目的: 建立UPLC指纹图谱及多指标定量测定结合化学模式的参芪博力康片质量评价方法。方法: 采用Waters BEH C18色谱柱（2.1 mm×100 mm,1.7 μm）,柱温30 ℃,以乙腈-0.1%甲酸流动相,为梯度洗脱,流速0.3 mL · min-1进样量1 μL。利用中药指纹图谱相似度评价软件对10批参芪博力康片建立指纹图谱,并确定共有峰,进行相似度评价,对人参皂苷Rg1、人参皂苷Re、朝藿定A、朝藿定B、人参皂苷Rf、五味子醇甲、人参皂苷Rb1、黄芪甲苷、人参皂苷Ro多组分含量测定方法进行方法学验证。基于指纹图谱共有峰峰面积测定结果,采用聚类分析法、主成分分析法等化学计量学方法进行评价。结果: 在指纹图谱中,确定25个共有峰,采用对照品指认出其中9个共有峰,并进行含量测定。9个成分精密度、重复性、稳定性RSD均小于3%,在各自不同进样量范围内线性关系良好,平均加样回收率在98.12%~107.14%,RSD为0.89%~2.4%,人参皂苷Rg1、人参皂苷Re、朝藿定A、朝藿定B、人参皂苷Rf、五味子醇甲、人参皂苷Rb1、黄芪甲苷、人参皂苷Ro含量分别为0.091~0.603、0.097~0.669、0.055~0.076、0.100~0.157、0.055~0.199、0.116~0.275、0.190~1.264、0.238~0.370、0.089~0.295 mg · g-1。聚类分析中,10批样品共聚为3类,与生产年限保持一致。主成分分析中成分1~3是主要因子。结论: 所建立的参芪博力康片质量评价方法准确度高,稳定性良好,具有可重复性,可用于参芪博力康片质量的控制。
Objective: To establish a quality evaluation method for Shenqi Bolikang tablets based on UPLC fingerprint and multi-index quantitative determination combined with chemometric methods. Methods: A Waters BEH C18 Column (2.1 mm×100 mm, 1.7 μm) was used at 30 ℃, the mobile phase consisted of acetonitrile and 0.1%formic acid in water with gradient elution. The flow rate was 0.3 mL · min-1, and injection volume was 1 μL. Similarity evaluation system for chromatographic fingerprint of traditional Chinese medicine was used to establish fingerprints for 10 batches of Shenqi Bolikang tablets, and the common peaks were determined to evaluate the similarity. The methods for simultaneous quantification of nine components were validated, including ginsenoside Rg1, ginsenoside Re, epimedin A, epimedin B, ginsenoside Rf, schisadrin, ginsenoside Rb1, astragaloside IV and ginsenoside Ro. Based on the results of fingerprint common peak area measurement, chemometric methods such as cluster analysis and principal component analysis were used for evaluation. Results: In the fingerprint chromatogram, 25 common peaks were indexed, 9 of which were identified with the reference substance, and their contents were determined. The RSD of precision, repeatability and stability of the nine components was less than 3%, and the linear relationship was good in the tested concentration ranges, the average recovery rate was 98.12%-107.14%, the RSD was 0.89%-2.4%, and the contents of ginsenoside Rg1, ginsenoside Re, epimedin A, epimedin B, ginsenoside Rf, schisandrin, ginsenoside Rb1, astragaloside IV and ginsenoside Ro were 0.091-0.603 mg · g-1, 0.097-0.669 mg · g-1, 0.055-0.076 mg · g-1, 0.100-0.157 mg · g-1, 0.055-0.199 mg · g-1, 0.116-0.275 mg · g-1, 0.190-1.264 mg · g-1, 0.238-0.370 mg · g-1, 0.089-0.295 mg · g-1, respectively. In the cluster analysis, the 10 batches of samples were clustered into 3 categories, which were consistent with the production years. In principal component analysis, components 1~3 were the main factors. Conclusion: The established method for evaluating the quality of Shenqi Bolikang tablets has high accuracy, good stability and reproducibility, which can be used to control the quality of Shenqi Bolikang tablets.
