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

Andrei Pirogov; Ekaterina Shirokova; Samvel Barsegyan; Nikita Gandlevskiy; Valeriya Akimova; Alessandro Barge; Aleksander Nosyrev

Toxicology Reports (Jun 2025)

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

Andrei Pirogov,
Ekaterina Shirokova,
Samvel Barsegyan,
Nikita Gandlevskiy,
Valeriya Akimova,
Alessandro Barge,
Aleksander Nosyrev

Affiliations

Andrei Pirogov: Department of chemistry, M.V. Lomonosov Moscow State University, Chair of Analytical Chemistry, Leninskiye gory str. 1/3, Moscow 119991, Russia
Ekaterina Shirokova: Department of chemistry, M.V. Lomonosov Moscow State University, Chair of Analytical Chemistry, Leninskiye gory str. 1/3, Moscow 119991, Russia
Samvel Barsegyan: 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, Russia
Nikita Gandlevskiy: Department 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.
Valeriya Akimova: 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, Russia
Alessandro Barge: Department of Drug Science and Technology, Turin University, via P. Giuria 9, Turin 10125, Italy
Aleksander Nosyrev: FSAEI of Higher Education I.M. Sechenov First Moscow State Medical University (Sechenov University), Trubetskaya str, 8/2, Moscow 119048, Russia

Journal volume & issue: Vol. 14
p. 101923

Abstract

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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.

Published in Toxicology Reports

ISSN: 2214-7500 (Online)
Publisher: Elsevier
Country of publisher: Ireland
LCC subjects: Medicine: Public aspects of medicine: Toxicology. Poisons
Website: http://www.journals.elsevier.com/toxicology-reports/

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