Generic placeholder image

Current Psychopharmacology

Editor-in-Chief

ISSN (Print): 2211-5560
ISSN (Online): 2211-5579

Research Article

Method Validation for the Determination of Carbamazepine in Spiked-saliva Using HPLC-UV for Therapeutic Drug Monitoring Application

Author(s): Ari Wibowo, Vitarani D.A. Ningrum* and Rahma N. Ilhamy

Volume 9, Issue 3, 2020

Page: [234 - 241] Pages: 8

DOI: 10.2174/2211556009999200727191226

open access plus

Abstract

Background: Carbamazepine has been used in the treatment of bipolar disorder, both in acute mania and maintenance therapy, particularly in developing countries. Not only its interaction with various drugs and auto-inducer nature, but the narrow therapeutic range of carbamazepine also makes monitoring necessary to guarantee the adequacy of its safety and therapeutic concentration. To date, the most common biological specimen used for therapeutic drug monitoring (TDM) purposes is still plasma, but saliva can become an alternative biological matrix since its level in saliva strongly correlates with carbamazepine plasma concentration.

Objective: This study validated the bioanalytical method parameters used for carbamazepine in spiked-saliva in accordance with the Food and Drug Administration (FDA) criteria in the Guidance for Industry Bioanalytical Method Validation.

Methods: HPLC-UV detector was employed at 285 nm λ with methanol: water: glacial acetic acid (65:34:1) as the mobile phase and C8 as the stationary phase (4.6x150 mm; 5 μm).

Results: The linearity test in a range of 0.0 - 5 μg/mL carbamazepine concentration resulted in a correlation coefficient of 0.999 with 0.20 μg/mL LoD, 0.30 μg/mL LLoQ, and 0.61 μg/mL LoQ. The coefficient of variation and %diff in the selectivity, accuracy, and precision parameters remained below 20%, indicating fulfillment of the criteria for a bioanalytical method, while the average % recovery was more than 90%.

Conclusion: The currently-developed bioanalytical method has fulfilled the stipulated validation criteria to be used for determining carbamazepine concentration in spiked-saliva as an alternative method for relative bioequivalence studies or TDM application in a clinical setting.

Keywords: Carbamazepine, high-performance liquid chromatography, method validation, spiked-saliva, therapeutic drug monitoring, ultraviolet detector.

