目的: 建立同仁大活络丸指纹图谱和多指标成分含量测定方法,并应用于10批次同仁大活络丸成品质量检测分析。方法: 采用UPLC-DAD多波长分析方法,使用Waters CORTECS T3色谱柱(100 mm×2.1 mm,1.6 μm),以乙腈-0.3%磷酸水为流动相,梯度洗脱,流速0.4 mL·min-1,柱温38 ℃,检测波长为195 nm(天麻素、麻黄碱、葛根素、苯甲酸、二苯乙烯苷、黄芩苷、丁香酚)和250 nm(小檗碱、甘草酸)。结果: 所建立的指纹图谱和指标性成分含量测定分析方法稳定可行。10批次同仁大活络丸成品指纹图谱相似度均大于0.9,其中9个指标性成分含量测定回收率范围92.7%~104.4%;含量范围:天麻素0.083~0.111 mg·g-1,麻黄碱0.080~0.163 mg·g-1,葛根素0.271~0.366 mg·g-1,苯甲酸1.414~2.070 mg·g-1,二苯乙烯苷0.302~0.608 mg·g-1,黄芩苷0.782~1.390 mg·g-1,小檗碱0.630~0.888 mg·g-1,丁香酚0.619~0.846 mg·g-1,甘草酸0.354~0.762 mg·g-1。结论: 所建立的同仁大活络丸指纹图谱和多指标成分含量测定方法准确、稳定,可用于同仁大活络丸的质量控制。
Objective: To establish the fingerprint and multi-index component determination analysis method of Tongren Dahuoluo pills, and apply it to the quality analysis of 10 batches of Tongren Dahuoluo pills. Methods: UPLC-DAD multi-wavelength analysis method was used, and a Waters CORTECS T3(100 mm×2.1 mm, 1.6 μm) column was used. The mobile phase was acetonitrile-0.3% phosphoric acid water with gradient elution at a flow rate of 0.4 mL·min-1. The column temperature was 38 ℃, and the detection wavelength was set at 195 nm for gastrodin, ephedrine, puerarin benzoic acid, stilbene glucoside, baicalin and eugenol, and 250 nm for berberine and glycyrrhizic acid. Results: The similarities of fingerprints of 10 batches of TRDHL were all above 0.9, and the adding standard recovery range was 92.7%-104.4%. The content ranges of 9 index components were as follows: gastrodin 0.083-0.111 mg·g-1, ephedrine 0.080-0.163 mg·g-1, puerarin 0.271-0.366 mg·g-1, benzoic acid 1.414-2.070 mg·g-1, stilbene glucoside 0.302-0.608 mg·g-1, baicalin 0.782-1.390 mg·g-1, berberine 0.630-0.888 mg·g-1, eugenol 0.619-0.846 mg·g-1 and glycyrrhizic acid 0.354-0.762 mg·g-1. Conclusion: The established fingerprint analysis combined with multi-index content determination method is stable and feasible, which can be used for the quality control of Tongren Dahuoluo pills.
[1] 柳琨, 高雪峰. 大活络丸治疗肺癌开胸术后伤口麻痹疼痛的疗效观察[J].湖北中医药大学学报, 2018, 20(5):64
LIU K, GAO XF. Clinical observation on Dahuoluo pills in treatment of wound paralysis and pain of patients with lung cancer after thoracotomy[J].J Hubei Univ Chin Med, 2018, 20(5):64
[2] WANG YY, ZHANG H, QI Y, et al. Clinical effective evaluation of Tongren Dahuoluo pill on knee osteoarthritis by musculoskeletal ultrasound[J].World J Integr Tradit Western Med, 2020, 6(12):1
[3] 郭中华, 都帅刚, 张仲博, 等. 大活络丸加减治疗股骨头坏死痰瘀阻络证的疗效及安全性[J].中国实验方剂学杂志, 2018, 24(13):172
GUO ZH, DU SG, ZHANG ZB, et al. Clinical efficacy and safety of DaHuoluo pills in treatment of osteonecrosis with phlegm stasis syndrome[J].Chin J Exp Tradit Med Form, 2018, 24(13):172
[4] 黄雪峰. 大活络丸在脑梗死患者神经功能恢复中的作用研究[J].中医药临床杂志, 2014, 26(7):677
