蛹虫草及其培养残基中腺苷和虫草素含量的快速测定  

Fast determination of adenosine and cordycepin in Cordyceps and its deserted solid medium

作　　者：李辰[1,2] 闫爱国 蔡春燕 刘志平[2] 

机构地区：[1]广东工业大学轻工化工学院,广东广州510006 [2]五邑大学分析测试中心,广东江门529020 [3]江门市农产品质量监督检验测试中心,广东江门529000 [4]江门市农业环境监测站,广东江门529000

出　　处：《色谱》2012年第7期711-715,共5页Chinese Journal of Chromatography

基　　金：广东高校优秀青年创新人才培育项目(LYM09130);五邑大学博士启动项目(30613016)

摘　　要：建立了以氰基正相色谱柱反相条件下快速分析腺苷和虫草素的方法。以微波辅助提取蛹虫草及其培养残基样品,每次提取1.5 min,共提取2次。采用Eclipse XDB-CN色谱柱测定提取液中腺苷和虫草素的含量,以甲醇-水(7∶93,v/v)为流动相进行等度洗脱,检测波长260 nm,并考察和分析了影响分离性能的流动相组成和pH值。结果腺苷和虫草素在4.5 min内实现完全分离且无基质干扰。腺苷和虫草素在线性范围内线性关系良好,线性相关系数r2分别为0.999 8和0.999 5,定量限(以10倍信噪比计)分别为0.21 mg/L(腺苷)和0.083 mg/L(虫草素)。该方法日内和日间精密度的相对标准偏差(RSD)小于2%;腺苷和虫草素的平均加标回收率为93.8%～102.9%,RSD值不大于3.62%(n=5)。本方法简便、快速、准确、成本低,可用于冬虫夏草、蛹虫草子实体、虫草培养残基及虫草制剂中腺苷和虫草素含量的快速测定。A fast analytical method for adenosine and cordycepin in Cordyceps and its deserted solid medium was developed by using a normal-phase cyan-group chromatographic column.The sample was extracted for 1.5 min using a microwave-assisted extraction system.The extraction was repeated twice.The analysis of adenosine and cordycepin was performed on an Eclipse XDB-CN column.The mobile phase was composed of methanol and water with a ratio of 7∶93（v/v） for isocratic elution.The detection wavelength was 260 nm.The composition and pH value of the mobile phase were investigated.The results showed that adenosine and cordycepin could be completely separated without matrix interference in 4.5 min.The linearity of the method was good with a linear correlation coefficient（r2） of 0.999 8 for adenosine and 0.999 5 for cordycepin.The limits of quantification（LOQs,S/N=10） of adenosine and cordycepin were 0.21 and 0.083 mg/L,respectively.The relative standard deviations（RSDs） of peak areas of six replicate injections were less than 2% both for intra-day and inter-day analysis.The average recoveries of adenosine and cordycepin ranged from 93.8% to 102.9% with the RSD not more than 3.62%（n=5）.The developed method is simple,fast,accurate and low-cost,and it can be used in the fast detection of adenosine and cordycepin in Cordyceps,carpohole,the deserted solid medium and its praeparatum.

关 键 词：正相色谱柱 腺苷 虫草素 蛹虫草 培养残基 

分 类 号：O658[理学—分析化学]