Determination of Anthelmintic Pharmaceuticals in Wastewater by Solid-Phase Extraction and Thin-Layer Chromatography
| Autor: | Tatjana Gazivoda Kraljević, Jasna Mrđa, Dragana Mutavdžić Pavlović, Romana Pavić |
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| Rok vydání: | 2019 |
| Předmět: |
Detection limit
Benzimidazole Chromatography 010405 organic chemistry Chemistry Silica gel 010401 analytical chemistry Clinical Biochemistry Extraction (chemistry) anthelmintics thin-layer chromatography NMR spectroscopy solid-phase extraction production wastewater 01 natural sciences Biochemistry Pyrantel Pamoate Thin-layer chromatography 0104 chemical sciences Analytical Chemistry chemistry.chemical_compound medicine Anthelmintic Solid phase extraction medicine.drug |
| Zdroj: | JPC - Journal of Planar Chromatography - Modern TLC. 32:421-429 |
| ISSN: | 1789-0993 0933-4173 |
| DOI: | 10.1556/1006.2019.32.5.10 |
| Popis: | The presented study describes the development, optimization, and validation of a method for the determination of four structurally different anthelmintics (benzimidazole, diphenyl sulfide, imidazothiazole, hexahydropyrazine, and tetrahydropyrimidine) in water samples. The studied compounds were albendazole, febantel, levamisole, praziquantel, and pyrantel pamoate. The method involves solid-phase extraction and preconcentration of the anthelmintics, separation by thin-layer chromatography (TLC), and quantification by videodensitometry. TLC and preparative TLC separation was performed on silica gel 60 F254 plates with chloroform—methanol—formic acid as the mobile phase. Spots were detected and quantified at λ = 254 nm by videodensitometry. The method provides a linear response over a concentration range of 200–1500 μg L-1, depending on the anthelmintic with a correlation coefficient of 0.9888 in most cases, except for albendazole (0.9634) and pamoic acid (0.9654) as a secondary component of pyrantel pamoate. Also, the method has revealed limits of detection (100–300 μg L-1), good precision (intra- and inter-day) with a relative standard deviation below 13%, and recoveries above 95% for all investigated pharmaceuticals. The developed method has been successfully applied to the analysis of anthelmintics in production wastewater samples obtained from the local pharmaceutical industry. In order to determine the structures of two compounds detected by TLC of pyrantel pamoate, the spots were separated by preparative TLC, and the structures of the isolated samples were analyzed using 1H and 13C nuclear magnetic resonance (NMR) spectroscopy. |
| Databáze: | OpenAIRE |
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