目的建立骨刺胶囊（昆布、骨碎补、白芍、党参等）指纹图谱,并结合质谱信息鉴定特征峰的化学结构信息。方法骨刺胶囊75%甲醇提取液的分析采用Phenomenex Luna C18柱（4.6 mm×250 mm,5μm）;流动相为乙腈-20 mmol/L甲酸铵水溶液体系...目的建立骨刺胶囊（昆布、骨碎补、白芍、党参等）指纹图谱,并结合质谱信息鉴定特征峰的化学结构信息。方法骨刺胶囊75%甲醇提取液的分析采用Phenomenex Luna C18柱（4.6 mm×250 mm,5μm）;流动相为乙腈-20 mmol/L甲酸铵水溶液体系;体积流量为1.0 m L/min,梯度洗脱;检测波长为254 nm。采用飞行时间质谱（TOFMS）结合离子阱多级质谱（Ion-trap/MSn）,鉴定骨刺胶囊指纹图谱中特征峰的结构,正、负两种离子模式扫描。结果骨刺胶囊HPLC-MS指认21个共有峰,表征昆布、白芍、杜仲、党参、马钱子、鸡血藤、骨碎补、延胡索和桂枝等9味药材的特征成分。以绿原酸为参照物峰,12批样品的相似度在0.821~0.945之间。结论该方法显示,骨刺胶囊主要化学成分相似,质量较稳定。展开更多
Fenugreek, a traditional Chinese medical plant, has been widely used as food ingredients because of its out- standing medicinal qualities. The hypoglycemic activity of fenugreek is one of its important pharmacological...Fenugreek, a traditional Chinese medical plant, has been widely used as food ingredients because of its out- standing medicinal qualities. The hypoglycemic activity of fenugreek is one of its important pharmacological properties. Both of saponin and flavonoid components have the hypoglycemic activity and their contents in fenugreek are 4%--8% and 1% ---2%, respectively. This paper focused on these two types of components to carry out purification research and chemical analysis. The heating reflux extraction method and macroporous resin purification method were designed to prepare the saponins and the flavonoids components from defatted fenugreek seeds. Petroleum ether ultrasonic skim and 70% ethanol refluxing were used for the extraction of saponins and flavonoid from fenugreek. The column of DM130 macroporous resin and D101 macroporous resin were respectively used to prepare fenugreek saponin and flavonoid components, and the total contents of them were 78.56% and 62.28%, respectively. The saponin and flavonoids were subsequently analyzed by an ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry（UPLC-Q-TOF-MS） along with an ultra-performance liquid chromatography and ion-trap tandem mass spectrometry（UPLC-IT-MS＂）. As a result, 57 saponins and 19 flavonoid compounds were characterized. The obtained results will provide a theory basis for further research on fenugreek, as well as research and development of hypogly- cemic new drugs.展开更多
文摘目的建立骨刺胶囊（昆布、骨碎补、白芍、党参等）指纹图谱,并结合质谱信息鉴定特征峰的化学结构信息。方法骨刺胶囊75%甲醇提取液的分析采用Phenomenex Luna C18柱（4.6 mm×250 mm,5μm）;流动相为乙腈-20 mmol/L甲酸铵水溶液体系;体积流量为1.0 m L/min,梯度洗脱;检测波长为254 nm。采用飞行时间质谱（TOFMS）结合离子阱多级质谱（Ion-trap/MSn）,鉴定骨刺胶囊指纹图谱中特征峰的结构,正、负两种离子模式扫描。结果骨刺胶囊HPLC-MS指认21个共有峰,表征昆布、白芍、杜仲、党参、马钱子、鸡血藤、骨碎补、延胡索和桂枝等9味药材的特征成分。以绿原酸为参照物峰,12批样品的相似度在0.821~0.945之间。结论该方法显示,骨刺胶囊主要化学成分相似,质量较稳定。
文摘Fenugreek, a traditional Chinese medical plant, has been widely used as food ingredients because of its out- standing medicinal qualities. The hypoglycemic activity of fenugreek is one of its important pharmacological properties. Both of saponin and flavonoid components have the hypoglycemic activity and their contents in fenugreek are 4%--8% and 1% ---2%, respectively. This paper focused on these two types of components to carry out purification research and chemical analysis. The heating reflux extraction method and macroporous resin purification method were designed to prepare the saponins and the flavonoids components from defatted fenugreek seeds. Petroleum ether ultrasonic skim and 70% ethanol refluxing were used for the extraction of saponins and flavonoid from fenugreek. The column of DM130 macroporous resin and D101 macroporous resin were respectively used to prepare fenugreek saponin and flavonoid components, and the total contents of them were 78.56% and 62.28%, respectively. The saponin and flavonoids were subsequently analyzed by an ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry（UPLC-Q-TOF-MS） along with an ultra-performance liquid chromatography and ion-trap tandem mass spectrometry（UPLC-IT-MS＂）. As a result, 57 saponins and 19 flavonoid compounds were characterized. The obtained results will provide a theory basis for further research on fenugreek, as well as research and development of hypogly- cemic new drugs.
