HPLC指纹图谱法评价知柏地黄丸(浓缩丸)的质量

Quality Evaluation of Zhibai Dihuang Pills(Concentrated Pills)by HPLC Fingerprint

目的:建立知柏地黄丸(浓缩丸)的高效液相色谱(HPLC)指纹图谱,并评价其质量。方法:色谱柱为Dikma Diamonsil C18,流动相为0.1%醋酸溶液-甲醇(梯度洗脱),流速为1.0 m L/min,检测波长为260 nm,柱温为30℃,进样量为10μL。以丹皮酚为参照,分别绘制A、B、C厂有效期内样品和A厂有效期内与有效期外样品的HPLC图谱。采用《中药色谱指纹图谱相似度评价系统》(2004 A)对A、B、C厂有效期内样品及A厂有效期内与有效期外样品进行相似度评价,分别确定共有峰。结果:A、B、C厂各10批有效期内样品的HPLC图谱分别有24、29、32个共有峰,A、B、C厂样品HPLC图谱与对照指纹图谱的相似度均大于0.94,具有较好的一致性。A厂有效期内样品的HPLC图谱与有效期外样品的HPLC图谱具有较好的一致性。结论:本研究建立的HPLC指纹图谱可为评价知柏地黄丸(浓缩丸)的质量提供参考,但其并不能有效鉴别有效期外的样品。

OBJECTIVE:To establish the HPLC fingerprint of Zhibai dihuang pills(concentrated pills),and to evaluate its quality.METHODS:The determination was performed on Dikma Diamonsil C18 column with mobile phase consisted of 0.1%acetic acid solution-methanol(gradient elution)at the flow rate of 1.0 mL/min.The detection wavelength was set at 260 nm,and column temperature was 30℃.The sample size was 10μL.Using paeonol as reference,HPLC chromatograms of samples from A,B,C manufacturers within validity period and samples from manufacturer A within validity period and out of validity period were drawn.The similarity of HPLC chromatogram for samples from A,B and C manufacturers and samples from A manufacturer within validity period and out of validity period was evaluated by TCM Chromatogram Fingerprint Similarity Evaluation System(2004 A).Common peaks of HPLC chromatogram for 3 manufacturers sample within validity period were confirmed.RESULTS:There were 24,29 and 32 common peaks in HPLC chromatograms for each 10 batches of samples from manufacturer A,B and C within validity period,respectively.The similarity of corresponding HPLC chromatograms of samples from manufacturer A,B and C compared with control HPLC chromatography were all higher than 0.94 with good agreement.HPLC chromatograms of sample from A manufacturer within validity period had good agreement with that from A manufacturer out of validity period.CONCLUSIONS:Established HPLC fingerprint analysis method can represent the quality of Zhibai dihuang pills(concentrated pills),but cannot effectively identify the expired samples.