高效液相色谱法同时测定栀黄芍药散乙醇提取物中7个成分的含量
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摘要
目的:建立高效液相色谱法(HPLC)用于同时测定栀黄芍药散乙醇提取物中栀子苷、芍药苷、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚的含量。方法:采用Kromasil100-5C18 (4.6 mm×250 mm,5μm)色谱柱,流动相为乙腈(A)-0.1%磷酸水溶液(B)系统,梯度洗脱(0～11 min,15%A～85%B;11～43 min,15%A～85%B→80%A～20%B;43～60min,15%A～85%B),流速1.0 mL·min-1,检测波长为230 nm,柱温25℃,进样量10μL。结果:栀子苷、芍药苷、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚线性范围分别为20.11～502.75μg (r=0.999 9),4.02～100.50μg (r=0.999 8),0.20～5.00μg (r=0.999 8), 0.60～15.00μg (r=0.999 8), 0.20～5.00μg (r=0.999 8), 0.40～10.00μg (r=0.999 9), 0.32～8.00μg (r=0.999 9)。加样回收率分别为100.78%,97.96%,100.41%,100.85%,104.98%,101.28%,100.97%;RSD分别为1.8%,1.5%,1.8%,1.6%,2.1%,1.4%,0.8%。结论:该方法专属性强、准确可靠,可用于栀黄芍药散乙醇提取物及其制剂的质量控制。
OBJECTIVE To establish an HPLC method for simultaneous determination of geniposide, paconiflorin,rhein, emodin, chrysophanol, aloe-emodin, and rhyscion in Zhihuang Shaoyao powder extracted with ethanol. METHODSThe separation was performed on Kromasil 100-5C18 column(4.6 mm×250 mm, 5 μm) with gradient elution at a temperature of 25 ℃ and a flow rate of 1.0 mL*min-1, and a sample size of 10 L. The acetonitrile and 0.1% phosphoric acid were used as the mobile phase with gradient elution(0–11 min, 15%A–85%B;11–43 min, 15%A–85%B→80%A–20%B;43–60 min,15%A–85%B) and the detection wavelength was 230 nm. RESULTS The calibration curves of geniposide, paconiflorin,aloe-emodin, rhein, emodin, chrysophanol and rhyscion were in good linearity over the ranges of 20.11–502.80 μg(r = 0.9999), 4.02 –100.60 μg(r = 0.999 8), 0.20–5.00 μg(r = 0.999 8), 0.60–15.02 μg(r = 0.999 8), 0.20–5.02 μg(r =0.999 8), 0.40–10.02μg(r=0.999 9), 0.32–8.03 μg(r=0.999 9). The average recoveries were 100.78%, 97.96%, 100.41%, 100.85%, 104.98%,101.28%, 100.97%, and RSD values were 1.8%, 1.5%, 1.8%, 1.6%, 2.1%, 1.4%, 0.8%. CONCLUSION The method is precise, specific, reliable, and can be used to determine the quality of Zhihuang Shaoyao powder extracted with ethanol and its preparation.
OBJECTIVE To establish an HPLC method for simultaneous determination of geniposide, paconiflorin,rhein, emodin, chrysophanol, aloe-emodin, and rhyscion in Zhihuang Shaoyao powder extracted with ethanol. METHODSThe separation was performed on Kromasil 100-5C18 column(4.6 mm×250 mm, 5 μm) with gradient elution at a temperature of 25 ℃ and a flow rate of 1.0 mL*min-1, and a sample size of 10 L. The acetonitrile and 0.1% phosphoric acid were used as the mobile phase with gradient elution(0–11 min, 15%A–85%B;11–43 min, 15%A–85%B→80%A–20%B;43–60 min,15%A–85%B) and the detection wavelength was 230 nm. RESULTS The calibration curves of geniposide, paconiflorin,aloe-emodin, rhein, emodin, chrysophanol and rhyscion were in good linearity over the ranges of 20.11–502.80 μg(r = 0.9999), 4.02 –100.60 μg(r = 0.999 8), 0.20–5.00 μg(r = 0.999 8), 0.60–15.02 μg(r = 0.999 8), 0.20–5.02 μg(r =0.999 8), 0.40–10.02μg(r=0.999 9), 0.32–8.03 μg(r=0.999 9). The average recoveries were 100.78%, 97.96%, 100.41%, 100.85%, 104.98%,101.28%, 100.97%, and RSD values were 1.8%, 1.5%, 1.8%, 1.6%, 2.1%, 1.4%, 0.8%. CONCLUSION The method is precise, specific, reliable, and can be used to determine the quality of Zhihuang Shaoyao powder extracted with ethanol and its preparation.
