Pulsed amperometric detection (PAD) of diuretic drugs in herbal formulations using a gold electrode following ion-pair chromatographic separation |
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Authors: | Leandro M de Carvalho Carine Viana Ana Paula L Moreira Paulo C do Nascimento Denise Bohrer Monique J Motta Géssica D da Silveira |
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Institution: | 1. Graduate Programm in Pharmaceutical Sciences, Federal University of Santa Maria (UFSM), Santa Maria, Rio Grande do Sul, Brazil 2. Department of Chemistry, Federal University of Santa Maria (UFSM), Santa Maria, Rio Grande do Sul, Brazil
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Abstract: | Herein, we present a new method based on separation by ion-pair chromatography with pulsed amperometric detection for evaluating various diuretics, including hydrochlorothiazide, chlorthalidone, furosemide, and amiloride, which are adulterants in herbal-based pharmaceutical formulations. The amperometric detection cycle (time?=?2 s) was performed at a gold electrode by applying a detection potential (E1) of +800 mV for 0.4 s and an oxidation potential (E2) of +1,000 mV for 0.40 s, followed by a reduction potential (E3) of ?200 mV for 1.20 s. The mobile phase for separating the diuretics was composed of 5 mmol L?1 phosphate buffer and 0.3 mmol L?1 sodium dodecyl sulfate in 50 % (v/v) methanol (pH 4.5). This method enabled the quantification of the drugs at low concentrations (i.e., 0.08 mg/capsule for hydrochlorothiazide, 0.01 mg/capsule for chlorthalidone, and 0.007 mg/capsule for furosemide). Twenty-six herbal formulations were analyzed, and eight samples (30.8 %) were found to contain diuretics that were added to the final composition (declared or not). |
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