Highly-sensitive quantification of carbamazepine and identification of its degradation and metabolism products in human liver by high performance liquid chromatography – High resolution mass spectrometry
A method for the qualitative and quantitative determination of carbamazepine in human post mortem liver tissues using high-performance liquid chromatography coupled with high-resolution mass spectrometry has been developed. Validation has been carried out and the main analytical characteristics of t...
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Elsevier
2025-06-01
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| Series: | Toxicology Reports |
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| Online Access: | http://www.sciencedirect.com/science/article/pii/S2214750025000411 |
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| author | Andrei Pirogov Ekaterina Shirokova Samvel Barsegyan Nikita Gandlevskiy Valeriya Akimova Alessandro Barge Aleksander Nosyrev |
| author_facet | Andrei Pirogov Ekaterina Shirokova Samvel Barsegyan Nikita Gandlevskiy Valeriya Akimova Alessandro Barge Aleksander Nosyrev |
| author_sort | Andrei Pirogov |
| collection | DOAJ |
| description | A method for the qualitative and quantitative determination of carbamazepine in human post mortem liver tissues using high-performance liquid chromatography coupled with high-resolution mass spectrometry has been developed. Validation has been carried out and the main analytical characteristics of the developed method have been determined. The limit of detection (LOD) is 1 ng/g, and the lower limit of quantification (LLOQ) is 5 ng/g. The range of working concentrations for the calibration curve is 5–2000 ng/g. When assessing analyte carryover, the analyte signal of the sample does not exceed 20 % of the signal at the LLOQ level. Degradation products of carbamazepine in model solutions were studied under the presence of hydrochloric acid, sodium hydroxide, and hydrogen peroxide oxidation. Twenty-two degradation products were identified. It was found that the most intensive degradation process of carbamazepine, resulting in various degradation products, is observed during its oxidation with an acidified solution of 3 % hydrogen peroxide at pH= 1–2. The stability of carbamazepine in liver tissues was studied during storage under ambient conditions over various periods. The maximum concentration decline is observed during the first week of storage (on average by 20 %), and then the concentration approximately halves over 8 weeks. Based on the analysis of forensic samples from human liver, 2 out of the 22 carbamazepine degradation products described in this study were detected. |
| format | Article |
| id | doaj-art-443c5dce832a495b979ff03adc62cc42 |
| institution | Kabale University |
| issn | 2214-7500 |
| language | English |
| publishDate | 2025-06-01 |
| publisher | Elsevier |
| record_format | Article |
| series | Toxicology Reports |
| spelling | doaj-art-443c5dce832a495b979ff03adc62cc422025-01-29T05:01:19ZengElsevierToxicology Reports2214-75002025-06-0114101923Highly-sensitive quantification of carbamazepine and identification of its degradation and metabolism products in human liver by high performance liquid chromatography – High resolution mass spectrometryAndrei Pirogov0Ekaterina Shirokova1Samvel Barsegyan2Nikita Gandlevskiy3Valeriya Akimova4Alessandro Barge5Aleksander Nosyrev6Department of chemistry, M.V. Lomonosov Moscow State University, Chair of Analytical Chemistry, Leninskiye gory str. 1/3, Moscow 119991, RussiaDepartment of chemistry, M.V. Lomonosov Moscow State University, Chair of Analytical Chemistry, Leninskiye gory str. 1/3, Moscow 119991, RussiaFederal State Budgetary Institution «Russian Centre of Forensic Medical Expertise» of the Ministry of Health of the Russian Federation, Polikarpov str, 12/13, Moscow 125284, RussiaDepartment of chemistry, M.V. Lomonosov Moscow State University, Chair of Analytical Chemistry, Leninskiye gory str. 1/3, Moscow 119991, Russia; Department of Drug Science and Technology, Turin University, via P. Giuria 9, Turin 10125, Italy; Corresponding author at: Department of chemistry, M.V. Lomonosov Moscow State University, Chair of Analytical Chemistry, Leninskiye gory str. 1/3, Moscow 119991, Russia.Federal State Budgetary Institution «Russian Centre of Forensic Medical Expertise» of the Ministry of Health of the Russian Federation, Polikarpov str, 12/13, Moscow 125284, RussiaDepartment of Drug Science and Technology, Turin University, via P. Giuria 9, Turin 10125, ItalyFSAEI of Higher Education I.M. Sechenov First Moscow State Medical University (Sechenov University), Trubetskaya str, 8/2, Moscow 119048, RussiaA method for the qualitative and quantitative determination of carbamazepine in human post mortem liver tissues using high-performance liquid chromatography coupled with high-resolution mass spectrometry has been developed. Validation has been carried out and the main analytical characteristics of the developed method have been determined. The limit of detection (LOD) is 1 ng/g, and the lower limit of quantification (LLOQ) is 5 ng/g. The range of working concentrations for the calibration curve is 5–2000 ng/g. When assessing analyte carryover, the analyte signal of the sample does not exceed 20 % of the signal at the LLOQ level. Degradation products of carbamazepine in model solutions were studied under the presence of hydrochloric acid, sodium hydroxide, and hydrogen peroxide oxidation. Twenty-two degradation products were identified. It was found that the most intensive degradation process of carbamazepine, resulting in various degradation products, is observed during its oxidation with an acidified solution of 3 % hydrogen peroxide at pH= 1–2. The stability of carbamazepine in liver tissues was studied during storage under ambient conditions over various periods. The maximum concentration decline is observed during the first week of storage (on average by 20 %), and then the concentration approximately halves over 8 weeks. Based on the analysis of forensic samples from human liver, 2 out of the 22 carbamazepine degradation products described in this study were detected.http://www.sciencedirect.com/science/article/pii/S2214750025000411CarbamazepineLiver metabolismHPLC-HRMS |
| spellingShingle | Andrei Pirogov Ekaterina Shirokova Samvel Barsegyan Nikita Gandlevskiy Valeriya Akimova Alessandro Barge Aleksander Nosyrev Highly-sensitive quantification of carbamazepine and identification of its degradation and metabolism products in human liver by high performance liquid chromatography – High resolution mass spectrometry Toxicology Reports Carbamazepine Liver metabolism HPLC-HRMS |
| title | Highly-sensitive quantification of carbamazepine and identification of its degradation and metabolism products in human liver by high performance liquid chromatography – High resolution mass spectrometry |
| title_full | Highly-sensitive quantification of carbamazepine and identification of its degradation and metabolism products in human liver by high performance liquid chromatography – High resolution mass spectrometry |
| title_fullStr | Highly-sensitive quantification of carbamazepine and identification of its degradation and metabolism products in human liver by high performance liquid chromatography – High resolution mass spectrometry |
| title_full_unstemmed | Highly-sensitive quantification of carbamazepine and identification of its degradation and metabolism products in human liver by high performance liquid chromatography – High resolution mass spectrometry |
| title_short | Highly-sensitive quantification of carbamazepine and identification of its degradation and metabolism products in human liver by high performance liquid chromatography – High resolution mass spectrometry |
| title_sort | highly sensitive quantification of carbamazepine and identification of its degradation and metabolism products in human liver by high performance liquid chromatography high resolution mass spectrometry |
| topic | Carbamazepine Liver metabolism HPLC-HRMS |
| url | http://www.sciencedirect.com/science/article/pii/S2214750025000411 |
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