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作 者:李俊[1] 苑红燕[1] 王军 刘江云[1] 蔡培烈[1] 杨世林[1,2]
机构地区:[1]苏州大学药学院,江苏苏州215123 [2]贵州益佰制药有限公司,贵州贵阳550001
出 处:《苏州大学学报(自然科学版)》2011年第2期86-89,94,共5页Journal of Soochow University(Natural Science Edition)
基 金:科技部国家科技合作计划项目(2008TR1157)
摘 要:目的:采用HPLC-ELSD分析方法,通过正交设计试验优化斑蝥中斑蝥素的提取工艺.方法:以斑蝥素含量为指标,通过正交实验确定最佳提取工艺.采用HPLC-ELSD法检测斑蝥中斑蝥素的含量,Cosmosil 5C18-AR-Ⅱ(250mm×4.6)色谱柱分离,流动相体积比为V(甲醇):V(水)=2∶3,等度洗脱,流速1.0 mL/m in.结果:最佳提取条件为药材加6倍量丙酮在25℃条件下提取3次,每次3h.斑蝥素的线性范围为2.04~20.4μg(r=0.999 1),检测限为0.48μg,加样回收率为97.9%~99.2%,相对标准偏差为1.7%~2.5%.结论:该提取工艺合理,HPLC-ELSD检测方法简便快速、结果准确、重现性好.Objective:The extraction process of cantharidin in Mylabris cichorii was optimized by orthogonal experiment design,a HPLC-ELSD method was established to determine the amount of cantharidin.Methods:The optimum extraction method of cantharidin in Mylabris cichorii was developed by orthogonal experiment.The HPLC separation of cantharidin was achieved on a Cosmosil 5C18-AR-Ⅱ(250mm×4.6) column,using V(CH3OH)∶V(H2O)= 2∶3 as the mobile phase at a flow rate of 1.0 mL/min.Result:The extraction process was optimized as: the material was extracted 3 times by 6 volume acetone in 25 ℃,each time 3 h.As for HPLC-ELSD analysis,the linear detection range was 2.04~20.4 μg(r=0.999 1),the limit of detection(LOD) was 0.48 μg,the average recoveries and relative standard deviations(RSD) were 97.9%~99.2%,and 1.7%~2.5%,respectively.Conclusion:This extraction process is efficient.HPLC-ELSD analysis is quick,simple and accurate.
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