Detection of Carbamazepine and Its Metabolites in Blood Samples by LC-MS/MS.
10.12116/j.issn.1004-5619.2021.310901
- Author:
Hai-Yan CUI
1
;
Chen-Xi LÜ
1
;
Yan-Hua SHI
1
;
Ni YUAN
2
;
Jia-Hao LIANG
1
;
Quan AN
2
;
Zhong-Yuan GUO
1
;
Ke-Ming YUN
1
Author Information
1. School of Forensic Medicine, Shanxi Medical University, Jinzhong 030600, Shanxi Province, China.
2. China Institute for Radiation Protection, Taiyuan 030006, China.
- Publication Type:Journal Article
- Keywords:
10,11-dihydro-10,11-epoxycarbamazepine;
10,11-dihydro-10-hydroxycarbamazepine;
LC-MS/MS;
carbamazepine;
forensic toxicological analysis;
metabolites
- MeSH:
Chromatography, Liquid/methods*;
Tandem Mass Spectrometry;
Methanol;
Carbamazepine/analysis*;
Benzodiazepines/analysis*;
Solvents;
Chromatography, High Pressure Liquid;
Solid Phase Extraction
- From:
Journal of Forensic Medicine
2023;39(1):34-39
- CountryChina
- Language:English
-
Abstract:
OBJECTIVES:To establish a method for the detection of carbamazepine and its metabolites 10,11-dihydro-10,11-epoxycarbamazepine and 10,11-dihydro-10-hydroxycarbamazepine in blood samples by liquid chromatography-tandem mass spectrometry (LC-MS/MS).
METHODS:The blood samples were treated with 1-butyl-3-methylimidazolium hexafluorophosphate as an extraction solvent. The samples were extracted by ultrasound-assisted extraction and separated by ZORBAX Eclipse Plus C18, 95Å column. The mobile phase A aqueous solution containing 0.1% formic acid and 10 mmol/L ammonium acetate, and mobile phase B mixed organic solvent containing acetonitrile/methanol (Vacetonitrile∶Vmethanol=2∶3) were used for gradient elution at the flow rate of 1.00 mL/min. An electrospray ion source in positive mode was used for detection in the multiple reaction monitoring.
RESULTS:The linearities of carbamazepine and its metabolites 10,11-dihydro-10,11-epoxycarbamazepine and 10,11-dihydro-10-hydroxycarbamazepine in blood samples were good within the corresponding range, with correlation coefficients (r) greater than 0.995 6. The limits of detection were 3.00, 0.40 and 1.30 ng/mL, respectively. The limit of quantitation were 8.00, 1.00 and 5.00 ng/mL, respectively. The extraction recoveries ranged from 76.00% to 106.44%. The relative standard deviations of the intra-day and inter-day precisions were less than 16%. Carbamazepine and its main metabolite 10,11-dihydro-10,11-epoxycarbamazepine were detected in blood samples of death cases with a mass concentration of 2.71 μg/mL and 252.14 ng/mL, respectively.
CONCLUSIONS:This method has high sensitivity and good selectivity, which is suitable for the detection of carbamazepine and its metabolites in blood samples, and can be used for carbamazepine-related forensic identifications.
