加味结石颗粒HPLC指纹图谱研究及其主成分含量测定

HPLC Fingerprint of JiaWei JieShi Granules and Determination of Maincomponent

目的建立加味结石颗粒的HPLC指纹图谱,同时对其主要成分栀子苷进行含量测定,为其质量评价提供依据。方法采用YMC-Pack-ODS-A C_(18)(250 mm×4.6 mm,5μm)色谱柱,以0.1%磷酸水-乙腈为流动相,流速为0.8 mL·min^(-1),检测波长为238 nm,柱温为30℃,测定10批加味结石颗粒样品,采用《中药色谱指纹图谱相似度评价系统(2004A)》建立加味结石颗粒指纹图谱共有模式图,并计算相似度,再通过对照品色谱图对共有峰进行指认。结果加味结石颗粒HPLC指纹图谱共标定了13个共有峰,相似度均在0.95以上,指纹峰分别来自栀子(2、5、6号峰),川木通(8号峰),萹蓄(9号峰),连钱草(12号峰),甘草(13号峰),并通过对照品色谱图指认1号峰为绿原酸,6号峰为栀子苷,12号峰为木犀草素,13号峰为甘草酸,栀子苷的质量分数为1.04 mg·g^(-1)。结论该方法重复性好,简便可靠,可用于加味结石颗粒生产过程的稳定性和成品质量的可控性。

OBJECTIVE To establish an HPLC method for fingerprint analysis of JiaWei Jieshi Granules(JJG)for its quality control.METHODS The chromatographic behaviors were obtained by YMC-Pack-ODS-A C_(18)(250 mm×4.6 mm,5μm)with gradient elution using 0.1%phosphoric acid solution-acetonitrile as the mobile phase.The detection wavelength was 238 nm,the volume flow rate was 0.8 mL·min^(-1),and the column temperature was 30℃.The samples of 10 batches of JJG were determined,and the chromatographic fingerprint similarity evaluation system of Chinese medicine(2004A edition)was used to establish the common pattern of JJG fingerprints,and the similarity was calculated.Then the common peaks were identified by the reference chromatogram.RESULTS HPLC fingerprints of JJG were established by the determination of 10 batches of samples.The similarity was above 0.95.A total of 13 common peaks were calibrated.Three mutual peaks were from Gardeniae Fructus(peak 2,5,6),Clematidis Armandii Caulis(peak 8),Polygoni Avicularis Herba(peak 9),Glechomae Herba(peak 12),Glycyrrhizae Radix et Rhizoma(peak 13).The common peak was identified by reference chromatograms and peak 1 was chlorogenic acid,peak 6 was geniposide,peak 12 was luteolin,peak 13 was glycyrrhizic acid.The content of geniposide was 1.04 mg·g^(-1).CONCLUSION The method can be used for the quality control of JJG with good precision,accuracy,and reproducibility.