Gaweł Marta, Płodzik Martyna, Głowacki Rafał, Piechocka Justyna
Department of Environmental Chemistry, Faculty of Chemistry, University of Lodz, 163/165 Pomorska Str., 90-236 Łódź, Poland.
Doctoral School of Exact and Natural Sciences, University of Lodz, 12/16 Banacha Str., 90-237 Łódź, Poland.
Molecules. 2025 Jul 28;30(15):3152. doi: 10.3390/molecules30153152.
The article presents the first method based on high-performance liquid chromatography and ultraviolet detection (HPLC-UV) for the determination of timonacic (thioproline, 1,3-thiazolidine-4-carboxylic acid, tPro) in pharmaceutical tablets and face care products (creams, sera, foundations, suncreams). Sample preparation primarily involves solid-liquid extraction (SLE) of tPro with 0.2 mol/L phosphate buffer pH 6, derivatization with 0.25 mol/L 2-chloro-1-methylquinolinium tetrafluoroborate (CMQT), followed by polytetrafluoroethylene (PTFE) membrane filtration. The chromatographic separation of the stable UV-absorbing 2--quinolinium derivative is achieved within 14 min at 25 °C on a Zorbax SB-C18 (150 × 4.6 mm, 5 µm) column using gradient elution. The eluent consists of 0.1 mol/L trichloroacetic acid (TCA), pH 1.7, in a mixture with acetonitrile (ACN) delivered at a flow rate of 1 mL/min. The analyte is quantified by monitoring at 348 nm. The assay linearity was observed within 0.5-125 μmol/L. The limit of quantification (LOQ) was found to be 0.5 μmol/L. The accuracy ranged from 93.22% to 104.31% and 97.38% to 103.48%, while precision varied from 0.30% to 11.23% and 1.13% to 9.64% for intra- and inter-assay measurements, respectively. The method was successfully applied to commercially available on the Polish market pharmaceutical and cosmetic products.
本文介绍了基于高效液相色谱和紫外检测(HPLC-UV)的第一种方法,用于测定药片中的替莫那西(硫脯氨酸、1,3-噻唑烷-4-羧酸、tPro)以及面部护理产品(面霜、精华液、粉底、防晒霜)中的替莫那西。样品制备主要包括用0.2 mol/L pH 6的磷酸盐缓冲液对tPro进行固液萃取(SLE),用0.25 mol/L四氟硼酸2-氯-1-甲基喹啉鎓(CMQT)进行衍生化,然后进行聚四氟乙烯(PTFE)膜过滤。在25℃下,使用梯度洗脱,在Zorbax SB-C18(150×4.6 mm,5 µm)色谱柱上,14分钟内可实现稳定的紫外吸收2-喹啉鎓衍生物的色谱分离。洗脱液由0.1 mol/L三氯乙酸(TCA)、pH 1.7与乙腈(ACN)的混合物组成,流速为1 mL/min。通过在348 nm处监测对分析物进行定量。在0.5-125 μmol/L范围内观察到测定线性。定量限(LOQ)为0.5 μmol/L。准确度在93.22%至104.31%以及97.38%至103.48%之间,而批内和批间测量的精密度分别在0.30%至11.23%以及1.13%至9.64%之间。该方法已成功应用于波兰市场上的市售药品和化妆品。