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Method development for high performance liquid chromatography: novel organic modifiers and column packing conditions

机译：高效液相色谱的方法开发：新型有机改性剂和色谱柱填充条件

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Neutral eluents are proved to be applicable for the separations of organic acids and bases on reversed phase liquid chromatographic columns when an appropriate organic modifier is present. Straight chain alcohols, diols and amino alcohols are excellent candidates. The modifier can be incorporated into the eluent at low percentage or used to pre-treat the column. The function of the modifiers on the separations is to coat the surface of the stationary phase and make it less hydrophobic;Novel surfactant additives were used in mobile phases to improve the separations of various organic compounds. Compared with separations obtained without additives, shorter retention times and sharper peaks are obtained. The reason for the improvement appears to be a stronger solution-phase interaction between analyte and discrete additive molecules. The effect of additives is akin to gradient elution. Solvent strength and selectivity can be varied by controlling the type and concentration of the additive. Binding constants between solute and surfactant additives were calculated by relating capacity factor to surfactant concentration;An even greater reduction in k\u27 resulted from the use of binary additive systems, particularly those containing a cationic and an anionic surfactant. It is believed that an ion-pair is formed that is more effective in forming solution complexes with organic analytes than either additive alone. Other binary additive systems included mixtures of a neutral and a charged additive or a mixture of two anionic surfactant additives. A ternary mixture of additives was the most effective of all in modifying the chromatographic behavior of organic solutes in HPLC;Study of HPLC column packing conditions shows that the choice of slurry/packing solvent is critical to obtain a high efficiency column. Lower packing pressure yields columns with better performance when an appropriate solvent was chosen. A simple resin sizing method gives resin with narrower size range and thus better chromatographic columns.
机译：当存在适当的有机改性剂时，中性洗脱液被证明可用于在反相液相色谱柱上分离有机酸和碱。直链醇，二醇和氨基醇是极好的选择。改性剂可以低比例掺入洗脱液中或用于预处理色谱柱。改性剂对分离物的作用是覆盖固定相的表面并使其疏水性降低；在流动相中使用了新型表面活性剂添加剂，以改善各种有机化合物的分离度。与不添加添加剂的分离相比，保留时间更短，峰更锐利。改善的原因似乎是分析物和离散的添加剂分子之间更强的溶液相相互作用。添加剂的作用类似于梯度洗脱。溶剂强度和选择性可以通过控制添加剂的类型和浓度来改变。通过将容量因子与表面活性剂浓度相关联来计算溶质与表面活性剂添加剂之间的结合常数；使用二元添加剂体系（尤其是那些包含阳离子和阴离子表面活性剂的体系）导致k \ u27的更大降低。据信形成的离子对比单独使用任何一种添加剂更有效地与有机分析物形成溶液配合物。其他二元添加剂体系包括中性和带电添加剂的混合物或两种阴离子表面活性剂添加剂的混合物。添加剂的三元混合物在改变HPLC中有机溶质的色谱行为方面是最有效的； HPLC色谱柱填充条件的研究表明，选择浆料/填充溶剂对于获得高效色谱柱至关重要。当选择适当的溶剂时，较低的填充压力可使色谱柱的性能更好。一种简单的树脂上浆方法可以使树脂的粒径范围更窄，从而获得更好的色谱柱。

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    Li, Xue;

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  • 年度 1996
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  • 正文语种 en
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