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基于高效液相色谱和紫外检测的通用方法测定药品和化妆品中的硫代脯氨酸

Versatile High-Performance Liquid Chromatography and Ultraviolet Detection-Based Method for the Determination of Thioproline in Pharmaceutical and Cosmetic Products.

作者信息

Gaweł Marta, Płodzik Martyna, Głowacki Rafał, Piechocka Justyna

机构信息

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.

出版信息

Molecules. 2025 Jul 28;30(15):3152. doi: 10.3390/molecules30153152.

Abstract

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.

摘要

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。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/4400/12348203/0339d8d12698/molecules-30-03152-g001.jpg

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