title: LC of pharmaceutically important halogenated 8-hydroxyquinolines after precolumn derivatization with Pd (II).
abstract: An accurate, sensitive, and selective reversed phase high performance liquid chromatographic (HPLC) method was developed for the analysis of two halogenated 8-hydroxyquinoline derivatives; clioquinol (CQN) and iodoquinol (IQN). The proposed method depends on the complexation ability of the studied compounds with Pd(II) ions. Reversed phase chromatography was conducted using a 300 x 3.9 mm i.d. stainless steel column packed with 10 microm Bondclone phenyl at ambient temperature. A solution containing 0.005% w/v of Pd(II)-chloride in a mixture of acetonitrile-methanol-water (3:3:4 v/v/v) of pH 3.7 as a mobile phase pumped at a flow rate of 0.75 ml min(-1). UV-detection was performed at 282 and 285 nm for CQN and IQN, respectively. The method showed excellent linearity in the range 0.05-1.8 and 0.1-3.0 microg ml(-1) with limit of detection (S/N=2) 4.8 ng ml(-1) (1.57 x 10(-8) M) and 6.4 ng ml(-1) (1.61 x 10(-8) M) for CQN and IQN, respectively. The suggested method was successfully applied for the analysis of the studied drugs in bulk with average% recoveries of 99.68+/-0.44 for CQN and 99.65+/-0.53 for IQN. The proposed method was successfully applied for the analysis of the studied drugs in single or combined dosage forms with average% recoveries of 99.41+/-0.51-100.02+/-0.63. The proposed method could be used successfully for the determination of the studied compounds in the presence of their degradation product as they could be eluted with different retention times. The presence of metronidazole (MNZ) or tolnaftate (TFT) with the studied drugs does not affect their accurate determination. The results obtained were favorably compared with those obtained by the reference method. The results were satisfactorily, accurate, and precise.
authors.affiliation: Faculty of Pharmacy, Department of Analytical Chemistry, University of Mansoura, Mansoura, Egypt. zasheribah@mum.mans.eun.eg
authors.forename: M
authors.initials: M
authors.lastname: Rizk
authors.forename: F
authors.initials: F
authors.lastname: Belal
authors.forename: F
authors.initials: F
authors.lastname: Ibrahim
authors.forename: S
authors.initials: S
authors.lastname: Ahmed
authors.forename: Z A
authors.initials: ZA
authors.lastname: Sheribah
mesh_terms: D000891:Anti-Infective Agents, Local / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D007464:Clioquinol / Q000032:analysis; D004304:Dosage Forms; D006219:Halogens / Q000032:analysis*; D004103:Iodoquinol / Q000032:analysis; D007854:Lead / Q000737:chemistry*; D015125:Oxyquinoline / Q000032:analysis*; D010165:Palladium; D004364:Pharmaceutical Preparations / Q000032:analysis
chemical_list: D000891:Anti-Infective Agents, Local; D004304:Dosage Forms; D006219:Halogens; D004364:Pharmaceutical Preparations; D007854:Lead; C029891:lead chloride; D010165:Palladium; D015125:Oxyquinoline; D004103:Iodoquinol; D007464:Clioquinol