Novel Approach of Ultrasonic-assisted Ionic Liquid Dispersive Liquid-liquid Microextraction Coupled with LC-MS/MS to Determine Blood-harbored Carbamazepine

LÜ Chenxi, LU Xiaojun, LIANG Jiahao, XIE Wenkai, GUAN Qinglin, WEI Zhiwen, ZHANG Chao, DU Qiuxiang, YUN Keming, CUI Haiyan

Forensic Science and Technology ›› 2021, Vol. 46 ›› Issue (5) : 478-483. DOI: 10.16467/j.1008-3650.2021.0110
Research Articles

Novel Approach of Ultrasonic-assisted Ionic Liquid Dispersive Liquid-liquid Microextraction Coupled with LC-MS/MS to Determine Blood-harbored Carbamazepine

  • LÜ Chenxi, LU Xiaojun, LIANG Jiahao, XIE Wenkai, GUAN Qinglin, WEI Zhiwen, ZHANG Chao, DU Qiuxiang, YUN Keming, CUI Haiyan*
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Abstract

Objective To establish a novel approach of determining carbamazepine in whole blood through ultrasonic-assisted ionic liquid dispersive liquid-liquid microextraction coupled with HPLC-MS/MS (high performance liquid chromatography-tandem spectrometry). Methods With the selected 1-butyl-3-methylimidazolium hexafluoro-phosphate ([Bmim][PF6]) as extract solvent and 10,11-dihydrocarbamazepine as internal standard, the blank whole blood samples were added of carbamazepine, subjected to treating with ultrasound-assisted ionic liquid dispersive liquid-liquid microextraction. The harvested extraction was consecutively separated with ZORBAX Eclipse Plus C18 column that was flowed with mobile phases [A: 0.1% formic acid aqueous solution plus 10mM ammonium acetate and B: acetonitrile/methanol (v/v, 2:3)] running at the rate of 1mL/min. The detection was chosen under the mode of ESI+ plus MRM (multiple reaction monitoring). Results Carbamazepine was of linearity with it ranging from 8.00ng/mL to 300.00ng/mL in whole blood, with its correlation coefficient (R2) greater than 0.995, limit of detection (LOD) being 3.00ng/mL and limit of quantification (LOQ) 8.00ng/mL. The here-established approach was of extraction recovery greater than 80%, intra- and inter-day precision (relative standard deviation, RSD) being both less than 20%. Through verification of the here-established approach, a real forensic case was identified with carbamazepine of 2.71μg/mL in the victim's whole blood. Conclusions The here-developed approach is environmentally friendly, rapid, of good enrichment effect, high sensitivity and low consumption of organic solvent, capable of being used for determination of carbamazepine in biological samples from related forensic poisoning cases.

Key words

forensic toxicology / HPLC-MS/MS / ultrasonic-assisted ionic liquid dispersion liquid-liquid microextraction / carbamazepine / whole blood

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LÜ Chenxi, LU Xiaojun, LIANG Jiahao, XIE Wenkai, GUAN Qinglin, WEI Zhiwen, ZHANG Chao, DU Qiuxiang, YUN Keming, CUI Haiyan. Novel Approach of Ultrasonic-assisted Ionic Liquid Dispersive Liquid-liquid Microextraction Coupled with LC-MS/MS to Determine Blood-harbored Carbamazepine. Forensic Science and Technology. 2021, 46(5): 478-483 https://doi.org/10.16467/j.1008-3650.2021.0110

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