Graphical Abstract
[1]
Chen C-H, Lin S-K. Carbamazepine treatment of bipolar disorder: a retrospective evaluation of naturalistic long-term outcomes. BMC Psychiatry 2012; 12: 47.
[http://dx.doi.org/10.1186/1471-244X-12-47 ] [PMID: 22620289]
[2]
Wiffen PJ, Derry S, Moore RA, Kalso EA. Carbamazepine for chronic neuropathic pain and fibromyalgia in adults. Cochrane Database Syst Rev 2014; 2014; (4): CD005451.
[PMID: 24719027] [http://dx.doi.org/10.1002/14651858.CD005451.pub3]
[3]
Patsalos PN, Berry DJ, Bourgeois BFD, et al. Antiepileptic drugs--best practice guidelines for therapeutic drug monitoring: a position paper by the subcommission on therapeutic drug monitoring, ILAE Commission on Therapeutic Strategies. Epilepsia 2008; 49(7): 1239-76.
[http://dx.doi.org/10.1111/j.1528-1167.2008.01561.x ] [PMID: 18397299]
[4]
Shakya G, Malla S, Shakya KN, Shrestha R. Therapeutic drug monitoring of antiepileptic drugs. JNMA J Nepal Med Assoc 2008; 47(171): 94-7.
[http://dx.doi.org/10.31729/jnma.294 ] [PMID: 19079370]
[5]
Nilsson L, Bergman U, Diwan V, Farahmand BY, Persson P-G, Tomson T. Antiepileptic drug therapy and its management in sudden unexpected death in epilepsy: a case-control study. Epilepsia 2001; 42(5): 667-73.
[http://dx.doi.org/10.1046/j.1528-1157.2001.22000.x ] [PMID: 11380576]
[6]
Aurlien D, Gjerstad L, Taubøll E. The role of antiepileptic drugs in sudden unexpected death in epilepsy. Seizure 2016; 43: 56-60.
[http://dx.doi.org/10.1016/j.seizure.2016.11.005 ] [PMID: 27886630]
[7]
Hughes JR. A review of sudden unexpected death in epilepsy: prediction of patients at risk. Epilepsy Behav 2009; 14(2): 280-7.
[http://dx.doi.org/10.1016/j.yebeh.2008.12.004 ] [PMID: 19130900]
[8]
Al-Hassany L, Kloosterboer SM, Dierckx B, Koch BC. Assessing methods of measuring medication adherence in chronically ill children-a narrative review. Patient Prefer Adherence 2019; 13: 1175-89.
[http://dx.doi.org/10.2147/PPA.S200058 ] [PMID: 31413546]
[9]
Kilbourne AM, Post EP, Bauer MS, et al. Therapeutic drug and cardiovascular disease risk monitoring in patients with bipolar disorder. J Affect Disord 2007; 102(1-3): 145-51.
[http://dx.doi.org/10.1016/j.jad.2007.01.006 ] [PMID: 17276514]
[10]
Mercolini L, Saracino MA, Protti M. Current advances in biosampling for therapeutic drug monitoring of psychiatric CNS drugs. Bioanalysis 2015; 7(15): 1925-42.
[http://dx.doi.org/10.4155/bio.15.123 ] [PMID: 26295991]
[11]
Patsalos PN, Berry DJ. Therapeutic drug monitoring of antiepileptic drugs by use of saliva. Ther Drug Monit 2013; 35(1): 4-29.
[http://dx.doi.org/10.1097/FTD.0b013e31827c11e7 ] [PMID: 23288091]
[12]
Wang A, Wang CP, Tu M, Wong DTW. Oral biofluid biomarker research: current status and emerging frontiers. Diagnostics (Basel) 2016; 6(4): 45.
[http://dx.doi.org/10.3390/diagnostics6040045 ] [PMID: 27999326]
[13]
Pynnönen S. The pharmacokinetics of carbamazepine in plasma and saliva of man. Acta Pharmacol Toxicol (Copenh) 1977; 41(5): 465-71.
[http://dx.doi.org/10.1111/j.1600-0773.1977.tb02157.x ] [PMID: 579557]
[14]
Troupin AS, Friel P. Anticonvulsant level in saliva, serum, and cerebrospinal fluid. Epilepsia 1975; 16(2): 223-7.
[http://dx.doi.org/10.1111/j.1528-1157.1975.tb06051.x ] [PMID: 1149709]
[15]
Rosenthal E, Hoffer E, Ben-Aryeh H, Badarni S, Benderly A, Hemli Y. Use of saliva in home monitoring of carbamazepine levels. Epilepsia 1995; 36(1): 72-4.
[http://dx.doi.org/10.1111/j.1528-1157.1995.tb01668.x ] [PMID: 8001513]
[16]
Ruiz ME, Conforti P, Fagiolino P, Volonté MG. The use of saliva as a biological fluid in relative bioavailability studies: comparison and correlation with plasma results. Biopharm Drug Dispos 2010; 31(8-9): 476-85.
[http://dx.doi.org/10.1002/bdd.728 ] [PMID: 20878879]
[17]
Idkaidek N, Arafat T. Saliva versus plasma pharmacokinetics: theory and application of a salivary excretion classification system. Mol Pharm 2012; 9(8): 2358-63.
[http://dx.doi.org/10.1021/mp300250r ] [PMID: 22784220]
[18]
Baumann RJ. Salivary Monitoring of Antiepileptic Drugs. J Pharm Pract 2007; 20: 147-57.
[http://dx.doi.org/10.1177/0897190007305139]
[19]
Djordjević S, Kilibarda V, Vucinić S, Stojanović T, Antonijević B. Toxicokinetics and correlation of carbamazepine salivary and serum concentrations in acute poisonings. Vojnosanit Pregl 2012; 69(5): 389-93.
[http://dx.doi.org/10.2298/VSP1205389D ] [PMID: 22764539]
[20]
al Za’abi M, Deleu D, Batchelor C. Salivary free concentrations of anti-epileptic drugs: an evaluation in a routine clinical setting. Acta Neurol Belg 2003; 103(1): 19-23.
[PMID: 12704979]
[21]
Liu H, Delgado MR. Therapeutic drug concentration monitoring using saliva samples. Focus on anticonvulsants. Clin Pharmacokinet 1999; 36(6): 453-70.
[http://dx.doi.org/10.2165/00003088-199936060-00006 ] [PMID: 10427469]
[22]
Hutchinson L, Sinclair M, Reid B, Burnett K, Callan B. A descriptive systematic review of salivary therapeutic drug monitoring in neonates and infants. Br J Clin Pharmacol 2018; 84(6): 1089-108.
[http://dx.doi.org/10.1111/bcp.13553 ] [PMID: 29442362]
[23]
Krasowski MD, McMillin GA. Advances in anti-epileptic drug testing. Clin Chim Acta 2014; 436: 224-36.
[http://dx.doi.org/10.1016/j.cca.2014.06.002 ] [PMID: 24925169]
[24]
Food and Drug Administration. Guidance for Industry: Bioanalytical Method Validation. US Department of Health and Human Services 2001; 4-10. Available from:. http://www.labcompliance.de/documents/FDA/FDA-Others/Laboratory/f-507-bioanalytical-4252fnl. pdf
[25]
Swartz ME, Krull IS. Validation of chromatographic methods. Pharm Technol 1998; 22: 104-19.
[26]
Tiwari G, Tiwari R. Bioanalytical method validation: an updated review. Pharm Methods 2010; 1(1): 25-38.
[http://dx.doi.org/10.4103/2229-4708.72226 ] [PMID: 23781413]
[27]
EMA. Guideline on bioanalytical method validation. EMEA, committee for medicinal products for human use. Europeans Medicines Agency 2012; 44: 1-23.EMEA/CHMP/EWP/192217/2009
[28]
Miles MV, Tennison MB, Greenwood RS. Intraindividual variability of carbamazepine, phenobarbital, and phenytoin concentrations in saliva. Ther Drug Monit 1991; 13(2): 166-71.
[http://dx.doi.org/10.1097/00007691-199103000-00013 ] [PMID: 2053125]

© 2024 Bentham Science Publishers | Privacy Policy