Department of Chemistry and Pharmaceutical, Quzhou College, Quzhou 324000, China.
Molecules. 2010 Jan 13;15(1):305-14. doi: 10.3390/molecules15010305.
A sensitive, selective and reliable liquid chromatography-mass spectrometry coupled with electrospray ionization interface method for simultaneous separation and determination of thymine, adenine, adenosine and cordycepin in Cordyceps sinensis has been established. The optimum separation for these analytes was achieved using a gradient elution system and a 2.0 x 150 mm Shimadzu VP-ODS column. 2-Chloroadenosine was used as internal standard for this assay. [M+H]+ ions at m/z 127, 136, 268, 252 and 302 were chosen and selective ion monitoring (SIM) mode was used for quantitative analysis of the four main nucleosides. The regression equations were linear in the range of 1.0-117.5 microg x mL(-1) for thymine, 1.8-127.0 microg x mL(-1) for adenine, 0.6-114.0 microg x mL(-1) for adenosine and 0.5-107.5 microg x mL(-1) for cordycepin. The limits of quantitation (LOQ) and detection (LOD) were 1.0 and 0.2 microg x mL(-1) for thymine, 1.8 and 0.6 microg x mL(-1) for adenine, 0.6 and 0.1 microg x mL(-1) for adenosine and 0.5 and 0.1 microg x mL(-1) for cordycepin, respectively. The recoveries of the four nucleosides ranged from 98.47 to 99.32%. The developed method was successfully used to determine nucleosides in Cordyceps sinensis from different sources.
建立了一种灵敏、选择性好、可靠的液相色谱-质谱联用（LC-MS）电喷雾接口法，用于同时分离和测定冬虫夏草中的胸腺嘧啶、腺嘌呤、腺苷和蛹虫草素。采用梯度洗脱系统和 2.0×150mm Shimadzu VP-ODS 柱对这些分析物进行了最佳分离。2-氯腺苷作为该测定的内标。选择 [M+H]+离子在 m/z 127、136、268、252 和 302 处，并采用选择离子监测（SIM）模式对四种主要核苷进行定量分析。胸腺嘧啶的回归方程在 1.0-117.5μg·mL-1范围内呈线性，腺嘌呤在 1.8-127.0μg·mL-1范围内呈线性，腺苷在 0.6-114.0μg·mL-1范围内呈线性，蛹虫草素在 0.5-107.5μg·mL-1范围内呈线性。定量限（LOQ）和检测限（LOD）分别为 1.0 和 0.2μg·mL-1，1.8 和 0.6μg·mL-1，0.6 和 0.1μg·mL-1，0.5 和 0.1μg·mL-1。四种核苷的回收率在 98.47%至 99.32%之间。该方法成功地用于测定不同来源的冬虫夏草中的核苷。
