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目的:建立同时快速测定冬虫夏草中腺嘌呤、腺苷和虫草素含量的方法。方法:LC-ESI-MS法,采用选择性离子检测(SIM)和电喷雾离子化(ESI),色谱条件为Sh im adzuVP-ODS色谱柱;流动相为水-甲醇-甲酸(92∶7∶1),以甲醇为提取溶剂和2-氯腺苷为内标。结果:腺嘌呤线性回归方程为Y=0.072 64X+0.006 22,线性范围为0.8~130.0 mg.L-1,r=0.998 7;腺苷线性回归方程为Y=0.159 7X+0.014 6,线性范围为0.5~124.5 mg.L-1,r=0.999 1;虫草素线性回归方程为Y=0.194 2X+0.018 6,线性范围为0.5~128.5 mg.L-1,r=0.999 4;腺嘌呤、腺苷和虫草素的加标回收率分别为98.76%,99.37%和99.26%。结论:方法灵敏、快速和选择性好,可用于同时快速测定冬虫夏草中腺嘌呤、腺苷和虫草素含量及质量控制。
Objective: To establish a rapid and rapid method for the determination of adenine, adenosine and cordycepin in Cordyceps sinensis. Methods: The LC-ESI-MS method was performed on SIM-ESI and ESI on Chimodzu VP-ODS column. The mobile phase was water-methanol-formic acid 1), methanol as extraction solvent and 2-chloro-adenosine as internal standard. Results: The linear regression equation of adenine was Y = 0.072 64X + 0.006 22, the linear range was 0.8-130.0 mg.L-1, r = 0.998 7, the linear regression equation of adenine was Y = 0.159 7X + 0.014 6, the linear range was 0.5 ~ 124.5 mg.L-1 and r = 0.999 1 respectively. The linear regression equation of cordycepin was Y = 0.194 2X + 0.018 6 with a linear range of 0.5 ~ 128.5 mg.L-1 and r = 0.999 4. And Cordycepin spiked recoveries were 98.76%, 99.37% and 99.26%, respectively. Conclusion: The method is sensitive, rapid and selective. It can be used for simultaneous determination of adenine, adenosine and cordycepin in Cordyceps sinensis and its quality control.