高效液相色谱法测定苦木注射液中7种生物碱含量  

Simultaneous Determination of Seven Alkaloids in Kumu Injection by HPLC

作　　者：赖正权 艾伟鹏 廖慧君 廖祝元 丘金燕 蔡雨峰 杨婷婷 黄裕茵 廖醒环 苏子仁 LAI Zhengquan;AI Weipeng;LIAO Huijun;LIAO Zhuyuan;QIU Jinyan;CAI Yufeng;YANG Tingting;HUANG Yuyin;LIAO Xinghuan;SU Ziren(Department of Pharmacy,General Hospital,Shenzhen University,Shenzhen 518055,China;Department of Clinical Pharmacy and Pharmaceutical Services,Union Shenzhen Hospital,Huazhong University of Science and Technology(the 6th Affiliated Hospital of Shenzhen University),Shenzhen 518052,China;Jiangxi Qingfeng Pharmaceutical Co.Ltd,Ganzhou 341000,China;Guangzhou University of Chinese Medicine,Mathematical Engineering Academy of Chinese Medicine,Guangzhou 510006,China)

机构地区：[1]深圳大学总医院药学部,深圳518055 [2]华中科技大学协和深圳医院(深圳大学第六附属医院)药学部,深圳518052 [3]江西青峰药业有限公司,赣州341000 [4]广州中医药大学,中医药数理工程研究院,广州510006

出　　处：《医药导报》2021年第4期498-502,共5页Herald of Medicine

基　　金：深圳市科技计划项目(JCYJ20190808114807611);广东省自然科学基金面上项目(2019A1515010815);广东省普通高校青年创新人才类项目(2018KQNCX216)。

摘　　要：目的建立高效液相色谱(HPLC)法同时测定苦木注射液中1-甲酸-6-羟基-β-咔巴啉、1-甲酸-β-咔巴啉、1-丙酸基-β-咔巴啉、3-甲基-铁屎米-5,6-二酮、3-甲基-4-甲氧基-铁屎米-5,6-二酮、4-甲氧基-5-羟基铁屎米酮、4,5-二甲氧基-铁屎米酮共7种生物碱含量的方法。方法采用Phenomenex Gemini C_(18)色谱柱(250 mm×4.6 mm,5μm),甲醇-30 mmol·L^(-1)乙酸铵(冰醋酸调pH值4.5)溶液梯度洗脱;流速1.0 mL·min-1;柱温30℃;检测波长254 nm。结果7种生物碱浓度分别在1.00~30.00,5.10~153.00,0.76~22.80,0.38~11.40,0.24~7.20,0.40~12.00,0.10~3.00μg·mL^(-1)范围内与峰面积呈良好的线性关系(r≥0.9999),精密度、重复性良好,RSD均小于3%;在室温条件下48 h内稳定;平均加样回收率99.22%~101.65%,RSD 0.82%~2.21%。结论所建立的方法简便、准确、重复性良好,可用于该品种的质量评价。Objective To develop a HPLC method for the simultaneous determination of seven alkaloids(6-Hydroxy-β-Carboline-1-carboxylic acid,β-Carboline-1-carboxylic acid,β-Carboline-1-propanoic acid,3-Methylcanthin-5,6-dione,4-Methoxy-3-methylcanthine-5,6-dione,5-Hydroxy-4-methoxycanthin-6-one,4,5-Dimethoxycanthin-6-one)in Kumu injection.Methods The chromatographic analysis were performed on a Phenomenex Gemini C_(18)column(4.6 mm×250 mm,5μm)with the gradient elution solvent system composed of methanol and 30 mmol·L^(-1)aqueous ammonium acetate(adjusted with glacial acetic acid to pH 4.5).The flow rate of the mobile phase was 1.0 mL·min-1with the column temperature of 30℃,and the detection wavelength was set at 254 nm.Results These seven alkaloids were showed good linearities(r≥0.9999)within the concentration ranges tested(1.00-30.00,5.10-153.00,0.76-22.80,0.38-11.40,0.24-7.20,0.40-12.00,0.10-3.00μg·mL^(-1)).The RSD was less than 3%and the RSD was stable in 48 h at room temperature.The average recoveries were 99.22%~101.65%with the RSD between 0.82%-2.21%.Conclusion The method is simple,accurate and repeatable,which can be used for the quality evaluation of Kumu injection.

关 键 词：苦木注射液 生物碱 高效液相色谱法 含量测定 β-咔巴啉类生物碱 铁屎米酮类生物碱 

分 类 号：R286[医药卫生—中药学] R927.2[医药卫生—中医学]