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All Journal JURNAL ILMU KEFARMASIAN INDONESIA
SUDIBYO MARTONO
Gadjah Mada University
Medicine & Pharmacology

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Isocratic High Performance Liquid Chromatographic Method for Determination of Metoprolol and Its Metabolite in Human Urine PRI ISWATI UTAMI; SUGIYANTO SUGIYANTO; SUDIBYO MARTONO; LUKMAN HAKIM
JURNAL ILMU KEFARMASIAN INDONESIA Vol 14 No 1 (2016): JIFI
Publisher : Fakultas Farmasi Universitas Pancasila

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Abstract

An isocratic reversed phase high performance liquid chromatographic (HPLC) method has been developed for the determination of metoprolol (MET) and α-hydroxymetoprolol (α-OH MET) in human urine. Analytes were extracted using dichloromethane. The optimized separations were performed on a Purospher® STAR RP-18e LiChroCART® (250 x 4.6 mm, 5μm) HPLC column within 12 min by an isocratic elution with 25 mmol/L aqueous potassium dihydrogen phosphate buffer (pH 3.0) containing 15% (v/v) acetonitrile and 15% (v/v) methanol, and UV detection at 234 nm. The method was validated for linearity, accuracy, precision and specificity. The calibration curves for both analytes were linear over the range investigated (1.0-64.0 μg/mL) with correlation coefficients of 0.999. Relative standard deviation (RSD) values were below 2%. For all of the analytes, recoveries value from 98.36±1.68 to 101.32±1.36 % and the limits of detection for MET and α-OH MET were 0.22 and 0.14 μg/mL, respectively. The method developed has been demonstrated to be sensitive and reliable for the measurement of MET and α-OH MET simultaneously in human urine.
Validasi Metode Kromatografi Lapis Tipis untuk Penentuan Konsentrasi Kurkumin dalam Sampel Disolusi yang Mengandung Ektrak Curcuma longa DEWI SETYANINGSIH; YOSI BAYU MURTI; ACHMAD FUDHOLI; WOUTER L.J. HINRICHS; ROCHMAT MUDJAHID; SUDIBYO MARTONO; TRIANA HERTIANI
JURNAL ILMU KEFARMASIAN INDONESIA Vol 14 No 2 (2016): JIFI
Publisher : Fakultas Farmasi Universitas Pancasila

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Curcumin is a lipophilic compound which suffers from the poor bioavailability after oral administration. Increasing its dissolution rate can be a successful strategy to improve the bioavailability. Along with the formulation developments, a rapid and simple analytical method to determine curcumin concentrations in the dissolution medium is required. The aim of this study was to develop and to validate an analytical method based on thin layer chromatography (TLC) to determine curcumin concentrations in a dissolution medium containing 0.5% w/v sodium lauryl sulfate (SLS) and 20 mM sodium phosphate buffer. A polyvinylpyrrolidone K30 based solid dispersion of Curcuma longa extract and its corresponding physical mixture were dissolved in a medium containing 0.5% w/v SLS and 20 mM sodium phosphate buffer (pH 6.0). Dissolution samples were spotted on a normal TLC plate and eluents of various compositions were evaluated. The retardation factor (Rf), resolution (Rs), and asymmetry factor (As0.05) of the optimized method were determined. Using the optimized eluent, proper separation of curcumin peak was achieved with an Rf of 0.50, Rs of 2.62 and As 0.05of 0.87. Linearity (5-30 μg/mL) was demonstrated by r value of 0.9965. The TLC method provided precision with RSD ≤3.50 and accuracy with recovery value of 94-105%.
Co-Authors ACHMAD FUDHOLI Dewi Setyaningsih LUKMAN HAKIM PRI ISWATI UTAMI ROCHMAT MUDJAHID SUGIYANTO SUGIYANTO Triana Hertiani WOUTER L.J. HINRICHS YOSI BAYU MURTI