Objective: To determine the contents of five constituents (cinnamaldehyde, cryptotanshinone, tanshinone Ⅰ, atractylodin, tanshinone ⅡA) in Yishen Juanbi capsules and to establish the HPLC fingerprints. Methods: A quantitative analysis of multi-components by single-marker(QAMS) method was developed to determine cinnamaldehyde, cryptotanshinone, tanshinone I, atractylodin and tanshinone ⅡA. Tanshinone ⅡA was selected as internal reference and the relative correction factors (RCFs) of other four components were calculated. The QAMS method was evaluated by external standard method. The analysis was performed on a column of Kromasil 100-5 C18 (250 mm×4.6 mm, 5 μm) with gradient elution of acetonitrile-0.02% phosphoric acid aqueous solution at a flow rate of 1.0 mL·min-1. The detection wavelengths were set at 270 nm, and the column temperature was 20 ℃. The fingerprints of Yishen Juanbi capsules were established by HPLC, and evaluated by similarity evaluation, cluster analysis (CA) and principal component analysis (PCA) . The analysis was performed on a column of Agilent 5 TC-C18 (250 mm×4.6 mm, 5 μm) with gradient elution of acetonitrile-0.02% phosphoric acid aqueous solution at a flow rate of 1.0 mL·min-1. The detection wavelengths were set at 320 nm and 270 nm, and the column temperature was 20 ℃. Results: The established RCFs had a good reproducibility. No significant differences were found between the quantitative results of external standard method and QAMS method. Relative errors of the two methods were within ±2%. The HPLC fingerprint of Yishen Juanbi capsules was established with 36 common peaks, and 12 constituents were identified by comparing with the control product spectrogram. The similarities of 10 batches of samples were all above 0.95. The contents of cinnamaldehyde, cryptotanshinone, tanshinone Ⅰ, atractylodin, tanshinone ⅡA in 3 batches of samples were 0.077-0.244, 0.402-0.472, 0.098-0.136, 0.086-0.186, 0.454-0.517 mg·g-1 respectively by QAMS.There was no significant difference between the QAMS and the ESM. Conclusion: The established method of QAMS and HPLC fingerprint analysis is simple, accurate and reproducible, and can provide a reference for the quality evaluation of Yishen Juanbi capsules.
[1] 郭海明, 郭来旺. 蚁参蠲痹胶囊治疗类风湿关节炎的临床研究[J].中国药物与临床, 2009,9(5):439
GUO HM, GUO LW. Clinical research of Yishen Juanbi capsules in the treatment of rheumatoid arthritis[J].Chin Rem Clin, 2009, 9(5):439
[2] 王智民, 高慧敏, 付雪涛, 等. “一测多评”法中药质量评价模式方法学研究[J].中国中药杂志, 2006, 31(23):1925
WANG ZM, GAO HM, FU XT, et al. Multi-components quantitation by one marker new method for quality evaluation of Chinese herbal medicine[J].China J Chin Mater Med, 2006, 31(23):1925
[3] 周霖, 孙志, 薛文华, 等. 基于UPLC指纹图谱结合化学模式识别的丹灯通脑软胶囊质量控制研究[J].中国中药杂志, 2018, 43(16):3279
ZHOU L, SUN Z, XUE WH, et al. Quality control of Dandeng Tongnao Ruanjiaonang based on UPLC fingerprint combined with chemical pattern recognition[J].China J Chin Mater Med, 2018, 43(16):3279
[4] 王康华, 张英涛, 杨秀伟, 等. 妇科千金胶囊HPLC特征图谱和多指标成分定量分析[J].中国中药杂志, 2019,44(8):1564
WANG KH, ZHANG YT, YANG XW, et al. Characterisitic fingerprint and multi-components quantitative determination for Fuke Qianjin capsules by HPLC[J].China J Chin Mater Med, 2019, 44(8):1564
[5] 吴笛, 臧忠良, 王德勤, 等. 一测多评法测定复方丹参片中4种丹参酮类成分的含量[J].中国药学杂志, 2012, 47(18):1509
WU D, ZANG ZL, WANG DQ, et al. Simultaneous determination of four tanshinones in compound Salvia Miltrorrhiza tablets by quantitative analysis of muti-components by single marker[J].Chin Pharm J, 2012,47(18):1509
[6] 张凯月, 李志成, 张晔, 等. 一测多评法同时测定十味香鹿胶囊中5个人参皂苷[J].中成药, 2020,42(3):583