[1] 白仲梅,魏学冰.高效液相色谱法测定参芪博力康片中淫羊藿苷的含量[J].兰州大学学报(医学版),2010,36(2):61
BAI ZM,WEI XB.Determination of icariin Shenqibolikang tablets by high performance liquid chromatography[J].J Lanzhou Univ(Med Sci),2010,36(2):61
[2] 李军涛,李向前,任利民,等.HPLC法同时测定参芪博力康片中7种成分的含量[J].西北药学杂志,2020,35(6):823
LI JT,LI XQ,REN LM,et al.Simultaneous determination of 7 components in Shenqibolekang tablets by HPLC[J].Northwest Pharm J,2020,35(6):823
[3] 张晓虹,曹雪芹,董欣昱,等.参芪博力康片中人参薄层鉴别方法的比较研究[J].中国高新科技,2022,(4):133
ZHANG XH,CAO XQ,DONG XY,et al.Comparative research on identification methods of ginseng thin layer in Shenqi Bolikang tablets[J].China High New Technol,2022,(4):133
[4] 廖嘉穗,付娟,张日美,等.基于HPLC指纹图谱结合化学计量学及多成分定量测定的腰痹通胶囊质量评价研究[J].中草药,2024,55(8):2579
LIAO JS,FU J,ZHANG RM,et al.Quality evaluation of Yaobitong capsules based on HPLC fingerprint combined with chemometrics and multi-component determination[J].Chin Tradit Herb Drugs,2024,55(8):2579
[5] 祁航,谢涛,吕东峰,等.玉泉丸HPLC指纹图谱的建立及6个成分定量分析[J].中草药,2019,50(23):5753
QI H,XIE T,LÜ DF,et al.Establishment of HPLC fingerprint of Yuquan pills and quantitative analysisof six components[J].Chin Tradit Herb Drugs,2019,50(23):5753
[6] 吴琳琳. 基于液相色谱-电喷雾检测器联用技术的中药质量分析方法学研究[D].杭州:浙江大学,2022
WU LL.Studies on the Methodologies of Quality Analysis of Traditional Chinese Medicine using High Performance Liquid Chromatography with Charged Aerosol Detection technology[D].Hangzhou:Zhejiang University,2022
[7] 李婷,程显隆,游蓉丽,等.HPLC-CAD法测定芪蛭通络胶囊中苷类成分的含量[J].中国药学杂志,2022,57(14):1193
LI T,CHENG XL,YOU RL,et al.Determination of saponins in Qizhitongluo capsules by HPLC-CAD[J].Chin Pharm J,2022,57(14):1193
[8] 南易,郑伟,马凤霞,等.HPLC-CAD同时测定知母中芒果苷和知母皂苷B Ⅱ的含量[J].药物分析杂志,2021,41(1):111
NAN Y,ZHENG W,MA FX,et al.Simultaneous determination of mangiferin and timosaponin B Ⅱof Anemarrhenae Rhizoma by HPLC-CAD[J].Chin J Pharm Anal,2021,41(1):111
[9] 房思萌,隋玉荣,韩晓捷.高效液相色谱-电喷雾检测器测定熊去氧胆酸的有关物质[J].药物分析杂志,2023,43(9):1523
FANG SM,SUI YR,HAN XJ.Determination of ursodeoxycholic acid by HPLC-CAD[J].Chin J Pharm Anal,2023,43(9):1523
[10] 张春泥,王英姿,孙欣光,等.HPLC-CAD结合化学计量学的川楝子饮片指纹图谱研究[J].药学学报,2017,52(3):456
ZHANG CN,WANG YZ,SUN XG,et al.Chromatographic fingerprint analysis of Toosendan Fructus by HPLC-CAD coupled with chemometrics methods[J].Acta Pharm Sini,2017,52(3):456
[11] 陈学松. 马鞭草HPLC-CAD指纹图谱及主要成分的测定[J].中草药,2017,48(10):2007
CHEN XS.Chromatographic fingerprint and multi-components quantitative analysis of Verbena officinalis by HPLC-CAD[J].Chin Tradit Herb Drugs,2017,48(10):2007
[12] 刘蓬蓬,鞠成国,林桂梅,等.HPLC-CAD分析黄芪甲苷提取过程中黄芪皂苷类成分动态变化[J].中国中医药信息杂志,2022,29(11):92
LIU PP,JU CG,LIN GM,et al.Dynamic changes of saponins in the process of astragaloside IV extract using HPLC-CAD[J].Chin J Inf Tradit Chin Med,2022,29(11):92
[13] 程巧鸳,唐登峰,马临科,等.基于指纹图谱及多指标成分定量的健儿消食口服液质量评价[J].药物分析杂志,2016,36(1):148
CHENG QY,TANG DF,MA LK,et al.Quality evaluation of Jianerxiaoshi mixture by HPLC fingerprint and multi-component quantitative analysis[J].Chin J Pharm Anal,2016,36(1):148
[14] 贵书琪,郑艳萍,成俊,等.基于量值传递的仁术健胃颗粒工艺过程研究[J].中成药,2024,46(3):940
GUI SQ,ZHENG YP,CHENG J,et al.Research on the process of Renzhu stomach granules based on quantity value transfer[J].Chin Tradit Pat Med,2024,46(3):940
[15] 王铮,吕益涛,蒋倩倩,等.高效液相色谱法测定复方黄芪健脾口服液中黄芪甲苷含量[J].中国药业,2023,32(10):68
WANG Z,LÜ YT,JIANG QQ,et al.Content determination of astragaloside Ⅳ in compound Huangqi Jianpi oral liquid by HPLC[J].China Pharm,2023,32(10):68
[16] 崔灿,王琳,雷勇胜.HPLC-CAD法同时测定益肺清化颗粒的七种成分[J].海峡药学,2022,34(7):33
CUI C,WANG L,LEI YS.Simultaneous determination of 7 constituents in Yifei Qinghua granules by HPLC-CAD[J].Strait Pharm J,2022,34(7):33
