平火茶标准汤剂的质量分析  

Quality analysis of Pinghuo tea standard decoction

作　　者：赵新梅 桑宏扬 杨春静[2] 雷敬卫[1] 龚海燕[1] 谢彩侠[1] 张春亚 段浩瀚 余浩 ZHAO Xinmei;SANG Hongyang;YANG Chunjing;LEI Jingwei;GONG Haiyan;XIE Caixia;ZHANG Chunya;DUAN Haohan;YU Hao(School of Pharmacy,Henan University of Chinese Medicine,Zhengzhou 450046,China;Dept.of Pharmacy,Third Affiliated Hospital of Henan University of Chinese Medicine,Zhengzhou 450046,China)

机构地区：[1]河南中医药大学药学院,郑州450046 [2]河南中医药大学第三附属医院药剂科,郑州450046

出　　处：《中国药房》2025年第1期71-78,共8页China Pharmacy

基　　金：河南省中医药科学研究专项课题(No.2022ZY1101)。

摘　　要：目的建立平火茶标准汤剂指纹图谱和多指标含量测定的方法,并探究饮片-标准汤剂化学成分的量值传递关系。方法制备15批平火茶标准汤剂,测定其出膏率;采用高效液相色谱(HPLC)法建立该制剂的指纹图谱,并进行相似度评价和共有峰确定,同时进行化学计量学分析;同法测定该制剂中指标性成分含量并计算含量的转移率。色谱柱为Venusil C18,流动相为乙腈-0.1%磷酸溶液(梯度洗脱),柱温为30℃,检测波长为238 nm(0~37 min、85~102 min)、330 nm(37~85 min),流速为1.0 mL/min,进样量为10μL。结果15批平火茶标准汤剂HPLC指纹图谱的相似度均不小于0.968;共标定出24个共有峰,指认出了其中9个,分别为新绿原酸(峰3)、绿原酸(峰6)、栀子苷(峰9)、甘草苷(峰10)、木犀草苷(峰11)、异绿原酸A(峰14)、木犀草素(峰21)、山柰酚(峰23)、甘草酸(峰24)。聚类分析、主成分分析与正交偏最小二乘判别分析结果一致,均可将15批样品分为3类。15批平火茶标准汤剂的指标性成分栀子苷、木犀草苷、异绿原酸A、甘草苷、甘草酸的线性范围分别为0.020580~0.411600、0.001617~0.080850、0.006076~0.607600、0.005125~0.071740、0.017288~0.432200 mg/mL;精密度、重复性、稳定性、加样回收率试验的RSD均不高于4%(n均为6);含量范围分别为3.2279~10.0022、0.2974~0.5546、3.3501~6.1596、0.7206~1.0733、2.0031~3.0301 mg/g,饮片-标准汤剂含量的转移率范围分别为19.7628%~35.8405%、12.1233%~21.2540%、46.0972%~82.8694%、58.7088%~91.6296%、39.1143%~63.7106%。15批平火茶标准汤剂出膏率的转移率范围为61.15%~84.68%。结论本研究所建立的HPLC指纹图谱和含量测定方法简单且准确度高,可为平火茶标准汤剂的量值传递研究、质量控制、临床应用及后续制剂的开发提供参考。OBJECTIVE To establish the fingerprint of Pinghuo tea standard decoction and a method for determination of multi-component to clarify the transfer relationship of quantities and quality from pieces and standard decoction.METHODS Fifteen batches of Pinghuo tea standard decoction were prepared and the extract rate was determined;the fingerprint of the preparation was established by using high-performance liquid chromatography(HPLC);the similarity evaluation and the determination of common peaks were performed,and chemometric analysis was performed;the same method was used to determine the content of indicator components and the transfer rate was calculated.The chromatographic column was Venusil C18 column with mobile phase consisted of acetonitrile-0.1%phosphoric acid solution(gradient elution);the column temperature was 30℃,and the detection wavelengths were 238 nm(0-37 min,85-102 min)and 330 nm(37-85 min)at a flow rate of 1.0 mL/min with an injection volume of 10μL.RESULTS The similarity of HPLC fingerprints for 15 batches of Pinghuo tea standard decoction was not lower than 0.968.A total of 24 common peaks were calibrated and 9 peaks were recognized,which were as follows neochlorogenic acid(peak 3),chlorogenic acid(peak 6),geniposide(peak 9),glycyrrhizin(peak 10),galuteolin(peak 11),isochlorogenic acid A(peak 14),luteolin(peak 21),kaempferol(peak 23)and glycyrrhizic acid(peak 24).Cluster analysis,principal component analysis and orthogonal partial least squares discriminant analysis showed consistent results,all of which could classify the 15 batches of samples into three categories.The linear range of indicator components in 15 batches of Pinghuo tea standard decoction,such as geniposide,luteolin,isochlorogenic acid A,glycyrrhizin,and glycyrrhizic acid,were 0.020580-0.411600,0.001617-0.080850,0.006076-0.607600,0.005125-0.071740,and 0.017288-0.432200 mg/mL,respectively;RSDs of precision,repeatability,stability and recovery rate tests were all not higher than 4%(n=6).The mass fractions ranged 3.2279-10.0022,0.

关 键 词：平火茶标准汤剂 含量测定 指纹图谱 量值传递 质量控制 高效液相色谱法 

分 类 号：R284.1[医药卫生—中药学] R917[医药卫生—中医学]