Enhancing verapamil trace determination from biological matrices by bar adsorptive microextraction
Camilla Fonseca Silva1,2, Mariana Foles Mendes2, José Manuel Flôrencio Nogueira2
1Departamento de Ciências Naturais, Universidade Federal de São João del-Rei, Campus Dom Bosco, Praça Dom Helvécio 74, Fábricas, 36301-160, São João del-Rei, Minas Gerais, Brazil. keyller@ufsj.edu.br.
Abstract:
Verapamil is an L-type calcium channel blocker widely used in the treatment of cardiovascular diseases such as hypertension, angina and arrhythmias, requiring accurate therapeutic monitoring to maintain plasma, urine and saliva concentrations within a safe range. In this context, a novel analytical approach has been proposed to determine verapamil in biological samples, using bar adsorptive microextraction coated with reversed-phase polymers followed by high-performance liquid chromatography with diode array detection. Two adsorbents have been chosen, i.e. STRATA-CN and ENVI-18 polymers, showing recoveries from 56.01 ± 2.16% to 96.82 ± 0.61% under optimized experimental conditions, such as sample pH: 10.0 (STRATA-CN) and 8.0 (ENVI-18), 2 h of equilibrium time, stirring speed at 990 rpm, back-extraction solvent using methanol:acetonitrile (1 : 1 v/v), and 1 h under sonication. The analytical method showed linearity from 20 to 600 ng mL-1 (r ≥ 0.99), as well as adequate precision (with RSD% below 15%) and accuracy (with RE% within 15% of the nominal value). Finally, the analytical method was applied to plasma, urine and saliva samples and proved to be a promising alternative for the trace analysis of verapamil in biological matrices.
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