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  • 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.
  • 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)
Title
  • Liquid chromatographic method for enantiopurity control of alaptide using polysaccharide stationary phases
  • Liquid chromatographic method for enantiopurity control of alaptide using polysaccharide stationary phases (en)
skos:prefLabel
  • Liquid chromatographic method for enantiopurity control of alaptide using polysaccharide stationary phases
  • Liquid chromatographic method for enantiopurity control of alaptide using polysaccharide stationary phases (en)
skos:notation
  • RIV/61989592:15310/11:33117970!RIV12-MSM-15310___
http://linked.open...avai/riv/aktivita
http://linked.open...avai/riv/aktivity
  • P(ED2.1.00/03.0058), Z(MSM6198959216)
http://linked.open...iv/cisloPeriodika
  • 12
http://linked.open...vai/riv/dodaniDat
http://linked.open...aciTvurceVysledku
http://linked.open.../riv/druhVysledku
http://linked.open...iv/duvernostUdaju
http://linked.open...titaPredkladatele
http://linked.open...dnocenehoVysledku
  • 209667
http://linked.open...ai/riv/idVysledku
  • RIV/61989592:15310/11:33117970
http://linked.open...riv/jazykVysledku
http://linked.open.../riv/klicovaSlova
  • Reversed-phase system; HPLC; Chiral separation; Amylose and cellulose stationary phases; Alaptide (en)
http://linked.open.../riv/klicoveSlovo
http://linked.open...odStatuVydavatele
  • DE - Spolková republika Německo
http://linked.open...ontrolniKodProRIV
  • [22BC65F39683]
http://linked.open...i/riv/nazevZdroje
  • Journal of Separation Science
http://linked.open...in/vavai/riv/obor
http://linked.open...ichTvurcuVysledku
http://linked.open...cetTvurcuVysledku
http://linked.open...vavai/riv/projekt
http://linked.open...UplatneniVysledku
http://linked.open...v/svazekPeriodika
  • 34
http://linked.open...iv/tvurceVysledku
  • Lemr, Karel
  • Douša, Michal
http://linked.open...ain/vavai/riv/wos
  • 000291986600006
http://linked.open...n/vavai/riv/zamer
issn
  • 1615-9306
number of pages
http://bibframe.org/vocab/doi
  • 10.1002/jssc.201100135
http://localhost/t...ganizacniJednotka
  • 15310
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