[采用液相色谱-电喷雾电离质谱法快速同时测定冬虫夏草中的主要核苷]

[Rapid simultaneous determination of main nucleosides in Cordyceps sinensis with LC-ESI-MS].

作者信息

Zhou Jufeng, Huang Lanfang, Guo Fangqiu

机构信息

Department of Biochemistry, Xiangnan College, Chenzhou 423000, China.

出版信息

Zhongguo Zhong Yao Za Zhi. 2009 Sep;34(18):2349-52.

PMID:20030086

Abstract

OBJECTIVE

To establish an LC-MS method for rapid simultaneous determination of adenine,adenosine and cordycepin in Cordyceps sinensis.

METHOD

An electrospray ionization (ESI) interface and selective ion monitoring (SIM) mode were used. The analytical column was a Shimadzu VP-ODS column (2.0 mm x 150 mm) and the mobile phase was water-methanol-formic acid (92:7:1). Methanol was used as extraction solvent and 2-chloroadenosine was used as internal standard for this assay.

RESULT

The regression equations and coefficient were Y = 0.07264X + 0.00622 and r = 0.9987 for adenine, Y = 0.1597X + 0.0146 and r = 0.9991 for adenosine, Y = 0.1942X + 0.0186 and r = 0.9994 for cordycepin. The linear range was 0.8-130.0 mg x L(-1), 0.5 - 124.5 mg x L(-1) and 0.5-128.5 mg x L(-1) for adenine, adenosine and cordycepin, respectively. The average recovery was 98.76%, 99.37% and 99.26% for adenine, adenosine and cordycepin, respectively.

CONCLUSION

This established method was highly sensitive, fast and selective, which can be used for rapid simultaneous determination of adenine, adenosine and cordycepin in C. sinensis. This method also can be applied for the quality control of C. sinensis.

摘要

目的

建立一种液相色谱-质谱联用（LC-MS）方法，用于快速同时测定冬虫夏草中的腺嘌呤、腺苷和虫草素。

方法

采用电喷雾电离（ESI）接口和选择离子监测（SIM）模式。分析柱为岛津VP-ODS柱（2.0 mm×150 mm），流动相为水-甲醇-甲酸（92:7:1）。本实验以甲醇为提取溶剂，2-氯腺苷为内标。

结果

腺嘌呤的回归方程和系数分别为Y = 0.07264X + 0.00622，r = 0.9987；腺苷的回归方程和系数分别为Y = 0.1597X + 0.0146，r = 0.9991；虫草素的回归方程和系数分别为Y = 0.1942X + 0.0186，r = 0.9994。腺嘌呤、腺苷和虫草素的线性范围分别为0.8 - 130.0 mg·L⁻¹、0.5 - 124.5 mg·L⁻¹和0.5 - 128.5 mg·L⁻¹。腺嘌呤、腺苷和虫草素的平均回收率分别为98.76%、99.37%和99.26%。