建立了超高效液相色谱-三重四级杆线性离子阱质谱联用仪(ultra-performance liquid chromatography coupled with triple quadrupole linear ion trap mass spectrometer,UPLC-Q-Trap-MS)分析鱼肉游离氨基酸的方法,并结合化学计量学方...建立了超高效液相色谱-三重四级杆线性离子阱质谱联用仪(ultra-performance liquid chromatography coupled with triple quadrupole linear ion trap mass spectrometer,UPLC-Q-Trap-MS)分析鱼肉游离氨基酸的方法,并结合化学计量学方法研究不同大小虹鳟鱼肉中16种游离氨基酸的含量与该鱼肉滋味的相关性。采用Acquity UPLC BEH Amide(2.1 mm×100 mm,1.7μm)色谱柱,柱温35℃,以5 mmol/L甲酸铵-水(含0.1%体积分数甲酸)、5 mmol/L甲酸铵-乙腈(含0.1%体积分数甲酸)为流动相进行梯度洗脱,流速为0.3 mL/min,电喷雾离子源(正离子扫描),多反应监测模式检测;并结合滋味活度值及主成分分析探讨滋味轮廓差异。结果表明,所述分析条件下16种游离氨基酸分别在各自浓度范围内呈良好的线性关系,相关系数均大于0.99,平均加样回收率(n=6)为98.38%~103.57%,相对标准差为0.34%~2.89%;不同大小虹鳟鱼肉中各游离氨基酸含量及其滋味活度值具有显著差异(P<0.01),幼鱼肉呈现甜味、苦味特征,中鱼肉呈现鲜味、甜味和苦味特征,成鱼仅呈现出苦味特征。该研究为虹鳟鱼肉食品的品质评价提供参考。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
文摘建立了超高效液相色谱-三重四级杆线性离子阱质谱联用仪(ultra-performance liquid chromatography coupled with triple quadrupole linear ion trap mass spectrometer,UPLC-Q-Trap-MS)分析鱼肉游离氨基酸的方法,并结合化学计量学方法研究不同大小虹鳟鱼肉中16种游离氨基酸的含量与该鱼肉滋味的相关性。采用Acquity UPLC BEH Amide(2.1 mm×100 mm,1.7μm)色谱柱,柱温35℃,以5 mmol/L甲酸铵-水(含0.1%体积分数甲酸)、5 mmol/L甲酸铵-乙腈(含0.1%体积分数甲酸)为流动相进行梯度洗脱,流速为0.3 mL/min,电喷雾离子源(正离子扫描),多反应监测模式检测;并结合滋味活度值及主成分分析探讨滋味轮廓差异。结果表明,所述分析条件下16种游离氨基酸分别在各自浓度范围内呈良好的线性关系,相关系数均大于0.99,平均加样回收率(n=6)为98.38%~103.57%,相对标准差为0.34%~2.89%;不同大小虹鳟鱼肉中各游离氨基酸含量及其滋味活度值具有显著差异(P<0.01),幼鱼肉呈现甜味、苦味特征,中鱼肉呈现鲜味、甜味和苦味特征,成鱼仅呈现出苦味特征。该研究为虹鳟鱼肉食品的品质评价提供参考。
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.
