Polak Beata, Kryska Adrianna, Jaglińska Kamila, Traczuk Adam, Barwinek Barbara
Department of Physical Chemistry, Medical University of Lublin, Chodźki 4a, 20-093, Lublin, Poland.
Independent Unit of Spectroscopy and Chemical Imaging, Medical University of Lublin, Chodźki 4a, 20-093, Lublin, Poland.
Sci Rep. 2025 Apr 28;15(1):14777. doi: 10.1038/s41598-025-99617-1.
The modification of non-polar silica gel plates by aqueous-organic solvent containing sodium dodecyl sulphate was investigated. The changes that occurred in the sorbent were examined using the Raman spectroscopy technique. The abovementioned technique was also involved in the investigation of carbamazepine-SDS complexes. The approach of applying the Raman spectroscopy into the investigation of the chromatographic behavior of SDS, carbamazepine and RP-18 W sorbent was presented for the first time. The effect of sodium dodecyl sulphate, SDS, concentration on the chosen drug used in neurodegenerative disorder (sulpiride, olanzapine, carbamazepine, trazodone, clomipramine, and pridinol) retention has been investigated. Such examination for these medicines has been presented for the first time for thin-layer chromatography system. Modified the mobile phase composition has resulted in the separation of the mixture containing all compounds. To confirm micellar forming, critical micelle concentration for SDS in the applied mobile phase was determined using two techniques, i.e., conductometric and spectrophotometric with azorubine as the indicator. The effect of surfactant on the solute zone shape by means of tailing and asymmetry factors has been determined. For four of the six investigated compounds, these factors have been close to 1.0. The separation efficiency measured by the height of the theoretical plate varies from 39 to 73 μm depending on the solute investigated. The method has been optimised regarding the quantitative analysis of investigated compounds, opening up new possibilities for drug analysis. In terms of the LOD values are in the range of 0.22 µg/spot to 1.67 µg/spot, whereas LOQ values are in the range of 0.66 µg/spot to 5.07 µg/spot for olanzapine and trazodone, respectively. Furthermore, the method was also applied for the quantitative analysis of the investigated compounds in pharmaceutical preparations. Such proceedings for RP-18 W TLC system containing SDS was shown for the first time. The new method has better or comparable concentration ranges regarding some of investigated compounds to those presented previously. Additionally, for the first time, a strategy involving various techniques (TLC chromatography supported by UV- and Raman spectroscopy and conductometry) for complex analysis of the separation system was presented, inspiring potential future research directions.
研究了用含十二烷基硫酸钠的水 - 有机溶剂对非极性硅胶板进行改性。使用拉曼光谱技术研究了吸附剂中发生的变化。上述技术还用于卡马西平 - 十二烷基硫酸钠复合物的研究。首次提出了将拉曼光谱应用于十二烷基硫酸钠、卡马西平和RP - 18 W吸附剂色谱行为研究的方法。研究了十二烷基硫酸钠(SDS)浓度对用于神经退行性疾病的选定药物(舒必利、奥氮平、卡马西平、曲唑酮、氯米帕明和普立地诺)保留的影响。这种针对这些药物的检测在薄层色谱系统中尚属首次。改变流动相组成实现了含所有化合物混合物的分离。为确认胶束形成,使用两种技术,即电导率法和以偶氮玉红为指示剂的分光光度法,测定了所用流动相中SDS的临界胶束浓度。通过拖尾因子和不对称因子确定了表面活性剂对溶质区形状的影响。对于六种被研究化合物中的四种,这些因子接近1.0。根据所研究的溶质,理论塔板高度测得的分离效率在39至73μm之间变化。该方法针对所研究化合物的定量分析进行了优化,为药物分析开辟了新的可能性。就检测限(LOD)值而言,奥氮平和曲唑酮分别在0.22μg/斑点至1.67μg/斑点范围内,而定量限(LOQ)值分别在0.66μg/斑点至5.07μg/斑点范围内。此外,该方法还用于药物制剂中所研究化合物的定量分析。这种含SDS的RP - 18 W TLC系统的操作尚属首次展示。新方法对于一些所研究化合物的浓度范围比先前报道的更好或相当。此外,首次提出了一种涉及多种技术(紫外和拉曼光谱以及电导率法支持的TLC色谱)用于分离系统复杂分析的策略,为未来潜在的研究方向提供了启发。