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作 者:田香 丁瑞雪 巴根那[3] 白玉霞[3] 拉喜那木吉拉 饶小勇[1,2] 罗晓健[1,2] TIAN Xiang;DING Rui-xue;BA Gen-na;BAI Yu-xia;LAXI Na-mu-ji-la;RAO Xiao-yong;LUO Xiao-jian(Jiangxi University of Traditional Chinese Medicine,Nanchang 330006,China;National Pharmaceutical Engineering Center for Solid Preparation in Chinese Herbal Medicine,Nanchang 330006,China;Mongolian Medicine College,Inner Mongolia University for Nationalities,Tongliao 028000,China)
机构地区:[1]江西中医药大学,江西南昌330006 [2]中药固体制剂制造技术国家工程研究中心,江西南昌330006 [3]内蒙古民族大学蒙医药学院,内蒙古通辽028000
出 处:《中国中药杂志》2018年第19期3962-3969,共8页China Journal of Chinese Materia Medica
摘 要:建立蒙药地格达-4味汤(DGD-4D)HPLC指纹图谱,测定秦皮乙素、栀子苷、胡黄连苷Ⅰ和胡黄连苷Ⅱ含量,为DGD-4D质量控制提供依据。采用Diamonsil(2) C18(4.6 mm×250 mm,5μm)色谱柱,甲醇-0.1%磷酸水溶液为流动相,梯度洗脱,流速1.0 mL·min^-1,进样量10μL,检测波长254 nm,柱温30℃。建立15批DGD-4D HPLC指纹图谱共有模式,并采用化学计量学分析方法分析隐藏信息。采用HPLC对DGD-4D色谱峰进行指认,并对特征峰进行定量分析。建立DGD-4D HPLC指纹图谱,指认出17个共有峰,相似度均在0.9以上。主成分分析和聚类分析将样品大致分为4类。并结合偏最小二乘判别分析方法发现区分DGD-4D样品的4个标志性化合物,其中指认出栀子苷(9号峰)、胡黄连苷Ⅰ(14号峰)和胡黄连苷Ⅱ(12号峰)。定量分析条件通过方法学验证,平均加样回收率在95.91%~97.31%。对HPLC指纹图谱和主要成分同时进行分析,方法快速、简便、重复性好,可作为蒙药地格达-4味汤质量控制有效方法之一。To establish the high performance liquid chromatography(HPLC) fingerprint for Digeda-4 decoction(DGD-4 D), determine the contents of aesculetin, geniposide, picroside Ⅰ, picroside Ⅱ and ellagicacid in DGD-4 D, and provide the scientific foundation for quality control of DGD-4 D. The analysis was performed on Diamonsil(2)C18(4.6 mm×250 mm,5 μm) column, with methanol-0.1% phosphoric acid aqueous solution as mobile phase for gradient elution. The flow rate was 1.0 mL·min^-1;injection size was 10 μL;temperature was maintained at 30 ℃, and the detection wavelength was set at 254 nm. The common mode of DGD-4 D HPLC fingerprint was established, and the hidden information was analyzed by Chemometrics. Chromatographic peaks for DGD-4 D were identified by HPLC and quantitative analysis was conducted for characteristic peaks. There were 17 common peaks in the fingerprints and the similarity of the fingerprints was over 0.9 in all 15 batches. The samples were broadly divided into four kinds by principal component analysis and clustering analysis. Four marker compounds were verified by partial least squares discriminant analysis, and No. 9, 12 and 14 peaks were identified as geniposide, picroside Ⅱ, and picroside Ⅰ respectively. The average recoveries were in the range of 95.91%-97.31%. The HPLC fingerprint method for content determination is reliable, accurate, rapid, simple, and reproducible, and can be used as one of the effective methods to control the quality of DGD-4 D.
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