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Adsorption mechanism of triterpenoid saponins in reversed-phase liquid chromatography and hydrophilic interaction liquid chromatography: Mogroside V as test substance.
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2020-03-06 , DOI: 10.1016/j.chroma.2020.461010
Qing Fu 1 , Lin Ni 1 , Dasen Jiang 1 , Yanxiong Ke 1 , Yu Jin 1
Affiliation  

In this paper, adsorption mechanism of triterpenoid saponins in reversed-phase liquid chromatography (RPLC) and hydrophilic interaction liquid chromatography (HILIC) was proposed based on the study of the retention behavior of mogroside V as test substance. The change of peak shape of mogroside V and its influencing factors was first investigated. As the increase of sample loading, a tailing peak of mogroside V was observed in MeOHH2O of both two modes. It was the fronting peak in ACNH2O of HILIC while there was a transition from fronting peak to tailing peak in ACNH2O of RPLC that was largely affected by column temperature and ACN concentration. The adsorption isotherm of mogroside V in ACNH2O of RPLC was fitted by Moreau model, where a monolayer adsorption with large inter-molecular interaction was formed on the C18 surface. While in ACNH2O of HILIC, the adsorption of mogroside V was in accordance with BET model, showing multilayer adsorption behavior. In MeOHH2O of both HILIC and RPLC, there was always monolayer adsorption, which was fitted by Langmuir model. At last, by choosing the suitable chromatographic mode, controlling the key factors such as the solvent concentration and column temperature, and predicting the broadening trend of peak, three methods were screened out, namely, C18 column with 22% ACN (30 °C), Click XIon column with 90% MeOH or 70% ACN, to get mogroside V of purity greater than 98% from Siraitia grosvenorii extract. Among them, the RPLC method of 22% ACN that showed the highest loading sample per hour (1.92%) and the lowest solvent consumption emerged as the best approach.

中文翻译:

三萜皂苷在反相液相色谱和亲水作用液相色谱中的吸附机理:以罗汉果苷V为测试物质。

本文以罗汉果苷V为测试物质的保留行为为研究对象,提出了三萜皂苷在反相液相色谱(RPLC)和亲水相互作用液相色谱(HILIC)中的吸附机理。首先研究了罗汉果甙V峰形的变化及其影响因素。随着样品上样量的增加,两种模式的MeOHH2O中都观察到罗汉果苷V的拖尾峰。它是HILIC ACNH2O的前峰,而RPLC ACNH2O中从前峰到尾峰的过渡很大程度上受柱温和ACN浓度的影响。罗汉果苷V在RPLC的ACNH2O中的吸附等温线采用Moreau模型拟合,其中在C18表面形成了分子间相互作用大的单层吸附。而在HILIC的ACNH2O中,罗汉果苷V的吸附符合BET模型,显示出多层吸附行为。在HILIC和RPLC的MeOHH2O中,总是存在单层吸附,这是由Langmuir模型拟合的。最后,通过选择合适的色谱模式,控制溶剂浓度和色谱柱温度等关键因素,并预测峰的展宽趋势,筛选出三种方法,即使用22%ACN(30°C)的C18色谱柱在含有90%MeOH或70%ACN的XIon柱上单击,从罗汉果提取物中获得纯度高于98%的罗汉果苷V。其中,最好的方法是采用22%ACN的RPLC方法,显示每小时最高的上样量(1.92%)和最低的溶剂消耗量。显示多层吸附行为。在HILIC和RPLC的MeOHH2O中,总是存在单层吸附,这是由Langmuir模型拟合的。最后,通过选择合适的色谱模式,控制溶剂浓度和色谱柱温度等关键因素,并预测峰的展宽趋势,筛选出三种方法,即使用22%ACN(30°C)的C18色谱柱在含有90%MeOH或70%ACN的XIon柱上单击,从罗汉果提取物中获得纯度高于98%的罗汉果苷V。其中,最好的方法是采用22%ACN的RPLC方法,显示每小时最高的上样量(1.92%)和最低的溶剂消耗量。显示多层吸附行为。在HILIC和RPLC的MeOHH2O中,总是存在单层吸附,这是由Langmuir模型拟合的。最后,通过选择合适的色谱模式,控制溶剂浓度和色谱柱温度等关键因素,并预测峰的展宽趋势,筛选出三种方法,即使用22%ACN(30°C)的C18色谱柱在含有90%MeOH或70%ACN的XIon柱上单击,从罗汉果提取物中获得纯度高于98%的罗汉果苷V。其中,最好的方法是采用22%ACN的RPLC方法,显示每小时最高的上样量(1.92%)和最低的溶剂消耗量。通过选择合适的色谱模式,控制溶剂浓度和柱温等关键因素,并预测峰的扩展趋势,筛选出三种方法,即22%ACN(30°C)的C18色谱柱,单击XIon用90%MeOH或70%ACN色谱柱从罗汉果提取物中获得纯度高于98%的罗汉果苷V。其中,最好的方法是采用22%ACN的RPLC方法,显示每小时最高的上样量(1.92%)和最低的溶剂消耗量。通过选择合适的色谱模式,控制溶剂浓度和柱温等关键因素,并预测峰的扩展趋势,筛选出三种方法,即22%ACN(30°C)的C18色谱柱,单击XIon用90%MeOH或70%ACN色谱柱从罗汉果提取物中获得纯度高于98%的罗汉果苷V。其中,最好的方法是采用22%ACN的RPLC方法,显示每小时最高的上样量(1.92%)和最低的溶剂消耗量。从罗汉果提取物中获得纯度大于98%的罗汉果苷V。其中,最好的方法是采用22%ACN的RPLC方法,显示每小时最高的上样量(1.92%)和最低的溶剂消耗量。从罗汉果提取物中获得纯度大于98%的罗汉果苷V。其中,最好的方法是采用22%ACN的RPLC方法,显示每小时最高的上样量(1.92%)和最低的溶剂消耗量。
更新日期:2020-03-06
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