目的: 基于清热解毒口服液HPLC指纹图谱,建立质量评价方式,考察各厂家样品质量情况。方法:采用Diomonsil Plus C18色谱柱(250 mm×4.6 mm, 5 μm),以甲醇-0.4%甲酸水溶液为流动相,梯度洗脱,流速为1 mL·min-1,柱温为35 ℃,检测波长为238、280(29 min,238→280 nm),建立指纹图谱,结合化学计量学及统计学技术,进行初步质量评价。结果:清热解毒口服液指纹图谱共标定30个共有峰,全部进行归属,其中确证成分26个(根据对照品比对确证22个,根据QTOF/MS和文献确证4个),结合化学计量学中聚类分析和主成分分析,可将不同厂家样品予以区分,质量较好的厂家样品栀子苷、龙胆苦苷以及金银花的酚酸类成分含量明显更高,而质量差的厂家样品只有黄芩苷含量与其他厂家无明显差异。结论:该方法能宏观评价各厂家样品的优劣,将指纹图谱和化学计量学以及统计学技术联用是较为适宜、全面的质量评价手段。
Objective: To establish a quality evaluation method to investigate the quality of samples from different manufacturers based on the HPLC fingerprints of Qingrejiedu oral liquid. Methods: The analysis was performed on a Diomonsil Plus C18 column(250 mm×4.6 mm, 5 μm)) with methanol -0.4% formic acid aqueous solution as mobile phases in gradient elution,1 mL·min-1 as flow rate and 35 ℃ as column temperature. The detection wavelength were 238 nm(0-29 min) and 280 nm(29-90 min). The HPLC fingerprints were established to evaluate the quality of samples from different manufacturers combined with chemometrics and statistics. Results: Thirty chromatographic peaks were recognized as common peaks in the Qingrejiedu oral liquid fingerprints, all of which were attributed, and 26 components were confirmed. Among them 23 components were confirmed by comparison with reference substances and 4 components were identified by QTOF/MS and literature. Combining with cluster analysis and principal component analysis, the samples from different manufacturers could be distinguished. The contents of geniposide, gentiopicroside and phenolic acids, in the samples from manufacturers with better quality were significantly higher than those of the samples from manufacturers with poor quality. Only the content of baicalin had no obvious difference between them. Conclusion: This method can be used to macroscopically evaluate the quality of the samples from different manufacturers. The combination of fingerprint and stoichiometry or statistics technology is a suitable and comprehensive quality evaluation method.
[1] 中华人民共和国药典 2020 年版.一部[S]. 2020:1683
ChP 2020. Vol Ⅰ[S].2020:1683
[2] 中华人民共和国药典 2015年版.一部[S]. 2015:1552
ChP 2015. Vol Ⅰ[S].2015:1552
[3] 朱雪亚,李泽运,张潇,等.清热解毒口服液中6个药物成分的定量分析与网络药理学研究[J].药物分析杂志,2022, 42(9):1537
ZHU XY, LI ZY, ZHANG X, et al. Quantitative analysis and network pharmacology research based on 6 components in Qingre Jiedu oral liquid [J]. Chin J Pharm Anal, 2022, 42(9):1537
[4] 尤立华,杨秉呼,叶萌,等.清热解毒口服液HPLC指纹图谱[J].中国实验方剂学杂志, 2014, 20(14):84
YOU LH, YANG BH, YE M, et al. Fingerprint chromatograms of Qingre Jiedu Koufuye by HPLC [J]. Chin J Exp Tradit Med Form, 2014, 20(14):84
[5] 陈叶青,蒋丽萍,朱山寅,等.HPLC测定清热解毒口服液中4个成分的含量[J].华西药学杂志,2016,31(6):644
CHEN YQ,JIANG LP,ZHU SY,et al. Determination of four components in Qingre Jiedu oral liquid by HPLC[J]. West China J Pharm Sci, 2016, 31(6):644
