化学衍生辅助液相色谱-串联质谱测定枇杷膏中的齐墩果酸和熊果酸

建立了一种液相色谱-串联质谱(LC-MS/MS)同时测定齐墩果酸和熊果酸含量的分析方法,利用衍生化试剂N,N-二甲基乙二胺(DMED)和d4-N,N-二甲基乙二胺(d4-DMED)分别衍生样品和标准工作溶液中的目标分析物,并将标准工作液的衍生产物作为稳定同位素内标。该方法线性关系良好,相关系数均0.99;齐墩果酸和熊果酸的检出限(S/N=3)分别为0.92 ng/L和1.06 ng/L,加标回收率分别为98.7%~102.7%和97.2%~105.0%。该方法简单、快速、准确,可满足枇杷膏中齐墩果酸和熊果酸高灵敏度检测的需求。

Determination of oleanolic acid and ursolic acid in loquat leaf extract by chemical derivatization coupled with liquid chromatography-tandem mass spectrometry

A method for the determination of oleanolic acid (OA) and ursolic acid (UA) by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. By using derivatization reagents, N,N-dimethylethylenediamine (DMED) and d4-N,N-dimethylethylenediamine (d4-DMED), OA and UA in real samples and standard samples were derivatized separately. The derivative products of the standard samples were used as stable isotope internal standards, and accurately added to the samples and standard working solutions. Good linearities were obtained in the concentration range of 0.01-10 μ g/L with correlation coefficients (r²) greater than 0.99. The limits of detection of OA and UA were 0.92 ng/L and 1.06 ng/L, and the recoveries were between 98.7%-102.7% and 97.2%-105.0%, respectively. The method can be used for the detection of OA and UA in loquat leaf extract with high sensitivity.