期刊
TALANTA
卷 158, 期 -, 页码 77-88出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.talanta.2016.05.036
关键词
Antiepileptic drugs; Online-SPE-LC-HRMS/MS; Therapeutic drug monitoring
资金
- National Basic Research Program of China (973 program) [2013CB911104, 2013CB911100]
- National Natural Science Foundation of China [21572116]
- Fundamental Research Funds for the Central Universities [20141081129]
- Tianjin Science and Technology Program [13JCYBJC24300, 13JCQNJC13100]
A simple and efficient bioanalytical method for simultaneous determination of phenobarbital (PB), phenytoin (PHT), carbamazepine (CBZ), and its active metabolite carbamazepine 10,11-epoxide (CBZE) in human plasma using online solid phase extraction (SPE)-liquid chromatography (LC) coupled with high resolution mass spectrum (HRMS) under targeted MS/MS (t-MS2) analysis mode has been developed. The procedure integrated an automated sample clean-up of human plasma by Oasis (R) HLB SPE cartridge, a separation by ZORBAX SB-C18 analysis column, and a quantification by Q-Exactive Hybrid Quadrupole-Orbitrap. The total running time was 13 min. The lower limit of quantification (LLOQ) of PB, PHT, CBZ, and CBZE were 0.008, 0.008, 0.0016 and 0.0016 mu g mL(-1) respectively and the linearities were in the range of 0.008-2.500, 0.008-2.500, 0.0016-0.500 and 0.0016-0.500 mu g mL(-1) respectively. The mean recovery was between 91.82% and 108.27% and the matrix effect was between 93.29% and 102.09%. The relative standard deviations of interday and intraday were less than 6.41%. The method has been successfully applied in therapeutic drug monitoring (TDM) of four Chinese epilepsy patients. This fully automated, simple, sensitive and reliable online-SPE-LC-HRMS/MS method serves well for TDM of PB, PHI; CBZ and CBZE at clinics for either single or combination treatment. (C) 2016 Elsevier B.V. All rights reserved.
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