摘要
目的:对肺抑瘤合剂进行薄层鉴别及定量测定,建立合理可行的质量控制方法与标准。方法:采用薄层色谱法(TLC)对制剂中黄芪、薏苡仁、浙贝母、甘草进行定性鉴别;建立测定肺抑瘤合剂中指标性成分黄芪甲苷的高效液相色谱-蒸发光散射检测(HPLC-ELSD)方法;采用Agilent ZORBAXSB-C_(18)色谱柱(4. 6 mm×250 mm,5μm),流动相为乙腈-水(32∶68),流速为1. 0 mL/min,柱温为25℃。ELSD参数:漂移管温度为90℃,雾化温度为40℃,氮气流速为1. 20 L/min。结果:TLC图斑点清晰,专属性强,能有效鉴别4味药材;黄芪甲苷进样量在0. 9160~9. 1600μg范围内与峰面积线性关系良好,回归方程为l gY=1. 418l g X+2. 480,r=0. 999 5,平均加样回收率为96. 99%,RSD为0. 96%(n=6)。结论:建立的鉴别和含量测定方法专属性强、重复性好、简便准确,可作为控制肺抑瘤合剂质量的方法。
Objective: To establish the rational and feasible method and standard of quality control by performingthin-layer chromatography (TLC) identification and quantitative determination of pulmonary tumor-inhibitingmixture. Methods: HuangQi[Astragalus membranaceus (Fisch.) Bunge.], Yiyiren (semen coicis), ZheBeiMu (Fritillariathunbergii Miq.) and GanCao (licorice) in the preparations were identified qualitatively by TLC, and HPLC-ELSDmethod of indicative components Astragaloside A contained in pulmonary tumor-inhibiting mixture was established,AgilentZORBAX SB-C18 chromatographic column (4.6 mm×250 mm,5 μm) was used, acetonitrile-water (32:68) asmobile phase, flow velocity was 1.0 mL/min, column temperature was 25℃. ELSD parameters: the temperature ofdrift tube was 90℃, atomization temperature 40℃, nitrogen velocity was 1.20 L/min. Results: TLC spots were clearwith strong specialization, and four kinds of herbs could be effectively identified; astragaloside A was in good linearrelationship in the peak area and the range from 0.916 0 to 9.1600 μg, regression equation was lgY=1.418lgX +2.480, r=0.999 5, average sample recovery was 96.99%, RSD was 0.96%(n=6). Conclusion: The established identifi-cation and content determination methods, which are specific, reproducible, simple and accurate, could be taken asthe method of controlling the quality of pulmonary tumor-inhibiting mixture.
作者
隋晓丽
张红艳
田晓倩
彭召云
李芳
刘健
郑心
SUI Xiaoli;ZHANG Hongyan;TIAN Xiaoqian;PENG Zhaoyun;LI Fang;LIU Jian;ZHENG Xin(The Second Affiliated Hospital to Shandong University of Traditional Chinese Medicine,Jinan 250001,China;Shandong University of Traditional Chinese Medicine)
出处
《西部中医药》
2018年第9期46-50,共5页
Western Journal of Traditional Chinese Medicine
基金
山东省科技计划项目(编号2014GSF119015)
济南市科技计划项目(编号201602185)