Simultaneous separation and determination of active components in Cordyceps sinensis and Cordyceps militarris by LC/ESI-MS
Simultaneous separation and determination of active components in Cordyceps sinensis and Cordyceps militarris by LC/ESI-MS
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DOI：
10.1016/s0731-7085(03)00415-1
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发表时间：
2003-12-04
影响因子：
3.4
通讯作者：
Cheng, BM
中科院分区：
文献类型：
--
作者：
Huang, LF;Liang, YZ;Cheng, BM
建立了一种简便、快速的等度液相色谱/质谱联用（LC/MS）-电喷雾离子化（ESI）法同时分离测定冬虫夏草及其代用品中腺嘌呤、次黄嘌呤、腺苷和虫草素的方法。2-使用氯腺苷作为该测定的内标物。以水-甲醇-甲酸（85：14：1，v/v/v）为移动的流动相，Shimadzu VP-ODS色谱柱（2.0 × 150 mm）为分离柱。采用选择性离子监测（SIM）模式（[M +H]（+）m/z 136、137、268、252和302）对上述四种活性成分进行定量分析。腺嘌呤、次黄嘌呤、腺苷和虫草素的线性范围分别为1.4-140.0 μ g/ml、0.6-117.5 μ g/ml、0.5-128.5 μ g/ml和0.5-131.5 μ g/ml。腺嘌呤的定量限和检测限分别为1.4和0.5 μ g/ml，次黄嘌呤为0.6和0.2 μ g/ml，腺苷和虫草素为0.5和0.1 μ g/ml。4种成分的回收率在93.5 ~ 107.0%之间。用该方法测定了天然铯及其替代物中的核苷含量，并进行了比较。(C)2003 Elsevier B. V.保留所有权利。
A simple and rapid isocratic LC/MS coupled with electrospray ionization (ESI) method for simultaneous separation and determination of adenine, hypoxanthine, adenosine and cordycepin in Cordyceps sinensis (Cs) and its substitutes was developed. 2-Chloroadenosine was used as internal standard for this assay. The optimum separation for these analytes was achieved using the mixture of water, methanol and formic acid (85:14:1, v/v/v) as a mobile phase and a 2.0 x 150 mm Shimadzu VP-ODS column. Selective ion monitoring (SIM) mode ([M +H](+) at m/z 136, 137, 268, 252 and 302) was used for quantitative analysis of above four active components. The regression equations were liner in the range of 1.4-140.0 mug ml(-1) for adenine, 0.6-117.5 mug ml(-1) for hypoxanthine, 0.5-128.5 mug ml(-1) for adenosine and 0.5-131.5 mug ml(-1) for cordycepin. The limits of quantitation (LOQ) and detection (LOD) were, respectively 1.4 and 0.5 mug ml(-1) for adenine, 0.6 and 0.2 mug ml(-1) for hypoxanthine, 0.5 and 0.1 mug ml(-1) for adenosine and cordycepin. The recoveries of four constituents were from 93.5 to 107.0%. The nucleoside contents of various types of natural Cs and its substitutes were determined and compared with this developed method. (C) 2003 Elsevier B.V. All rights reserved.