静电离子色谱法测定草乌药材中新乌头碱、次乌头碱及乌头碱含量  

Determination of mesaconitine,hypaconitine and aconitine in Aconiti Kusnezoffii Radix by electrostatic ion chromatography

作　　者：张玉荣[1] 王瑞忠 何轶[3] 张聿梅[3] 鲁静[3] ZHANG Yu-rong;WANG Rui-zhong;HE Y;ZHANG Yu-mei;LU Jing(The First Affiliated Hospital of Xi’an Medical University,Xi’an 710077,China;Xi’an Daxing Hospital,Xi’an 710016,China;National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]西安医学院第一附属医院,西安710077 [2]西安大兴医院,西安710016 [3]中国食品药品检定研究院,北京100050

出　　处：《药物分析杂志》2020年第7期1319-1324,共6页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:优化《中华人民共和国药典》2015年版草乌含量测定项下方法,并测定草乌中新乌头碱、次乌头碱及乌头碱的含量。方法:采用Xcharge C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.05%磷酸水溶液为流动相进行梯度洗脱,流速1 mL·min^-1,柱温30℃,检测波长235 nm。结果:新乌头碱、次乌头碱及乌头碱的检测下限分别为2.68、3.49和7.14μg·g^-1,线性范围分别为20.9~1045μg·mL^-1(r=0.9999)、15.12~756μg·mL^-1(r=0.9999)、9.43~471.5μg·mL^-1(r=0.9999),回收率分别为98.3%、97.7%和97.6%;3批样品中新乌头碱、次乌头碱及乌头碱的含量范围分别为3.51~4.85、1.23~1.44、0.40~0.74 mg·g^-1。结论:本研究建立的高效液相色谱方法稳定可靠,分析时间短,可用于草乌药材中双酯型生物碱的含量测定。Objective:To optimize the determination method of mesaconitine,hypaconitine and aconitine in Aconiti Kusnezoffii Radix in Chinese Pharmacopoeia 2015 Edition.Methods:A Xcharge C18(4.6 mm×250 mm,5μm)column was adopted for the test,and a mixture of acetonitrile and 0.05%aqueous phosphoric acid was used as the mobile phase with gradient elution at a flow rate of 1 mL·min^-1.The column temperature was 30℃and the detection wavelength was 235 nm.Results:The detection limits of mesaconitine,hypaconitine and aconitine were 2.68μg·g^-13.49μg·g^-1 and 7.14μg·g^-1,respectively.The linear relationships of mesaconitine,hypaconitine and aconitine were observed in the ranges of 20.9^-1045μg·mL^-1,15.12-756μg·mL^-1 and 9.43-471.5μg·mL^-1.The average recoveries of mesaconitine,hypaconitine and aconitine were 98.3%,97.7%and 97.6%,respectively.The contents of mesaconitine,hypaconitine and aconitine were 3.51-4.85 mg·g^-1,1.23^-1.44 mg·g^-1,0.40-0.74 mg·g^-1,respectively.Conclusion:The developed HPLC method is stable,reliable and fast,which can be used for the determination of diester-alkaloids in Aconiti Kusnezoffii Radix.

关 键 词：草乌 新乌头碱 次乌头碱 乌头碱 双酯型生物碱 含量测定 静电离子色谱法 

分 类 号：R917[医药卫生—药物分析学]