蒙药闹羊花配方颗粒指纹图谱及含量测定研究

Fingerprint and content determination of Mongolian medicine Rhododendri Mollis Flos formula granules

目的建立15批蒙药闹羊花配方颗粒的指纹图谱及其中金丝桃苷等5种黄酮类成分的含量测定方法,以评价闹羊花配方颗粒的质量。方法采用HPLC法,以COSMOSIL C18为色谱柱,以乙腈(A)-0.2%磷酸水(B)为流动相,梯度洗脱,检测波长为255 nm,柱温为40℃,流速为1.0 mL·min-1;采用《中药色谱指纹图谱相似度评价系统(2012版)》建立15批闹羊花配方颗粒的指纹图谱并评价相似度;使用软件SPSS 27.0、SIMCA14.1进行化学模式识别,分析并筛选影响闹羊花配方颗粒质量的标志物;测定闹羊花配方颗粒中金丝桃苷、槲皮苷、阿福豆苷、槲皮素、山柰酚5种成分的含量。结果15批闹羊花配方颗粒指纹图谱中有15个共有峰被标定,有5种成分[金丝桃苷(峰7)、槲皮苷(峰9)、阿福豆苷(峰11)、槲皮素(峰13)、山柰酚(峰15)]被指认,相似度均>0.940;化学模式识别结果显示,S1~S7、S15号样品为一类,S8~S14号样品为一类,峰1、2、6、9~15的VIP值>1;15批闹羊花配方颗粒中金丝桃苷、槲皮苷、阿福豆苷、槲皮素、山柰酚的含量分别为0.007%~0.013%、0.067%~0.121%、0.007%~0.010%、0.040%~0.085%、0.001%~0.002%。结论该研究建立的指纹图谱及含量测定方法可行、稳定、简便,可用于评价闹羊花配方颗粒的质量。

Objective To establish the fingerprint of 15 batches of Mongolian medicine Rhododendri Mollis Flos formula granules and determine the content of 5 flavonoids to evaluate their quality.Methods High performance liquid chromatography(HPLC)was performed on COSMOSIL C18 column with acetonitrile(A)-0.2%phosphoric acid water(B)as the mobile phase by gradient elution.The detection wavelength was 255 nm,the column temperature was 40℃,and the flow rate was 1.0 mL·min-1.The fingerprint of 15 batches of Rhododendri Mollis Flos formula granules was established and the similarity was evaluated by Similarity Evaluation System of TCM Chromatographic Fingerprint(2012 Edition).SPSS 27.0 and SIMCA14.1 software were used to conduct chemical pattern recognition and screen the markers affecting the quality of Rhododendri Mollis Flos formula granules.The content of 5 components(hypericin,quercitrin,afzelin,quercetin and kaempferol)in Rhododendri Mollis Flos formula granules was determined.Results In the fingerprint of 15 batches of Rhododendri Mollis Flos formula granules,15 common peaks were identified,and the 5 components[hypericin(peak 7),quercitrin(peak 9),afzelin(peak 11),quercetin(peak 13),and kaempferol(peak 15)]were respectively identified,with similarity being all greater than 0.940.The chemical pattern recognition showed that samples S1~S7 and S15 belonged to one category,and samples S8~S14 belonged to the other category.The VIP values of peaks 1,2,6,and 9~15 were greater than 1.The content of hypericin,quercitrin,afzelin,quercetin and kaempferol in 15 batches of Rhododendri Mollis Flos formula granules ranged 0.007%~0.013%,0.067%~0.121%,0.007%~0.010%,0.040%~0.085%,and 0.001%~0.002%,respectively.Conclusion The fingerprint and content determination method are feasible,stable and simple,which can be used to control the quality of Rhododendri Mollis Flos formula granules.