HUANG XF. Study on the effect of Dahuoluo pills on the recovery of nerve function in patients with cerebral infarction[J].Clin J Tradit Chin Med, 2014, 26(7):677
[5] 陈晶. 大活络丸治疗类风湿性关节炎的临床观察[J].光明中医, 2013, 28(8):1625
CHEN J. Clinical observation of Dahuoluo pills in treatment of rheumatoid arthritis[J].Guangming J Chin Med, 2013, 28(8):1625
[6] 刘洋, 刘明, 董世芬, 等. 同仁大活络丸对脑缺血再灌注损伤大鼠恢复早期的神经保护作用[J].世界科学技术-中医药现代化, 2012, 14(3):1642
LIU Y, LIU M, DONG SF, et al. Neuroprotective effect of Dahuoluo pill from cerebral ischemia reperfusion injury in rats in early convalescence[J].Mod Tradit Chin Med World Sci Technol, 2012,14(3):1642
[7] 张海鸣, 刘子沐, 王成芳, 等. HPLC法测定同仁大活络丸中黄芩苷的含量[J].西北药学杂志, 2012, 27(1):9
ZHANG HM, LIU ZM, WANG CF, et al. Determination of baicalin in Tongren Dahuoluo pills by HPLC[J].Northwest Pharm J, 2012, 27(1):9
[8] 田进国, 张静, 任健, 等. 同仁大活络丹与同仁牛黄清心丸红外指纹图谱的研究[J].中国中药杂志,2004, 29(4):42
TIAN JG, ZHANG J, REN J, et al. Studies on IR fingerprint of Tongren Dahuoluo pills and Tongren Niuhuangqingxin pills[J].China J Chin Mater Med, 2004, 29(4):42
[9] 郝博, 曹帅, 夏晶, 等. 大活络丸及其同系列品种中牛黄的质量分析研究[J].药物分析杂志, 2016, 36(8):1470
HAO B, CAO S, XIA J, et al. Quality analysis of Bovis Calculus in Dahuoluo pills and its homologous series[J].Chin J Pharm Anal, 2016, 36(8):1470
[10] 郭琪, 杨莹, 雷虹. 一测多评法测定大活络丸中6种指标性成分的研究[J].解放军药学学报, 2018, 34(4):355
GUO Q, YANG Y, LEI H. Quantitative analysis of six index components of Dahuoluo pills using single maker method[J].Pharm J Chin PLA, 2018, 34(4):355
[11] 张晓娟. 大活络丸质量评价性研究[D].张家口:河北北方学院, 2016
ZHANG XJ. Evaluative Research of the Quality of Dahuoluo Pills[D].Zhangjiakou:Hebei North University, 2016
[12] 王欣美, 王枚博, 吴赵云, 等. 大活络丸的质量标准研究[J].中国实验方剂学杂志, 2013, 19(14):145
WANG XM, WANG MB, WU ZY, et al. Study on the quality standard of Dahuoluo Wan[J].Chin J Exp Tradit Med Form, 2013, 19(14):145
[13] 胡青, 钟吉强, 毛秀红, 等. 液质联用法检测大活络丸和同仁大活络丸中贵毒药味和添加化合物[J].药物分析杂志, 2010, 30(8):1593
HU Q, ZHONG JQ, MAO XH, et al. LC-MS detection of valuable or toxic ingredients and 48 chemical drugs added into Dahuoluo pills and Tongren Dahuoluo pills[J].Chin J Pharm Anal, 2010, 30(8):1593
[14] 谢巧, 车静, 廖莉, 等. 安息香属植物化学成分及药理作用研究进展[J].中药材, 2020, 43(1):243
XIE Q, CHE J, LIAO L, et al. Advances in studies on chemical constituents and pharmacological effects of benzoin[J].J Chin Med Mater, 2020, 43(1):243
[15] 张丽, 张卿, 梁秋明, 等. 安息香化学成分及其体外抗肿瘤活性[J].中国实验方剂学杂志, 2020, 26(4):191
ZHANG L, ZHANG Q, LIANG QM, et al. Chemical constituents of Benzoinum and its anti-tumor activities in vitro[J].Chin J Exp Tradit Med Form, 2020, 26(4):191
[16] 谢巧, 廖莉, 栗圣榕, 等. 基于色度原理分析安息香颜色与化学成分的相关性[J].中成药, 2020, 42(9):2372
XIE Q, LIAO L, LI SR, et al. Analysis of correlation between color and chemical constituents of benzoin based on chroma principle[J].Chin Tradit Pat Med, 2020, 42(9):2372
