摘要
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ShimadzuVP-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 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 × 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. 072 64X ＋ 0. 006 22 and r = 0. 998 7 for adenine, Y = 0. 159 7X ＋ 0. 014 6 and r = 0. 999 1 for adenosine, Y=0. 194 2X ＋ 0. 018 6 and r = 0. 999 4 for cordycepin. The linear range was 0. 8-130.0 mg·L^-1, 0. 5- 124. 5 mg· L^-1 and 0. 5-128.5 mg ·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. sirtensis.
出处
《中国中药杂志》
CAS
CSCD
北大核心
2009年第18期2349-2352,共4页
China Journal of Chinese Materia Medica
基金
中国博士后科学基金项目(20060400887)