引文
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[19] Wang XP, Cui XM, He Y, et al. Simultaneous determination of 5 index components in Yuyin tablets by HPLC[J]. Chin Hosp Pharm J(中国医院药学杂志),2018, 38(03):242-245.
[2] Ge GY. Zhizi Dahuang power External application in the treatment of 54 cases of acute soft tissue injury[J]. Shanxi J Tradit Chin Med(陕西中医杂志),1998(03):55.
[3] Chen SH, Liu HY,Zhong GS. The effect of external use of Gardenia jasminoides on swelling and analgesic effect[A].Proceedings of the eighteenth China national pharmaceutical history and Herbal Medicine Symposium,Specialized Committee(第十八届全国药学史暨本草学术研讨会学术论文集),2015, 2:280-281.
[4] Hao SJ, Pan D. Clinical effect of external application of Gardenia powder in the treatment of soft tissue injury in the ankle[N]. J Hubei Institute for Natlities(湖北民族学院学报),2015, 32(1):68.
[5] Cai H. The treatment of acute contusion and sprain with gardenia powder[N]. Chin J Tradit Chin Med(中国中医药2014, 9(24):005.
[6] Pan WJ, Zhang XR, Lv QQ. External application of raw Gardenia powder in treatment of 100 cases of traumatic soft tissue and pain[J]. Zhejiang J Tradit Chin Med(浙江中医杂志),2011,46(3):192.
[7] Guo JH, Liu X. Progress in the study of iridoid glycosides of traditional Chinese Medicine[J]. Drug Evaluation Research(药物评价研究),2011,34(4):293.
[9] Ch. P. Vol(中国药典).一部[S].2015:23-24;105;248.
[10] Ou ZC, Yu JW. Effect of rhubarb powder and vinegar on external application in the treatment of acute ankle sprain[J]. Strait Pharm J(海峡药学),2016, 28(07):201-203.
[11] Dai DS, Cui SZ. Current situation and progress of rhubarb external use[J]. Guangming Tradit Chin Med(光明中医),2006,(11):57.
[12] Yang WX. olecular mechanism of anti cancer, antiinflammatory and antiviral effects of anthraquinone derivatives of rhubarb(a review)[A].Paper collection of the2004 annual meeting of the Tianjin Biomedical Engineering Society[C]. Tianjin Institute of Biomedical Engineering(天津生物工程协会论文集),2005:1.
[14] Liu J. Research progress in pharmacological activity and pharmacological activity of rhubarb[A]. The tenth Academic Conference on TCM identification of Chinese society of traditional Chinese medicine and a symposium on methods and Technical Symposium on the identification of Chinese medicinal materials in WHO[C]. Chinese traditional Chinese Medicine Association of Chinese medicine identification branch(中华中医药学会论文集),2010:7. 374-380.
[15] Zhang L. Pharmacological action and modern research progress of Paeonialactiflora[J]. Clinical Res J of Tradit Chin Med(中医临床研究),2014, 6(29):25-26.
[16] Liu WZ, Fan JW, Gao YH, et al. Simultaneous determination of eight iridoid glycosides in Gardeniae Fructus by HPLC[J]. Chinese Journal of Pharmaceutical Analysis(药物分析杂志),2012, 37(16):2417-2421.
[17] Shi YQ, Tang SH, Wang AJ. Simultaneous Determination of geniposide, paeoniflorin, baicalin, berberine hydrochloride and emodin in HuanglianShuangqing Pills by HPLC.[J].Chin JPharm Anal(药物分析杂志),2013, 28(25):1615-1616.
[18] Liu CL, Liu DH, Huang YC, et al. HPLC Fingerprint Analysis of Medicinal Slices of Radix et RhizomaRhei[J]. Traditional Chinese Drug Research&Clinical Pharmacology(中药新药于临床药理), 2009, 20(5):442-445.
[19] Wang XP, Cui XM, He Y, et al. Simultaneous determination of 5 index components in Yuyin tablets by HPLC[J]. Chin Hosp Pharm J(中国医院药学杂志),2018, 38(03):242-245.