黄芪药材中黄芪甲苷UPLC-ELSD含量测定方法的优化  

Optimization of Determination of Astragaloside Ⅳ in Astragali Radix

作　　者：刘和平 彭招华 张润容 黄静 黄文漳 曹晖 

机构地区：[1]丽珠医药集团股份有限公司国家中药现代化工程技术研究中心,广东珠海519020

出　　处：《中国实验方剂学杂志》2015年第5期92-94,共3页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：广东省粤港关键领域重点突破项目(2010A032100001);广东省战略性新兴产业核心技术攻关项目(2011A081403002);国家工业和信息化部扶持中药材生产建设项目(工信消费函[2012]138号);广东省部产学研结合项目(2010A090200064)

摘　　要：目的:优化黄芪甲苷含量测定的供试液制备方法,建立黄芪药材中黄芪甲苷UPLC-ELSD含量测定的方法。方法:采用UPLC-ELSD测定黄芪甲苷含量流动相乙腈-水(32∶68),柱温30℃,流速0.5 m L·min-1,ELSD检测器温度45℃,载气干燥压缩空气,压力0.5 k Pa,增益值7。采用甲醇和氨水混合超声提取黄芪中黄芪甲苷,经正丁醇萃取,通过单因素试验优选供试品溶液的制备方法。结果:供试品制备方法为加甲醇80 m L和浓氨水40 m L,超声提取30 min,用水饱和正丁醇萃取4次,每次40 m L。采用优化的方法测得11批样品中黄芪甲苷含量明显高于2010年版《中国药典》黄芪项下含测方法的结果。结论:优化的供试液制备方法操作简单、有效成分损失少。建立的含量测定方法准确可靠、灵敏度高。Objective： To optimize sample solution preparation method and establish assay method of astragaloside IV in Astragali Radix. Method： UPLC-ELSD was used to determine the content of astragaloside IV with mobile phase of acetonitrile-water （32： 68） , column temperature of 30℃ , flow rate of 0.5 mL ·min-1 , temperature of ELSD at 45 ℃ , carrier gas was dry compressed air with pressure of 0.5 kPa, gain value was 7. Ammonia-methanol mixture was used to ultrasonic extract of astragaloside IV as well as n-butanol extraction. Preparation method of test solution was optimized through single-factor tests. Result： Optimal preparation method was as following： added methanol 80 mL and concentrated ammonia 40 mL, ultrasonic extraction for 30 rain, purification by subsequent extraction with n-butanol for four times every 40 mL in sample preparation. The content of astragaloside IV from 11 batches of Astragali Radix by this optimizing method were significantly higher than the result determined by HPLC method in 2010 edition of Chinese Pharmacopoeia. Conclusion： This optimized sample preparation method is simple with less loss of effective constituents. UPLC analysis method is accurate and reliable with high sensitivity.

关 键 词：黄芪 黄芪甲苷 含量测定 供试液 单因素试验 

分 类 号：R284.1[医药卫生—中药学]