摘要
目的建立阿那日五味散中化学成分定性鉴别及安石榴苷含量测定的方法。方法以胡椒碱为对照品,以甲苯-乙酸乙酯-丙酮为展开系统对制剂中荜茇药材进行薄层鉴别。建立阿那日五味散中安石榴苷高效液相色谱(HPLC)的测定方法,色谱柱为Agilent C 18柱(4.6 mm×250 mm,5μm),流动相为甲醇-0.1%三氟乙酸,梯度洗脱,进样量为10μL,柱温30℃,于370 nm波长处检测,流速为1.0 mL/min。结果展开系统为甲苯-乙酸乙酯-丙酮(7∶2∶1),薄层色谱中胡椒碱的斑点清晰,与相邻斑点分离较好,阴性无干扰。安石榴苷浓度在8.297~531.000μg/mL范围内与峰面积的线性关系良好(r=0.9996),平均加样回收率为98.3%,RSD值为2.0%(n=6)。阿那日五味散中安石榴苷的平均含量为(44.48±1.73)mg/g。结论本研究建立的TLC鉴别方法适用于制剂中胡椒碱的鉴别,HPLC方法简便、快速、准确,适用于制剂中的安石榴苷的含量测定。
ObjectiveTo establish a method for qualitative identification of chemical constituents and content determination of punicalagin in Anari Wuwei powders.MethodsPiperine was used as the reference substance and toluene-ethyl acetate-acetone was used as the development system for TLC identification of piperine in the preparation,and methodological investigation was carried out.Punicalagin was determined by high performance liquid chromatography(HPLC).The HPLC analysis was performed with an Agilent C 18 column(250 mm×4.6 mm,5μm).Methanol-0.1%trifluoroacetic acid was used as mobile phase and gradient elution was carried out.The flow rate was set at 1.0 mL/min,the column temperature was 30℃,the detection wavelength was 370 nm,and the injection volume was 10μL.ResultsThe expansion system is toluene-ethyl acetate-acetone(7∶2∶1).The spots of piperine in the thin layer chromatography were clear,and the separation from the adjacent spots was good and the negative was not polluted.The mass concentration of angarnet glycosides was shown to have a good linear relationship with the peak area in the range of 8.297~531.000μg/mL(r=0.9996),and its average sample recovery rate was 98.3%,and the RSD value was 2.0%(n=6).The average content of Angarnet glycosides in Anawei powder was(44.48±1.73)mg/g.ConclusionThe HPLC identification method established and described in this study was shown to be suitable for the identification of piperine in the preparation.The HPLC method is simple,rapid and accurate,which is suitable for the determination of the content of punicalagin in the preparation.
作者
古丽巴哈尔·艾力
李蒙华
李玉玲
滕亮
Gulibahaer Aili;LI menghua;LI Yuling;TENG Liang(College of Pharmacy,Xinjiang Medical University,Urmuqi 830011,China;Department of Pharmacology,The First Affiliated Hospital of Xinjiang Medical University,Urmuqi 830054,China)
出处
《新疆医科大学学报》
CAS
2019年第12期1615-1618,共4页
Journal of Xinjiang Medical University
基金
新疆维吾尔自治区重点研发计划项目(2017B03013-2)
