【摘要】 目的:建立滇重楼地上部分总皂苷高效液相色谱法（HPLC）指纹图谱,为滇重楼地上部分总皂苷的质量控制提供参考。方法:采用Ecosil HPLC C₁₈色谱柱（250 mm×4.6 mm, 5μm）进行分离,流动相为乙腈-水溶液,梯度洗脱,流速为1.0 mL·min^-1,检测波长为203 nm,柱温为31℃。建立6批滇重楼地上部分总皂苷HPLC特征图谱,并进行相似度评价;采用硅胶、反向硅胶RP-C₁₈柱色谱等方法对特征图谱中的3个未知共有峰化合物进行分离,应用质谱法（MS）、核磁共振（NMR）等方法进行结构鉴定;参照各对照品的色谱行为及其二极管阵列检测器（DAD）紫外光谱图,对共有峰进行归属和指认。结果:指纹图谱中的3个未知共有峰化合物为偏诺皂苷元-3-O-α-L-吡喃鼠李糖基-（1→4）-[α-L-吡喃鼠李糖基-（1→4）]-β-D-吡喃葡萄糖苷（cld01）、偏诺皂苷元-3-O-α-L-吡喃鼠李糖基-（1→4）-β-D-吡喃葡萄糖苷（cld02）、薯蓣皂苷元-3-O-α-L-吡喃鼠李糖基-（1→4）-[α-L-吡喃鼠李糖基-（1→4）]-β-D-吡喃葡萄糖苷（cld03）。cld02为首次从该植物中分离得到,cld03为首次从该植物地上部分分离得到;6批样品特征图谱与对照图谱的相似度均大于0.99,共归属指认了7个共有峰。结论:所建立的HPLC指纹图谱方法稳定、可靠、重复性好,可为滇重楼地上部分总皂苷质量控制提供参考。更多还原

【Abstract】 Objective:To establish the high performance liquid chromatography（HPLC） fingerprint of the total saponins of the above ground part of Paris polyphylla var.yunnanenis,and to provide the basis for the quality control of the total saponins of the above ground part of P. polyphylla var. yunnanenis. Methods:Silica gel and lichroprep RP-C₁₈ column chromatography were used to separate the three unknown common peak compounds in the fingerprint, and the mass spectrometry（MS）,nuclear magnetic resonance（NMR） were used to identify the structure; HPLC analysis was performed on Ecosil HPLC C₁₈ column（250 mm×4.6 mm, 5 μm）. The mobile phase was acetonitrile-water, gradient elution with the flow rate was 1.0 mL·min^-1,the detection wavelength was 203 nm, and the column temperature was 31 ℃. Fingerprints of six batches of total saponins of the above ground part of P. polyphylla var. yunnanenis were determined, and the similarity was evaluated. The common peaks were assigned and identified according to the chromatographic behavior of each reference substance and the UV spectrum. Results:The three unknown peaks in the fingerprint were: pennogenin-3-O-α-L-rhamnopyranosyl（1→4）-[α-L-rhamnopyranosyl（1→4）]-β-D-glucopyranoside（cld01）,pennogenin-3-O-α-L-rhamnopyranosyl（1→4）-β-D-glucopyranoside（cld02）,diosgenin-3-O-α-L-rhamnopyranosyl（1→4）-[α-L-rhamnopyranosyl（1→4）]-β-D-glucopyranoside（cld03）. Compound cld02 was isolated from the plant for the first time, cld03 was isolated from the above ground part of the plant for the first time; The similarities of fingerprint of six batches of samples and reference fingerprints were all greater than 0.99,There were 7 mutual peaks identified in total. Conclusion:The HPLC fingerprint method is stable, reliable and repeatable, which can provide the basis for the quality control of the total saponins of the above ground part of P. polyphylla var. yunnanenis.更多还原