Quantitative analysis of Loperamide hydrochloride in the presence its acid degradation products

Hemijska industrija (Impact Factor: 0.36). 01/2009; 63(1). DOI: 10.2298/HEMIND0901039S
Source: DOAJ


The aim of this work was to develop a new RP-HPLC method for the determination of loperamide hydrochloride in the presence of its acid degradation products. Separation of loperamide from degradation products was performed using ZORBAX Eclipse XDB C-18, column with a mobile phase consisting of 0.1% sodium-octansulphonate, 0.05% triethylamine, 0.1% ammonium hydroxide in water:acetonitrile (45:55 v/v). The mobile phase was adjusted to pH 3.2 with phosphoric acid. The method showed high sensitivity with good linearity over the concentration range of 10 to 100 μg cm-3. The method was successfully applied to the analysis of a pharmaceutical formulation (Loperamide, Zdravlje-Actavis, Serbia) containing loperamide hydrochloride with excellent recovery. The loperamide hydrochloride degradation during acid hydrolysis and kinetics investigation was carried out in hydrochloric acid solutions of 0.1, 1.0 and 1.5 mol dm-3, at different temperatures (25 and 40°C), by monitoring the parent compound itself. The first order reaction of loperamide degradation in acid solution was determined. The activation energy was estimated from the Arrhenius plot and it was found to be 38.81 kJ mol-1 at 40°C. The developed procedure was successfully applied for the rapid determination of loperamide hydrochloride in pharmaceutical formulation (Loperamide, Zdravlje-Actavis, Serbia) and in the presence of its acid degradation products.

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    • "In humans, following oral administration of loperamide solid formulations, about 50% of the administered loperamide is absorbed in the gastrointestinal tract, absorbance occurring within 1 h in high bounding percent to plasma proteins (95%) [8], at maximum concentration time of 6 h and half-life around 11 h [9], but only a little intact drug (1%) reaches systemic circulation, due to its extensive first pass metabolism [6] [7]. Loperamide determination in human body makes challenging work in bioavailability and bioequivalence research field, due to its low availability in plasma and low doses [6] [7], in pharmaceutical industries and in vitro studies, loperamide has been determined by HPLC easily [10] [11] [12] [13] [14], and more sensitive methods were required for in vivo determinations, as in rats by HPLC–UV [15] and HPLC–ECD [16]. In human body there were many determinant studies of loperamide by using LC-tandem MS [17] [18] [19] [20], but more sensitive bioanalytical methods with easier 1570-0232/© 2014 Elsevier B.V. All rights reserved. "
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