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目的:研究建立紫参片的HPLC法指纹图谱分析方法,并测定该制剂中藁苯内酯、正丁烯基苯酞、丹参酮Ⅰ、隐丹参酮、丹参酮ⅡA的含量,为其质量控制提供依据。方法:利用HPLC法,采用UltimateXB C18色谱柱(250 mm×4.6 mm,5μm),使用乙腈-0.3%磷酸水溶液为流动相进行梯度洗脱,以260 nm为检测波长。在紫参片样品的HPLC图中,以丹参酮ⅡA为对照参比物,对各色谱峰与丹参酮ⅡA色谱峰的相对保留时间和相对峰面积的RSD进行分析,运用中国药典委员会“中药色谱指纹图谱相似度评价系统2004A版”对10批紫参片的图谱进行相似度评价。采用外标法,利用藁苯内酯、隐丹参酮、丹参酮Ⅰ、丹参酮ⅡA的混合对照品测定其在10批该制剂中的含量。结果:在选定的条件下确定32个峰构成紫参片的指纹特征,各批次样品均具有上述特征,且特征峰的相对含量分布基本一致;各批次样品中丹参酮ⅡA色谱峰所对应的保留时间一致;每批样品的各色谱峰与丹参酮ⅡA色谱峰的相对保留时间和相对峰面积的RSD均符合指纹图谱的检测要求,10个批次样品的指纹图谱相似度均大于0.940,5个物质在10批该制剂中的含量基本一致。结论:HPLC指纹图谱方法与5个物质的含量测定方法准确、稳定、简便,均可用于紫参片的质量控制。
OBJECTIVE: To study the HPLC fingerprinting method for the determination of purple ginseng tablets, and to determine the content of terpene lactone, n-butenylphthalide, tanshinone Ⅰ, cryptotanshinone and tanshinone ⅡA in this preparation and provide the basis for its quality control. Methods: The HPLC method was applied on a Ultimate XB C18 column (250 mm × 4.6 mm, 5 μm) using a mobile phase of acetonitrile-0.3% phosphoric acid as mobile phase. The detection wavelength was 260 nm. In the HPLC chromatogram of purple ginseng sample, the relative retention time and relative peak area RSD of each chromatographic peak and tanshinone IIA chromatographic peak were analyzed with tanshinone IIA as a control reference substance. The Chinese Pharmacopoeia Commission Map similarity evaluation system 2004A version "10 batches of purple ginseng tablet similarity evaluation. Using external standard method, using tuberculin, cryptotanshinone, tanshinone Ⅰ, tanshinone Ⅱ A mixed reference substance was measured in 10 batches of the preparation of the content. Results: Fingerprints of 32 samples were identified under the selected conditions. The samples of each batch had the above characteristics and the distribution of the relative content of the characteristic peaks was basically the same. The tanshinone Ⅱ A peak corresponding to each batch of samples The retention time and relative peak area RSD of each peak of chromatographic peak and tanshinone ⅡA peak in each batch of samples were in accordance with the requirements of fingerprint detection. The similarity of fingerprints in 10 batches of samples was greater than 0.940,5 The contents of 10 batches of the preparation are basically the same. Conclusion: The method of HPLC fingerprint and the method of determination of five substances are accurate, stable and simple and can be used for the quality control of purple ginseng tablets.