新疆哈药金雀花药材质量控制方法研究

摘要

目的 通过TLC鉴别、多组分含量测定及HPLC指纹图谱技术建立新疆哈药金雀花药材的质量控制方法.方法 ①TLC鉴别:采用硅胶G板(10 cm×20 cm),以乙醚-正丁醇-冰乙酸-水(10:5:1:1)为展开剂展开,喷以质量浓度为10 g·L -1的三氯化铝乙醇溶液显色,105 ℃下加热20 min,在366 nm紫外光灯下检视.②含量测定与 HPLC指纹图谱的建立:采用Inertsil ODS-3色谱柱(250 mm×4.6 mm,5 μm),流动相为2 mL·L -1磷酸(A)-乙腈(B),线性梯度洗脱,流速:1.0 mL·min-1,检测波长:254 nm.结果 在样品TLC图中能观察到芦丁和山柰酚-3-O-芸香糖苷的相应斑点.含量测定结果表明,10批金雀花药材主要黄酮苷的平均含量为:芦丁3.59 mg·g -1,山柰酚-3-O-芸香糖苷1.02 mg·g -1.10批金雀花药材的 HPLC指纹图谱中有23个共有峰(19号峰为芦丁,22号峰为山柰酚-3-O-芸香糖苷)相似度均大于0.91.结论 建立的质量控制方法操作简单,重复性及稳定性良好,可反映新疆哈药金雀花药材的质量.%Objective To establish the quality control method of Xinjiang Kazakh medicine Parochetus communis by thin layer chro-matography(TLC),multiple component content determination and HPLC fingerprint.Methods ①The TLC identification was car-ried out on TLC pre-coated plates(silica gel G,10 cm×20 cm)using the mixture of ether-butyl alcohol-acetic acid-water at the proportion of 10:5:1:1 as the mobile phase.10 g·L -1AlCl3-ethanol solution was used for visualization,and TLC plate was heated under 105 ℃ until the spots became clear and detected under 366 nm ultraviolet lamp.②The content determination and es-tablishment of HPLC fingerprint was performed on an Inertsil ODS-3 chromatographic column(250 mm×4.6 mm,5 μm)with the mobile phase consisted of 2 mL · L -1phosphoric acid(A)and acetonitrile(B)with gradient elution at a flow rate of 1.0 mL·min-1and the detection wavelength was set at 254 nm.Results The spots of rutin and kaempferol-3-O-rutinoside were detec-ted in the TLC of sample solution and the content determination results showed that the average contents of rutin and kaempferol-3-O-rutinoside in 10 batches of Parochetus communis were 3.59 and 1.02 mg·g -1,respectively.23 of commom peaks(of which peak 19 was rutin and peak 22 was kaempferol-3-O-rutinoside)were detected in the HPLC fingerprint of sample solution and the similarity of the 10 batches of Parochetus communis was greater than 0.91.Conclusion The quality control method established in this study was simple,reproducible and stable and can reflect the quality of Xinjiang Kazakh medicine Parochetus communis.