经典名方开心散基准样品HPLC特征图谱研究

HPLC Specific Chromatograms of Benchmark Substances of the Famous Classical Formula Kaixin Powder

目的:建立经典名方开心散基准样品高效液相色谱特征图谱,全面表征开心散处方中4个药味的成分特征,为开心散制剂质量控制提供可靠方法。方法:采用Waters Xbridge Shield RP18色谱柱(150 mm×4.6 mm,3.5μm),第1套方法以乙腈为流动相A,含0.1%磷酸水溶液为流动相B,梯度洗脱,柱温为35℃,进样量为10μL,检测波长为242 nm;第2套方法以乙腈为流动相A,水为流动相B,梯度洗脱,柱温为30℃,进样量为20μL,检测波长为203 nm。使用不同批次饮片制备17批开心散基准样品,将色谱图经“中药色谱指纹图谱相似度评价系统”(2004A版)进行峰匹配,明确共有峰个数,生成对照特征图谱,归属和指认共有峰。结果:建立了2套特征图谱分析方法,其中第1套确定特征峰13个,归属远志药味特征峰9个、石菖蒲药味2个、茯苓药味2个,指认5个成分为远志酮Ⅲ、3,6?-二芥子酰基蔗糖、β-细辛醚、α-细辛醚和猪苓酸C;第2套确定特征峰12个,归属人参药味特征峰7个、远志药味2个、共有峰3个,指认6个成分为人参皂苷Rg1、人参皂苷Re、人参皂苷Rf、人参皂苷Rb1、人参皂苷Rb2和人参皂苷Rd。结论:建立的2套特征图谱分析方法简单可行,具有较好的针对性,为经典名方开心散基准样品及制剂质量控制提供了参考。

Objective:To establish HPLC specific chromatograms of benchmark substances of the famous classical formula Kaixin Powder,comprehensively characterize the components in the four medicinal herbs constituting Kaixin Powder,and provide a reliable method for the quality control of Kaixin Powder.Methods:The Waters Xbridge Shield RP18 column(150 mm×4.6 mm,3.5μm)was used.The elution of scheme 1 was performed with acetonitrile as mobile phase A and the aqueous solution containing 0.1%phosphoric acid as mobile phase B at the column temperature of 35℃,the injection volume of 10μL,and the detection wavelength of 242 nm.The elution of scheme 2 was performed with acetonitrile as mobile phase A and aqueous solution as mobile phase B at the column temperature of 30℃,the injection volume of 20μL,and the detection wavelength of 203 nm.A total of 17 batches of benchmark substances of Kaixin Powder were prepared with the decoction pieces of different batches.The chromatograms were matched by the Traditional Chinese Medicine Chromatographic Fingerprint Similarity Evaluation System(2004 A version)to determine the number of common peaks,generate specific chromatograms,and attribute and identify the common peaks.Results:Two sets of specific chromatograms were obtained.The first set determined 13 characteristic peaks,including 9 peaks indicating the components in Polygalae Radix,2 peaks indicating the components in Acori Tatarinowii Rhizoma,and 2 peaks indicating the components in Poria.In addition,this set of specific chromatograms identified 5 components,which were polygalaxanthoneⅢ,3,6′-disinapoyl sucrose,β-asarone,α-asarone,and polyporenic acid C.The second set of specific chromatograms determined 12 characteristic peaks,including 7 peaks indicating the components in Ginseng Radix et Rhizoma,2 peaks indicating the components in Polygalae Radix,and 3 common peaks.This set of specific chromatograms identified 6 components,which were ginsenosides Rg1,Re,Rf,Rb1,Rb2,and Rd.Conclusion:The established two HPLC methods are simple,feasible,and well targeted,which lay a foundation for the quality control of benchmark substances and preparations of the famous classical formula Kaixin Powder.