ZHANG KY, LI ZC, ZHANG Y, et al. Simultaneous determination of five ginsenosides in Shiwei Xianglu capsules by QAMS[J].Chin Tradit Pat Med, 2020,42(3):583
[7] 廖晓虎, 潘其麟, 王晓晓, 等. 基于一测多评法的复方丹参片质量评价研究[J].亚太传统医药, 2019, 15(11):46
LIAO XL, PAN QL, WANG XX, et al. Quality evaluation of Fufang Danshen tablets based on quantitative analysis of multi-components by singer-marker[J].Asia Pac Tradit Med, 2019,15(11):46
[8] 王智民,钱忠直,张启伟,等.一测多评法建立的技术指南[J].中国中药杂志, 2011, 36(6):657
WANG ZM, QIAN ZZ, ZHANG QW, et al. The guidelines for establishment of QAMS[J].China J Chin Mater Med, 2011, 36(6):657
[9] 武爱玲. 一测多评法与外标法测定养血止疼丸中3种丹参酮类成分[J].世界中医药, 2017, 12(11):2783
WU AL. Simultaneous determination of 3 tanshinones in Yangxue Zhiteng pills by QAMS[J].Word Chin Med, 2017, 12(11):2783
[10] 中华人民共和国药典2020年版. 一部[S].2020: 77
ChP 2020. Vol Ⅰ[S].2020:77
[11] 计思敏. 白花、紫花丹参中丹参酮类成分的差异性及其抗类风湿性关节炎的作用研究[D].武汉: 湖北中医药大学, 2017
JI SM. Research of Difference of Chemical Compositions between Tanshinones from Salvia miltiorrhiza Bunge. f. alba. and Salvia miltiorrhiza Bunge. s and Its Anti-Inflammatory Activities[D].Wuhan: Hubei University of Chinese Medicine, 2017
[12] 张珊. 丹参酮ⅡA通过调节中性粒细胞活性治疗类风湿关节炎的研究[D].北京: 北京中医药大学, 2017
ZHANG S. Tanshinone ⅡA Ameliorates Chronic Arthritis in Mice by Modulating Neutrophil Activities[D].Beijing: Beijing University of Chinese Medicine, 2017
[13] 徐西林, 张晓峰, 吕航, 等. 丹参注射液对骨性关节炎模型兔膝关节软骨细胞p-IκBα 表达影响的实验研究[J]. 中国中医药科技, 2017, 24(4):438
XU XL, ZHANG XF, LÜ H, et al. Experimental study on effect of Salvia miltrorrhiza injection on p-IκBα protein expression in knee articular chondrocytes of rabbits with osteoarthritis[J].Chin Med Technol, 2017, 24(4):438
[14] 樊国琴, 刘春芳, 赵娟, 等. 道地和非道地苍术对类风湿性关节炎大鼠病情及促炎细胞因子和炎症介质的影响[J].中国中药杂志, 2010, 35(20):2731
FAN GQ, LIU CF, ZHAO J, et al. Comparative study of effect of Atractylodes lancea between geo-authentic and non-authentic producing areas on collagen-induced arthritis in rats[J].China J Chin Mater Med, 2010, 35(20):2731
[15] 夏天卫, 周国威, 姚晨, 等. 桂枝及肉桂治痹的中医认识与现代药学研究进展[J].中国实验方剂学杂志, 2019, 25(6):218
XIA TW, ZHOU GW, YAO C, et al. Troditional Chinese medicine cognition and modern pharmaceutical research on effect of cassia twig and Cinnamomum cassia in treating paralysis[J].Chin J Exp Tradit Med Form, 2019, 25(6):218
[16] QADIR MMF, BHATTI A, ASHRAF MU, et al. Immunomodulatory and therapeutic role of Cinnamomum verum extracts in collagen-induced arthritic BALB/c mice[J].Inflammopharmacology, 2018, 26(1):157
[17] 徐依依. 基于苍术燥性对RA药效学及代谢组学研究[D].武汉: 湖北中医药大学, 2020
XU YY. Study on Rheumatoid Arthritis Pharmacodynamics and Metabolomics Based on Atractylodes macrocephala[D].Wuhan: Hubei University of Chinese Medicine, 2020
[18] 张保国, 李昌勤, 刘庆芳. 蚂蚁的临床研究与应用[J].中成药, 2004, 26(8):68
ZHANG BG, LI CQ, LIU QF. Clinical research and application of ants[J].Chin Tradit Pat Med, 2004, 26(8):68
[19] 王忠, 袁国英, 张继贵, 等. 复方玄驹口服液补肾壮阳药效学研究[J].中药新药与临床药理, 1996, 7(2):51
WANG Z, YUAN GY, ZHANG JG, et al. Pharmacodynamic study of compound Xuanju oral liquid for invigorating kidney and strengthening Yang[J].Tradit Chin Drug Res Clin Pharmacol, 1996,7(2):51
[20] 黄芳, 蒋娅兰, 吴惠勤, 等. 衍生化HPLC法测定蚂蚁制品中的蚁酸的含量[J].中成药, 2016, 38(12):2713
HUANG F, JIANG YL, WU HQ, et al. Determination of formic acid in ant products by derivatization HPLC method [J].Chin Tradit Pat Med, 2016, 38(12):2713
[21] 邹耀华, 殷红妹, 刘宇文. 衍生色谱法测定蚂蚁中蚁酸含量[J].中国卫生检验杂志, 2010, 20(8):1880
ZOU YH, YIN HM, LIU YW. Determination of formic acid in ants by derivation chromatography[J].Chin J Health Lab Technol, 2010, 20(8):1880
[22] 符影, 程悦, 陈建萍, 等. 鸡血藤化学成分及药理作用研究进展[J].中草药, 2011, 42(6):1229
FU Y, CHENG Y, CHEN JP, et al. Advances in studies on chemical constituents in Spatholobi Caulis and their pharmacological activities[J].Chin Tradit Herb Drugs, 2011, 42(6):1229
