质量分析

基于UHPLC多成分测定与主成分分析的金藤清痹颗粒质量评价*

展开
  • 1.鲁南制药集团股份有限公司 经方与现代中药融合创新全国重点实验室,临沂 276006;
    2.鲁南厚普制药有限公司 中药制药共性技术山东省工程研究中心,临沂 276006
第一作者 Tel:13754746480;E-mail:lilydeng791217@sina.com
**Tel:(0539)8336639;E-mail: lunanfanjianwei@163.com

收稿日期: 2023-09-14

  网络出版日期: 2024-06-21

基金资助

*山东省重点研发计划(重大科技创新工程)项目(2021CXGC010508);山东省新旧动能转换重大产业攻关项目(鲁动能办〔2021〕23号)

Quality evaluation of Jinteng Qingbi granules based on UHPLC multi-index component determination and principal component analysis*

Expand
  • 1. State Key Laboratory of Integration and Innovation of Classic Formula and Modern Chinese Medicine, Lunan Pharmaceutical Group Co.,Ltd., Linyi 276006, China;
    2. Shandong Engineering Research Center of Generic Manufacture Technology of Traditional Chinese Medicine, Lunan Hope Pharmaceutical Co.,Ltd., Linyi 276006, China

Received date: 2023-09-14

  Online published: 2024-06-21

摘要

目的: 建立同时测定金藤清痹颗粒中青藤碱、新绿原酸、木兰花碱、隐绿原酸、绿原酸、异绿原酸B、异绿原酸A、异绿原酸C、哈巴俄苷、藁本内酯和甘草酸铵11个成分含量的UHPLC法,并结合主成分分析对制剂进行质量评价。方法: 采用UHPLC波长切换法,色谱柱为Waters XSelect® CSH C18柱(150 mm×4.6 mm,2.5 μm),以甲醇-乙腈(1∶1)为流动相A,0.2%磷酸水溶液为流动相B,梯度洗脱,流速1.0 mL·min-1,柱温25 ℃,检测波长218 nm(0~17 min时,检测青藤碱)、326 nm (17~25 min和34~98 min时,检测新绿原酸、隐绿原酸、绿原酸和异绿原酸A、异绿原酸B、异绿原酸C)、263 nm(25~34 min和98~125 min时,检测木兰花碱、哈巴俄苷、藁本内酯、甘草酸铵)。利用SPSS27.0软件对20批金藤清痹颗粒中成分含量进行多元统计分析。结果: 青藤碱、新绿原酸、木兰花碱、隐绿原酸、绿原酸、异绿原酸B、异绿原酸A、异绿原酸C、哈巴俄苷、藁本内酯和甘草酸铵11个成分的质量浓度分别在14.36~143.61 μg·mL-1(r=0.999 9)、7.71~77.15 μg·mL-1 (r=0.999 8)、9.18~91.83 μg·mL-1(r=0.999 7)、10.71~107.07 μg·mL-1(r=0.999 8)、12.88~128.80 μg·mL-1(r=0.999 8)、5.20~51.95 μg·mL-1(r=0.999 7)、5.18~51.84 μg·mL-1(r=0.999 8)、5.40~53.95 μg·mL-1(r=0.999 8)、2.62~26.16 μg·mL-1(r=0.999 9)、6.31~63.06 μg·mL-1(r=0.999 9)和11.13~111.26 μg·mL-1(r=0.997 6)范围内与峰面积的线性关系良好;平均加样回收率(n=6)分别为98.3%、98.3%、98.5%、98.9%、99.2%、101.0%、98.1%、97.1%、96.8%、98.0%和98.7%,RSD均小于3.0%。20批金藤清痹颗粒样品中,上述青藤碱等11个成分的含量测定结果(n=6)依次为2.206~2.704、1.071~1.403、2.096~2.487、1.321~1.724、2.241~2.612、0.605~0.749、0.363~0.412、0.835~1.020、0.151~0.191、0.791~1.188和1.008~1.363 mg·g-1。主成分分析结果显示,连续生产的金藤清痹颗粒批次间质量差异较小,且以样品S1、S5和S7的综合质量相对更好。结论: 建立的UHPLC多指标成分含量测定方法简便、准确、稳定,结合主成分分析,可全面地评价金藤清痹颗粒的产品质量。

本文引用格式

邓丽华, 许克宁, 袁晓梅, 丁兵, 王丽苹, 徐丽, 杨本官, 刘源慧, 范建伟 . 基于UHPLC多成分测定与主成分分析的金藤清痹颗粒质量评价*[J]. 药物分析杂志, 2024 , 44(3) : 522 -531 . DOI: 10.16155/j.0254-1793.2024.03.18

