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

doi:10.3724/SP.J.1123.2016.08015

色谱 ›› 2017, Vol. 35 ›› Issue (1): 27-31.DOI: 10.3724/SP.J.1123.2016.08015

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

骆丹^1,2, 冯钰锜¹, 姚劲挺², 孙友宝², 黄涛宏², 端裕树²

1. 生物医学分析化学教育部重点实验室, 武汉大学化学与分子科学学院, 湖北武汉 430072;
2. 岛津企业管理(中国)有限公司, 上海 200052

收稿日期:2016-08-16 出版日期:2017-01-08 发布日期:2013-05-06
通讯作者: 冯钰锜,Tel:(027)68755595,E-mail:yqfeng@whu.edu.cn.
基金资助:
国家自然科学基金项目（21475098）.

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

LUO Dan^1,2, FENG Yuqi¹, YAO Jinting², SUN Youbao², HUANG Taohong², HASHI Yuki²

1. Key Laboratory of Analytical Chemistry for Biology and Medicine(Ministry of Education), College of Chemistry and Molecular Science, Wuhan University, Wuhan 430072, China;
2. Shimadzu(China) Co., Ltd., Shanghai 200052, China

Received:2016-08-16 Online:2017-01-08 Published:2013-05-06
Supported by:
National Natural Science Foundation of China (No. 21475098).

摘要/Abstract

摘要：

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。

关键词: 化学衍生, 齐墩果酸, 同位素质谱探针标记技术, 熊果酸, 液相色谱-串联质谱

Abstract:

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.

Key words: chemical derivatization, isotope mass spectrometer probe technology, liquid chromatography-tandem mass spectrometry (LC-MS/MS), oleanolic acid (OA), ursolic acid (UA)

中图分类号:

O658

骆丹, 冯钰锜, 姚劲挺, 孙友宝, 黄涛宏, 端裕树. 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[J]. 色谱, 2017, 35(1): 27-31.

LUO Dan, FENG Yuqi, YAO Jinting, SUN Youbao, HUANG Taohong, HASHI Yuki. Determination of oleanolic acid and ursolic acid in loquat leaf extract by chemical derivatization coupled with liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2017, 35(1): 27-31.

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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

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

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