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.
作者
楚世慈
吴飞
张磊
吴伟
胡志强
陈佳薇
洪燕龙
CHU Shi-ci;WU Fei;ZHANG Lei;WU Wei;HU Zhi-qiang;CHEN Jia-wei;HONG Yan-long(Shanghai University of Traditional Chinese Medicine TCM Health Service Collaborative Innovation Center,Shanghai 200120,China;Innovative Chinese Medicine Research Institute of Shanghai University of Traditional Chinese Medicine, Shanghai 200120,China;Jiangsu Kanion Pharmaceutical Limited by Share Ltd,Jiangsu Nanjing 222001,China;Department of Hematology,Affiliated People's Hospital of Fujian University of traditional Chinese Medicine,Fujian Fuzhou 350004,China)
出处
《中国医院药学杂志》
CAS
北大核心
2019年第2期146-150,共5页
Chinese Journal of Hospital Pharmacy
基金
国家科技重大专项(重大新药创制)(项目编号:2018-ZX09731016)
上海市卫计委中医药科技创新项目(ZYKC201603003)
关键词
栀黄芍药散
栀子
白芍
大黄
多成分同时测定
HPLC
Zhihuang Shaoyao powder
Fructus gardeniae
Radix Paeoniae Alba
Rhubarb
simultaneous determination
HPLC
