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天冬饮片与标准汤剂的质量评价方法探索 被引量:9
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作者 靳如娜 郝丽霞 +4 位作者 王涛 吴红华 代云桃 石守刚 黄正军 《中国实验方剂学杂志》 CAS CSCD 北大核心 2020年第17期111-118,共8页
目的:建立天冬饮片及其标准汤剂的质量评价方法。方法:制备10批天冬标准汤剂。采用高效液相色谱-蒸发光散射检测法(HPLC-ELSD),以乙腈-水为流动相梯度洗脱,建立天冬饮片、标准汤剂的指标成分含量测定方法以及天冬饮片的指纹图谱检测方... 目的:建立天冬饮片及其标准汤剂的质量评价方法。方法:制备10批天冬标准汤剂。采用高效液相色谱-蒸发光散射检测法(HPLC-ELSD),以乙腈-水为流动相梯度洗脱,建立天冬饮片、标准汤剂的指标成分含量测定方法以及天冬饮片的指纹图谱检测方法。采用UHPLC-LTQ-Orbitrap-MS/MS对指纹图谱中主要共有峰进行成分指认,以乙腈-0.1%甲酸水溶液为流动相,电喷雾离子源(ESI),正、负离子模式扫描,检测范围m/z 100~1400。结果:天冬饮片、标准汤剂中原薯蓣皂苷与原新薯蓣皂苷的总质量分数分别为0.41%~0.72%和0.33%~0.59%,这2个成分的转移率73.6%~98.3%。天冬标准汤剂的出膏率59.0%~73.0%,pH 4.9~5.6。天冬饮片的HPLC指纹图谱中呈现了10个共有峰,且均为皂苷类成分,包括原新薯蓣皂苷,原薯蓣皂苷,天冬皂苷甲及其同分异构体,甲基原薯蓣皂苷,asparagoside F,(25R)-26-O-β-D-葡萄吡喃糖基-呋甾-5,20-二烯-3β,26-二醇-3-O-[α-L-鼠李吡喃糖基(1→2)]-[β-D-葡萄吡喃糖基(1→4)-α-L-鼠李吡喃糖基(1→4)]-β-D-葡萄吡喃糖苷,26-O-β-D-葡萄吡喃糖基-呋甾-20(22)-烯-3β,26-二醇-3-O-[α-L-鼠李吡喃糖基(1→2)]-[α-L-鼠李吡喃糖基(1→4)]-β-D-葡萄吡喃糖苷,伪原薯蓣皂苷,aspacochioside C。结论:建立了天冬饮片及其标准汤剂的质量评价方法,且建立的方法稳定可行,可为含天冬制剂的质量评价及控制提供参考。 展开更多
关键词 天冬 饮片 标准汤剂 原薯蓣皂苷 原新薯蓣皂苷 指纹图谱 高效液相色谱-蒸发光散射检测法(HPLC-ELSD)
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Simultaneous Determination of Four Major Steroidal Saponins in seven species of Dioscorea L.By HPLC-ELSD 被引量:1
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《Chinese Herbal Medicines》 CAS 2011年第1期-,共5页
Objective To control the quality of the species in Dioscorea L.better.Methods An HPLC-ELSD method was developed for the first time to simultaneously determine four bioactive ingredients:dioscin,gracillin,protoneodiosc... Objective To control the quality of the species in Dioscorea L.better.Methods An HPLC-ELSD method was developed for the first time to simultaneously determine four bioactive ingredients:dioscin,gracillin,protoneodioscin,and protoneogracillin in 31 samples belonging to seven species of Dioscorea L.from different areas.The column was an Inertsil HILIC(250 mm×4.6 mm,5μm).The separation was carried out with a gradient program.The mobile phase was acetonitrile-water at a flow rate of 0.8 mL/min.Results The standard curve was rectilinear in the range of 0.464-12.97μg(r=0.9969)for dioscin,0.310-7.09μg(r=0.9953)for gracillin,0.469- 11.66μg(r=0.9970)for protoneodioscin,and 0.276-6.87μg(r=0.9992)for protoneogracillin.The recoveries of the markers were 98.1%,100.1%,97.2%,and 96.4%,respectively.The contents of the four components were quite different among the seven species of Dioscorea L.Conclusion The proposed HPLC-ELSD method is convenient,fast,accurate,and applicable for simultaneous analysis of multiple bioactive components of species in Dioscorea L.for quality control,which could facilitate discovering new natural resources of steroidal saponin. 展开更多
关键词 DIOSCIN Dioscorea L. gracillin HPLC-ELSD protoneodioscin protoneogracillin
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