[6] 朱伟堃,井改革,赵蕊蕊,等. 基于HPLC和多元统计分析的清热解毒口服液质量评价模式研究[J]. 食品与药品, 2021,23(6):493
ZHU WK, JING GG, ZHAO RR,et al. Study on quality evaluation model of Qingre Jiedu Oral Liquid based on HPLC and multivariate statistical analysis[J]. Food Drug, 2021, 23(6):493
[7] 张振巍, 张娜娜,白丹丹,等.一测多评法测定清热解毒口服液中4种成分的含量[J]. 中国药房, 2013, 24(28):2676
ZHANG ZW, ZHANG NN, BAI DD, et al. Content determination of 4 components in Qingre Jiedu Oral Liquid by QAMS[J]. China Pharm, 2013, 24(28):2676
[8] 朱伟堃,周欣,王劲, 等. 不同厂家清热解毒口服液的质量分析与评价[J]. 中南药学, 2021,19(9):1887
ZHU WK, ZHOU X, WANG J, et al. Quality evaluation of Qingre Jiedu oral liquid from different manufactures[J]. Cent South Pharm, 2021, 19(9):1887
[9] 朱姮,于金倩,刘倩,等. 基于RRLC-DAD-ESI-Q-TOF-MS技术的山东金银花多指标定量指纹图谱分析[J]. 中国实验方剂学杂志, 2017,23(19):82
ZHU H, YU JQ, LIU Q, et al. Multiple indicator quantitative fingerprint of Lonicerae Japonicae Flos from Shandong province based on RRLC-DAD-ESI-Q-TOF-MS[J]. Chin J Exp Tradit Med Form, 2017, 23(19):829
[10] 柴冲冲,曹妍,毛民,等.基于HPLC特征图谱、UPLC-Q-TOF/MS定性及多成分定量的黄芩酒炙前后化学成分变化研究[J].中草药,2020,51(9):2436
CHAI CC, CAO Y, MAO M, et al. Comparison of chemical compositions before and after wine-frying of Scutellaria baicalensis based on HPLC characteristic chromatogram, UPLC-Q-TOF/MS qualitative and multi-component quantitative analysis[J]. Chin Tradit Herb Drugs, 2020, 51(9):2436
[11] HE LL, ZHANG ZF, LU LY, et al. Rapid identification and quantitative analysis of the chemical constituentsin Scutellaria indica L. by UHPLC-QTOF-MS and UHPLC-MS/MS [J]. J Pharm Biomed Anal, 2016, 17(1):1259
[12] 汤丹,曹东敏,黄广枭,等. HPLC-DAD-Q-Exactive静电场轨道阱高分辨质谱快速分析栀子中主要成分[J]. 广东化工, 2019, 46(13):156
TANG D, CAO D, HUANG GX, et al. Rapid analysis of main compounds in Gardenia jasminoides by HPLC-DAD-Q-exactive-orbitrap mass spectrometry[J]. Guangdong Chem Ind, 2019, 46(13):15
[13] 徐姣,赵嵘,代云桃,等.栀子标准汤剂的质量评价方法考察[J].中国实验方剂学杂志, 2017, 23(7):30
XU J, ZHAO R, DAI YT, et al. Quality evaluation of standard decoction of Gardeniae Fructus[J]. Chin J Exp Tradit Med Form, 2017, 23(7):30
[14] 徐境荣,于钦川,赖莉,等.基于多指标成分含量测定探索黄芩药材质量综合评价模式[J]. 药学学报, 2021, 56(11):3141
XU JR, YU QC, LAI L, et al. Comprehensive quality evaluation of Scutellaria baicalensis Georgi by determination of multi-component content[J]. Acta Pharm Sin, 2021, 56(11):3141
[15] 洪挺,张昆艳,许妍,等. 清热解毒颗粒的HPLC指纹图谱建立及聚类分析[J].中国现代应用药学, 2019, 36(24):3056
HONG T, ZHANG KY, XU Y, et al. Establishment of HPLC fingerprint of Qingre Jiedu granules and cluster analysis[J]. Chin J Mod Appl Pharm, 2019, 36(24):3056
[16] 解静,高杉,李琳,等. 网络药理学在中药领域中的研究进展与应用策略[J].中草药, 2019, 50(10):2257
XIE J, GAO S, LI L, et al. Research progress and application strategy on network pharmacology in Chinese materia medica[J]. Chin Tradit Herb Drugs, 2019, 50(10):2257
