title: Determination of glucosamine and carisoprodol in pharmaceutical formulations by LC with pre-column derivatization and UV detection.
abstract: A simple and reliable precolumn derivatization liquid chromatography method with ultraviolet detection has been developed and validated for the analysis of glucosamine (GS) in various dietary supplement formulations and raw materials. Additionally, the proposed method was used for analysis of carisoprodol (CR) found in ternary mixture with paracetamol (PR) and caffeine (CF). The linearity ranges were 1-100 μg/mL for GS, 1-150 μg/mL for CR, PR and CF. Derivatization was used with 1,2-naphthoquinone-4-sulphonic acid sodium salt in the presence of borate buffer. Chromatographic separation of GS-naphthoquinone derivative was achieved by using a mixture of acetonitrile and water (pH 7.3 adjusted with 0.1 M NaOH) in the ratio 10:90, v/v and flow-rate of 1.0 mL/min. UV detection was carried out at 280 nm. For PR, CF, and CR-naphthoquinone derivative, the chromatographic separation was achieved by using mixture of acetonitrile and 20 mM KH(2)PO(4) (pH 3.0 adjusted with phosphoric acid) in the ratio 20:80, v/v and flow-rate of 1.0 mL/min. UV detection was carried out at 275 nm. The limits of detection were 37.2, 35.9, 30.4 and 40.0 ng/mL for GS, CR, PR and CF, respectively.
authors.affiliation: Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, University of Suez Canal, Ismailia 41522, Egypt. ghhadad@hotmail.com
authors.forename: Ghada M
authors.initials: GM
authors.lastname: Hadad
authors.forename: Randa A
authors.initials: RA
authors.lastname: Abdel-Salam
authors.forename: Samy
authors.initials: S
authors.lastname: Emara
mesh_terms: D000082:Acetaminophen / Q000737:chemistry; D000097:Acetonitriles / Q000737:chemistry; D002110:Caffeine / Q000737:chemistry; D002328:Carisoprodol / Q000032:analysis*; D002626:Chemistry, Pharmaceutical; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D056148:Chromatography, Reverse-Phase; D004338:Drug Combinations; D005944:Glucosamine / Q000032:analysis*; D057230:Limit of Detection; D015203:Reproducibility of Results; D013056:Spectrophotometry, Ultraviolet; D013607:Tablets / Q000737:chemistry
chemical_list: D000097:Acetonitriles; D004338:Drug Combinations; D013607:Tablets; D002328:Carisoprodol; D000082:Acetaminophen; D002110:Caffeine; D005944:Glucosamine; C032159:acetonitrile