C30-HPLC-PDA-TOF/MS对鱼肝油中维生素A酯顺反异构体的分离与鉴定

Separation and identification of cis-trans isomers of retinyl esters in fish liver oil by C30-HPLC-PDA-TOF/MS

目的:建立高效液相色谱/飞行时间质谱法对鱼肝油中不同维生素A酯的顺反异构体进行分离鉴定。方法:选择YMC C30色谱柱(250 mm×4.6 mm,5μm),以甲基叔丁基醚-甲醇-水为流动相梯度洗脱,对鱼肝油中各种维生素A酯进行分离,结合电喷雾正离子化/飞行时间质谱法进行结构推断。并通过对照品比对等方法,对分离得到的顺反异构体做构型鉴定。结果:在本试验研究的2种样品中,鳕鱼肝油胶囊中主要含有全反式与13-顺式维生素A棕榈酸酯,鲨鱼肝油中主要含有全反式与13-顺式维生素A油酸酯、棕榈酸酯与硬脂酸酯,以及全反式花生烯酸酯与十七烷酸酯。结论:本方法能有效地分离鉴定鱼肝油中的多种全反式与13-顺式维生素A酯,可为鱼肝油质量控制提供参考依据。

Objective:To develop an HPLC-TOF/MS method for the separation and identification of cis-trans isomers of retinyl esters in fish liver oil. Methods:The retinyl esters were separated by gradient elution with a mobile phase of MTBE-methanol-water on a YMC C30(250 mm×4.6 mm,5 μm)column. The structures of retinyl esters in fish liver oil were elucidated by ESI+-TOF/MS and by comparing with reference substances. Results:Cod liver oil capsule contain all-trans and 13-cis retinyl palmitate. Shark liver oil contains all-trans retinyl oleate,retinyl palmitate,retinyl stearate,retinyl gondoate,retinyl heptadecanoate and 13-cis retinyl oleate,retinyl palmitate,retinyl stearate. Conclusion:The established method is useful for the separation and identification of all-trans and 13-cis retinyl esters in fish liver oil. The results obtained are valuable for its manufacturing process and quality control.