一测多评结合指纹图谱的肝复乐胶囊质量控制研究

Study on Quality Control of Ganfule Capsules by QAMS and Fingerprint

目的建立一测多评(QAMS)法同时测定肝复乐胶囊中白术内酯Ⅰ、毛蕊异黄酮葡萄糖苷、野黄芩苷、芸香柚皮苷、橙皮苷、黄芩苷、芦荟大黄素7种药效特征成分含量的方法。方法采用YMC-Pack ODS-A色谱柱,以乙腈-0.1%甲酸水溶液为流动相,分段转换波长为285 nm(0~30 min、35~50 min)、260 nm(30~35 min、50~80 min),柱温25℃,流速0.8 mL/min,建立肝复乐胶囊HPLC指纹图谱,并以橙皮苷为内标,建立白术内酯Ⅰ、毛蕊异黄酮葡萄糖苷、野黄芩苷、芸香柚皮苷、橙皮苷、黄芩苷、芦荟大黄素的相对校正因子,计算7种成分的含量,并与外标法测定结果进行比较,以验证QAMS方法的准确性、重复性及可行性。结果10批指纹图谱共确定29个共有峰,指认白术内酯Ⅰ、毛蕊异黄酮葡萄糖苷、野黄芩苷、芸香柚皮苷、橙皮苷、黄芩苷、芦荟大黄素7种主要特征成分。10批样品图谱的相似度均大于0.95,峰形、分离度均较为良好,精密度及重复性RSD均小于1.5%,在24 h内供试品溶液稳定,测定成分线性关系良好,线性范围适当。QAMS法计算值与外标法实测值差异无统计学意义。结论本研究建立的QAMS方法可作为简便快捷的质量评价模式用于肝复乐胶囊中7种成分的质量控制。

Objective To establish a quantitative analysis of multi-components by single-marker(QAMS)method for the simultaneous determination of 7 medicinal properties of atractylenolideⅠ,verbascum isoflavone glycoside,wild baicalin,rutin naringin,hesperidin,baicalin,and aloe-emodin.Methods YMC-Pack ODS-A column was used with acetonitrile-0.1%formic acid as mobile phase,and the conversion wavelength was 285 nm(0–30 min,35–50 min)and 260 nm(30–35 min,50–80 min),respectively;column temperature was 25℃;flow rate was 0.8 mL/min.HPLC fingerprint of Ganfule Capsules was established,and hesperidin was set as the internal reference substance to establish the relative correction factors of atractylenolideⅠ,verbascum isoflavone glycoside,wild baicalin,rutin naringin,hesperidin,baicalin,and aloe-emodin.The contents of the above seven components were calculated and were compared with the results of the external standard method to verify the accuracy,repeatability and feasibility of the QAMS method.Results A total of 29 common peaks were identified in 10 batches of fingerprints.7 main characteristic components of atractylenolideⅠ,verbascum isoflavone glycoside,wild baicalin,rutin naringin,hesperidin,baicalin,and aloe-emodin were identified.The similarity of the 10 batch samples was more than 0.95.Under these conditions,the peak shape and resolution of the spectrum were relatively good;precision and repeatability RSD values were less than 1.5%;the sample solution was stable within 24 h;the measured component had a good linear relationship.There was no statistical significance between the calculated value of QAMS method and the measured value of the external standard method.Conclusion The QAMS method established in this study can be used as a simple and quick quality evaluation model,which can be used for the quality control of seven components in Ganfule Capsules.