantified by external standard method with fluorescence detector.The results showed that the linearity of 4 tocopherols and 4 tocotrienols in the concentration range of 0.5-80.0μg/ml and 0.5-30.0μg/ml was good,respectively,the correlation coefficient R^(2)was 0.995-0.999,the detection limit was 32-70μg/kg,the quantitation limit was 96-210μg/kg,the standard recovery rate was 86.3%-99.2%,and the relative standard deviation(RSD)was 2.5%-6.1%.The method had the advantages of simple operation,high sensitivity,good recovery and reproducibility,and accurate and reliable results,which could meet the requirements of qualitative and quantitative detection of various tocopherol isomers in oil seeds.