Abstract

Objective: To establish a UHPLC method for simultaneously determining sinomenine, neochlorogenic acid, magnolflorine, cryptochlorogenic acid, chlorogenic acid, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, harpagoside, ligustilide and ammonium glycyrrhizate in Jinteng Qingbi granules, and evaluate the quality of Jinteng Qingbi granules combined with principal component analysis. Methods: UHPLC wavelength switching method was employed in the study. The chromatographic separation was performed on a Waters XSelect® CSH C18 column (150 mm×4.6 mm, 2.5 μm) using methanol-acetonitrile (1∶1) as mobile phase A and 0.2% phosphoric acid aqueous solution as mobile phase B in a gradient mode at 25 ℃. The flow rate was 1.0 mL·min-1, and the UV detection wavelength was chosen at 218 nm for sinomenine during 0-17 min, 326 nm for neochlorogenic acid, cryptochlorogenic acid, chlorogenic acid, isochlorogenic acid B, isochlorogenic acid A and isochlorogenic acid C during 17-25 min and 34-98nm, 263 nm for magnolflorine, harpagoside, ligustilide and ammonium glycyrrhizate during 25-34 min and 98-125nm, respectively. Furthermore, multiple statistical analysis was conducted on the contents of 11 components in 20 batches of Jinteng Qingbi granules using SPSS27.0 software. Resluts: Satisfactory linearities of sinomenine, neochlorogenic acid, magnolflorine, cryptochlorogenic acid, chlorogenic acid, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, harpagoside, ligustilide and ammonium glycyrrhizate were in the ranges of 14.36-143.61 μg·mL-1 (r=0.999 9), 7.71-77.15 μg·mL-1 (r=0.999 8), 9.18-91.83 μg·mL-1 (r=0.999 7), 10.71-107.07 μg·mL-1 (r=0.999 8), 12.88-128.80 μg·mL-1 (r=0.999 8), 5.20-51.95 μg·mL-1 (r=0.999 7), 5.18-51.84 μg·mL-1 (r=0.999 8), 5.40-53.95 μg·mL-1 (r=0.999 8), 2.62-26.16 μg·mL-1 (r=0.999 9), 6.31-63.06 μg·mL-1 (r=0.999 9) and 11.13-111.26 μg·mL-1 (r=0.997 6), respectively. The average recoveries (n=6) were 98.3%, 98.3%, 98.5%, 98.9%, 99.2%, 101.0%, 98.1%, 97.1%, 96.8%, 98.0% and 98.7%, respectively, with RSDs less than 3.0%. The contents ranges of sinomenine and other 10 components of 20 batches of Jinteng Qingbi granules samples were 2.206-2.704, 1.071-1.403, 2.096-2.487, 1.321-1.724, 2.241-2.612, 0.605-0.749, 0.363-0.412, 0.835-1.020, 0.151-0.191, 0.791-1.188 and 1.008-1.363 mg·g-1, respectively. The results of principal component analysis showed that the quality differences between batches of continuously produced Jinteng Qingbi granules were relatively smaller, and the comprehensive quality of samples S1, S5 and S7 was relatively better. Conclusion: The established UHPLC method of multi-index component determination is simple, accurate and stable. Combined with principal component analysis, it can be used for quality evaluation of Jinteng Qingbi granules comprehensively.

