. . "Liquid chromatographic method for enantiopurity control of alaptide using polysaccharide stationary phases"@en . "RIV/61989592:15310/11:33117970" . "Liquid chromatographic method for enantiopurity control of alaptide using polysaccharide stationary phases" . . "12" . "000291986600006" . "15310" . . "Separation of veterinary drug alaptide ((S)-8-methyl-6,9-diazaspiro(4,5) decane-7,10-dione) from a chiral impurity (R-enantiomer) was developed. Five chiral columns (three amylose and two cellulose type) were evaluated in a reversed-phase system. Three of them offered satisfactory enantiomeric resolution. Finally, three methods were validated and proved to be applicable for the determination of a chiral impurity content below 0.1% (method A: 3-AmyCoat column, tris-[3,5-dimethylphenyl] carbamoyl amylose; mobile phase: water/methanol/propan-2-ol/butan-2-ol=75:20:3.5:1.5 v/v, flow rate: 0.40 mL/min; column temperature: 30 degrees C; method B: Chiralpak AS-3R, tris-[1-phenylethyl] carbamoyl amylose; water/acetonitrile=80:20 v/v, 0.40 mL/min; 40 degrees C; method C: Chiralcel OZ-3R, tris-[3-chloro-4-methylphenyl] carbamoyl cellulose; water/acetonitrile=80:20 v/v, 0.40 mL/min; 40 degrees C). Some decrease in efficiency with repeated sample injections was observed for the 3-AmyCoat column. The resistance to mass transfer in the stationary phase increased probably due to the change in chiral selector conformation. This effect was considerably suppressed by propan-2-ol or to a greater extent by butan-2-ol added to a mobile phase. Simple regeneration was also suggested to recover efficiency of the column." . . "[22BC65F39683]" . . "Separation of veterinary drug alaptide ((S)-8-methyl-6,9-diazaspiro(4,5) decane-7,10-dione) from a chiral impurity (R-enantiomer) was developed. Five chiral columns (three amylose and two cellulose type) were evaluated in a reversed-phase system. Three of them offered satisfactory enantiomeric resolution. Finally, three methods were validated and proved to be applicable for the determination of a chiral impurity content below 0.1% (method A: 3-AmyCoat column, tris-[3,5-dimethylphenyl] carbamoyl amylose; mobile phase: water/methanol/propan-2-ol/butan-2-ol=75:20:3.5:1.5 v/v, flow rate: 0.40 mL/min; column temperature: 30 degrees C; method B: Chiralpak AS-3R, tris-[1-phenylethyl] carbamoyl amylose; water/acetonitrile=80:20 v/v, 0.40 mL/min; 40 degrees C; method C: Chiralcel OZ-3R, tris-[3-chloro-4-methylphenyl] carbamoyl cellulose; water/acetonitrile=80:20 v/v, 0.40 mL/min; 40 degrees C). Some decrease in efficiency with repeated sample injections was observed for the 3-AmyCoat column. The resistance to mass transfer in the stationary phase increased probably due to the change in chiral selector conformation. This effect was considerably suppressed by propan-2-ol or to a greater extent by butan-2-ol added to a mobile phase. Simple regeneration was also suggested to recover efficiency of the column."@en . . . "5"^^ . "1615-9306" . "Liquid chromatographic method for enantiopurity control of alaptide using polysaccharide stationary phases" . . . "DE - Spolkov\u00E1 republika N\u011Bmecko" . . . "2"^^ . . "Dou\u0161a, Michal" . "10.1002/jssc.201100135" . "P(ED2.1.00/03.0058), Z(MSM6198959216)" . "RIV/61989592:15310/11:33117970!RIV12-MSM-15310___" . "Liquid chromatographic method for enantiopurity control of alaptide using polysaccharide stationary phases"@en . . . "1"^^ . "Journal of Separation Science" . . "Lemr, Karel" . . . . "209667" . "34" . . "Reversed-phase system; HPLC; Chiral separation; Amylose and cellulose stationary phases; Alaptide"@en .