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首页> 外文期刊>Journal of Pharmaceutical and Biomedical Analysis: An International Journal on All Drug-Related Topics in Pharmaceutical, Biomedical and Clinical Analysis >Fast separations on monolithic silica columns: method transfer, robustness and column ageing for some case studies.
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Fast separations on monolithic silica columns: method transfer, robustness and column ageing for some case studies.

机译:在整体硅胶色谱柱上快速分离:方法转移,耐用性和某些案例研究中的色谱柱老化。

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摘要

Six separation methods, developed on conventional silica high performance liquid chromatography (HPLC) columns were transferred to monolithic silica columns of 5 and 10 cm length. The transferred methods include the separation of an alkylbenzene mixture, the separations of drugs from their impurities (nimesulide, tetracycline, phenoxymethylpenicillin and erythromycin) and the separation of a green tea extract. The transfer of the first three methods was successful while for the latter three it was not. Increasing the flow rate up to 9 ml/min (where possible) inversely decreased the analysis time of the successfully transferred methods to 48 s (alkylbenzene mixture) 1.8 min (nimesulide mixture) and 3 min (tetracycline mixture) while still reasonable well separated peaks were obtained. The robustness and repeatability of the transferred and accelerated separations was found to be acceptable. Despite the use of flow rates up to 9 ml/min and frequent mobile phase changes with pH values varying from 3.5 to 7, the column performance was found to be rather constant and the column ageing to be minimal.
机译:在常规硅胶高效液相色谱(HPLC)色谱柱上开发的六种分离方法被转移到5和10 cm长的整体硅胶柱上。转移的方法包括分离烷基苯混合物,从药物杂质(尼美舒利,四环素,苯氧甲基青霉素和红霉素)中分离药物,以及分离绿茶提取物。前三种方法的转移是成功的,而后三种方法则不是。将流速提高到9 ml / min(在可能的情况下),将成功转移方法的分析时间反过来减少到48 s(烷基苯混合物),1.8 min(尼美舒利混合物)和3 min(四环素混合物),同时仍能得到合理分离的峰获得了。发现转移和加速分离的稳健性和可重复性是可以接受的。尽管使用的流速高达9 ml / min,并且流动相频繁变化,pH值在3.5到7之间变化,但发现色谱柱性能相当稳定,并且色谱柱老化最小。

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