参考文献

[1] 魏志萍,洪芬芳,杨树龙. 中药治疗类风湿关节炎的研究进展[J]. 中华中医药杂志,2017,32(12):5477
WEI ZP, HONG FF, YANG SL. Research progress on traditional Chinese medicine on the treatment of rheumatoid arthritis [J]. Chin J Tradit Chin Med Pharm, 2017, 32 (12): 5477
[2] 周政,赵灵灵,贾文瑞,等. 基于肠道菌群探讨金藤清痹颗粒抗类风湿关节炎的作用机制[J]. 现代药物与临床,2023,38(2):270
ZHOU Z, ZHAO LL, JIA WR, et al. Mechanism of Jinteng Qingbi granules against rheumatoid arthritis based on gut microbiota [J]. Mod Drugs Clin, 2023, 38 (2): 270
[3] 袁博,曹炜,张解玉,等. 基于“虚、痰瘀、毒”论治类风湿关节炎[J]. 中国中医药信息杂志,2022,29(5):140
YUAN B, CAO W, ZHANG XY, et al. Treatment of rheumatoid arthritis from “deficiency, phlegm, stasis and toxicity” [J]. Chin J Inf Tradit Chin Med, 2022, 29 (5): 140
[4] 唐今扬,周彩云,王鑫,等. 金藤清痹颗粒治疗类风湿性关节炎模型大鼠的作用机制研究[J]. 北京中医药,2022,41(7):728
TANG JY, ZHOU CY, WANG X, et al. Study on the mechanism of Jinteng Qingbi granules in treating rheumatoid arthritis in model rats [J]. Beijing J Tradit Chin Med, 2022, 41 (7): 728
[5] 唐今扬,周彩云,王鑫,等. 金藤清痹颗粒通过调节免疫微环境对类风湿性关节炎大鼠的干预作用[J]. 中成药,2022,44(11):3459
TANG JY, ZHOU CY, WANG X, et al. Effects of Jinteng Qingbi granules on rheumatoid arthritis rats through intervention of immune microenvironment [J]. Chin Tradit Pat Med, 2022, 44 (11): 3459
[6] YBZ00332008 金藤清痹颗粒. 国家食品药品监督管理总局国家药品标准[ S ]. 2008
YBZ00332008 Jinteng Qingbi Keli. National Drug Standard of China Food and Drug Administration [S]. 2008
[7] 郝乘仪,于蕾,昌盛,等. HPLC-DAD法同时测定小儿退热合剂中多指标成分含量[J]. 药物分析杂志,2019,39(5):930
HAO CY, YU L, CHANG S, et al. Simultaneous determination the contents of index components in Xiaoer Tuire mixture by HPLC-DAD [J]. Chin J Pharm Anal, 2019, 39 (5): 930
[8] 庄会芳,袁晓梅,庄建林,等. UPLC波长切换法同时测定心通颗粒中7个成分的含量[J]. 药物分析杂志,2023,43(8):1284
ZHUANG HF, YUAN XM, ZHUANG JL, et al. Simultaneous determination of seven components in Xintong granules by UPLC wavelength switching method [J]. Chin J Pharm Anal, 2023, 43 (8): 1284
[9] 刘雯,郭海姣,覃洁萍,等. 基于多组分含量测定及主成分分析的狗仔花质量控制[J]. 中国医院药学杂志,2021,41(2):135
LIU W, GUO HJ, QIN JP, et al. Quality control of Vernonia patula Merr based upon multi-component determination and principal component analysis [J]. Chin J Hosp Pharm, 2021, 41 (2): 135
[10] 邵镪钎,李丹,蒋攀,等. 基于主成分及聚类分析的川明参的综合评价[J]. 中草药,2018,49(14):3389
SHAO QQ, LI D, JIANG P, et al. Comprehensive evaluation of yield and quality of Chuanmingshen violaceum based on principal component and cluster analysis [J]. Chin Tradit Herb Drugs, 2018, 49 (14): 3389
[11] 胡杨,李先芝,钱全全,等. HPLC法同时测定金银花配方颗粒中6种成分[J]. 中成药,2021,43(7):1717
HU Y, LI XZ, QIAN QQ, et al. Simultaneous determination of six constituents in Jinyinhua Formula granules by HPLC[J]. Chin Tradit Pat Med, 2021, 43 (7): 1717
[12] 邱连建,索彩仙,潘礼业,等. 基于多元统计分析的金银花、山银花及川银花质量评价研究[J]. 广东药科大学学报,2020,36(5):620
QIU LJ, SUO CX, PAN LY, et al. The quality evaluation of Lonicerae japonicae Flos, Lonicerae Flos and Lonicerae similis Flos based on multivariate statistical analysis [J]. J Guangdong Pharm Univ, 2020, 36 (5): 620
[13] 王青青,方明月,刘双月,等. HPLC测定市售青风藤中青藤碱和木兰花碱含量[J]. 中国现代中药,2018,20(11):1367
WANG QQ, FANG MY, LIU SY, et al. Content assay of sinomenine and magnoflorine in commercial Caulis sinomenii by HPLC [J]. Mod Chin Med, 2018, 20 (11): 1367
[14] 骆媱,潘娉娉,章建华,等. HPLC法同时测定丹参-当归药对中7个成分的含量[J]. 药物分析杂志,2018,38(10):1689
LUO Y, PAN PP, ZHANG JH, et al. Simultaneous determination of seven components in Radix Salviae Miltiorrhizae-Radix Angelicae Sinensis drug pair by HPLC [J]. Chin J Pharm Anal, 2018, 38 (10): 1689
[15] 杨帆,蒋丽娟,高艳艳,等. 基于对照品和对照提取物的2个含玄参复方和制剂定量研究[J]. 药物分析杂志,2022,42(10):1838
YANG F, JIANG LJ, GAO YY, et al. Quantitative study of two formulation and preparation containing Scrophulariae Radix based on reference substances and reference extract [J]. Chin J Pharm Anal, 2022, 42 (10): 1838
[16] 陈洁,陈文茜,郭文鼎,等. HPLC指纹图谱结合主成分分析对不同产地头顶一颗珠质量的评价[J]. 中国中医药信息杂志,2017,24(11):58
CHEN J, CHEN WQ, GUO WD, et al. Evaluation of quality coherence of Trillium tschonoskii Maxim. from different producing areas based on HPLC fingerprint and PCA [J]. Chin J Inf Tradit Chin Med, 2017, 24 (11): 58
[17] 周冰倩,高喜梅,杨颖,等. 不同来源竹茹药材HPLC指纹图谱和化学计量学分析[J]. 中草药,2022,53(3):853
ZHOU BQ, GAO XM, YANG Y, et al. Quality analysis of Caulis Bambusae in Taeniam from different origins by HPLC coupled with chemometrics [J]. Chin Tradit Herb Drugs, 2022, 53 (3): 853
[18] 冯飞,许金国,严国俊,等. 基于UPLC特征图谱与一测多评法的人参药材质量评价研究[J]. 中国中药杂志,2022,47(13):3530
FENG F, XU JG, YAN GJ, et al. Quality evaluation of Ginseng Radix et Rhizoma based on UPLC characteristic chromatogram and quantitative analysis of multi-components by single marker (QAMS) [J]. China J Chin Mater Med, 2022, 47 (13): 3530
文章导航

/