title: Identification of ɛ-caprolactam, melamine and urea in polyvinylpyrrolidone powders by micellar electrokinetic chromatography.
abstract: A sodium dodecyl sulfate micellar electrokinetic chromatography (SDS-MEKC) method for the simultaneous separation and identification of ɛ-caprolactam, melamine and urea deliberately added to polyvinylpyrrolidone (povidone) products has been developed. All samples to be analyzed contained paracetamol as an internal marker (IM). The optimized separations were performed in 50mM phosphate buffer (pH 7.0) containing 2% (w/v) sodium dodecyl sulfate (SDS) in fused silica capillaries with UV absorption detection at 200nm. The method was validated with respect to repeatability and intermediate precision, selectivity and robustness with satisfactory results. The relative migration times (RMT) were found to be between 0.03% and 0.13% for intra-day precision and between 0.50% and 0.60% for inter-day precision in four days. The detection limits were determined to be 1.3 (11.5μM), 0.4 (3.5μM) and 41μg/ml (0.4mM) for ɛ-caprolactam, melamine and urea, respectively.
authors.affiliation: Medical Products Agency, P.O. Box 26, SE-751 03 Uppsala, Sweden; Division of Analytical Pharmaceutical Chemistry, Department of Medicinal Chemistry, Uppsala University, Biomedical Centre, Box 574, SE-751 23 Uppsala, Sweden. Electronic address: ahmad.amini@mpa.se.
authors.forename: A
authors.initials: A
authors.lastname: Amini
mesh_terms: D002209:Caprolactam / Q000737:chemistry*; D020374:Chromatography, Micellar Electrokinetic Capillary / Q000379:methods*; D057230:Limit of Detection; D008823:Micelles; D011205:Povidone / Q000737:chemistry*; D011208:Powders / Q000737:chemistry*; D012967:Sodium Dodecyl Sulfate / Q000737:chemistry; D014227:Triazines / Q000737:chemistry*; D014508:Urea / Q000737:chemistry*
chemical_list: D008823:Micelles; D011208:Powders; D014227:Triazines; D012967:Sodium Dodecyl Sulfate; D002209:Caprolactam; D014508:Urea; D011205:Povidone; C011907:melamine
keywords: MEKC; Melamine; Polyvinylpyrrolidone; Povidone; ɛ-Caprolactam