| 在线超临界色谱联用接口装置的研制与应用 |
| 点此下载全文 |
|
| 基金项目:辽宁省教育厅项目（L2015258） |
|
| 中文摘要:建立了动态和静态接口装置，使其能在线联用超临界色谱确定蒽在超临界二氧化碳中的溶解度及溶解平衡过程。静态接口由2个高压阀组成，动态接口由1个高压阀和1个齿轮泵组成。采用静态法测定蒽在超临界二氧化碳中的溶解度，以考察温度和压力对溶解度的影响。实验结果表明，在40~60 ℃和10~275 MPa条件下，自行研制的在线超临界色谱联用体系具有较高的稳定性和较好的重现性，溶解度的相对标准偏差（RSD）为04%~24%，准确性为950%~977%。采用Méndez-Santiago Teja（MST）模型公式对实验数值关联计算，确定了蒽的溶解度与二氧化碳密度的准线性函数变化关系，计算数值与实验结果之间的相对平均绝对值偏差（AARD）为323和1468。搭建的接口装置亦能够完成超临界流体技术与常规光谱、质谱分析仪器的在线联用分析，在药物合成与分析、过程分析技术（PAT）等领域具有较好的应用潜力。 |
| 中文关键词:在线超临界色谱 接口 溶解度 二氧化碳 |
| |
| Development and Application of Interface Device for Online Supercritical Fluid Chromatography |
|
|
| Abstract:Two interface devices for online supercritical fluid chromatography（SFC）were developed for the determination of solubility of anthracene in supercritical carbon dioxide and its dissolving equilibrium according to the static and dynamic operating modes.The static interface was consisted of two high pressure valves，and the dynamic interface was composed of one high pressure valve and one gear pump.The gear pump built into the dynamic interface maintained a constant flow of supercritical fluid carbon dioxide solution from the solubility vessel through the interface sample injection valve in a return flow circuit.The solubility of anthracene in supercritical carbon dioxide was measured by static method，the impacts of temperature and pressure on solubility were investigated，and the obtained solubility data were correlatedly calculated according to the density based on model of Méndez-Santiago Teja（MST）.A series of progressively more concentrated anthracene/carbon dioxide solutions were separately prepared by increasing the pressure in controlled steps.Solubility of anthracene was measured at 40，50 and 60 ℃ in the pressure range of 100-275 MPa using 25 MPa steps.The experimental results demonstrated that good stability and reproducibility for the self-developed equipment were acquired with RSD value range of 04%-24% and experimental accuracy of 950%-977%.All sets of experimental solubility data were correlated according to the density based MST model，the calculated average absolute relative deviation（AARD）values were 323 and 1468，respectively.The developed interface devices could become a bridge for the combination of conventional analytical equipments such as FT-IR/UV/mass spectrometry with supercritical fluid technique in applications of online monitoring pharmaceutical compound synthesis and analysis，process analysis technique（PAT）. |
| Key Words:online supercritical fluid chromatography interface solubility carbon dioxide |
| 引用本文：刘瑜，严志强，郭威，李犇.在线超临界色谱联用接口装置的研制与应用[J].分析测试学报,2018,37(8):894-899. |
| 摘要点击次数: 1639 |
| 全文下载次数: 828 |
| 查看全文 下载PDF阅读器 |
|
|
