LC-MS/MS法测定血液中卡马西平及其代谢物

Objective 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. Con⁃ clusion 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. © 2023 Journal of Forensic Medicine. All rights reserved.

Detection of Carbamazepine and Its Metabolites in Blood Samples by LC-MS/MSCSCD