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Statements

Subject Item
n2:RIV%2F61989592%3A15310%2F11%3A33117970%21RIV12-MSM-15310___
rdf:type
n5:Vysledek skos:Concept
dcterms:description
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.
dcterms: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
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
skos:notation
RIV/61989592:15310/11:33117970!RIV12-MSM-15310___
n5:predkladatel
n6:orjk%3A15310
n3:aktivita
n19:P n19:Z
n3:aktivity
P(ED2.1.00/03.0058), Z(MSM6198959216)
n3:cisloPeriodika
12
n3:dodaniDat
n8:2012
n3:domaciTvurceVysledku
n18:4316851
n3:druhVysledku
n15:J
n3:duvernostUdaju
n21:S
n3:entitaPredkladatele
n16:predkladatel
n3:idSjednocenehoVysledku
209667
n3:idVysledku
RIV/61989592:15310/11:33117970
n3:jazykVysledku
n11:eng
n3:klicovaSlova
Reversed-phase system; HPLC; Chiral separation; Amylose and cellulose stationary phases; Alaptide
n3:klicoveSlovo
n4:Alaptide n4:HPLC n4:Reversed-phase%20system n4:Amylose%20and%20cellulose%20stationary%20phases n4:Chiral%20separation
n3:kodStatuVydavatele
DE - Spolková republika Německo
n3:kontrolniKodProRIV
[22BC65F39683]
n3:nazevZdroje
Journal of Separation Science
n3:obor
n20:CB
n3:pocetDomacichTvurcuVysledku
1
n3:pocetTvurcuVysledku
2
n3:projekt
n12:ED2.1.00%2F03.0058
n3:rokUplatneniVysledku
n8:2011
n3:svazekPeriodika
34
n3:tvurceVysledku
Douša, Michal Lemr, Karel
n3:wos
000291986600006
n3:zamer
n14:MSM6198959216
s:issn
1615-9306
s:numberOfPages
5
n17:doi
10.1002/jssc.201100135
n9:organizacniJednotka
15310