Determination of the 2-bromomethyl-2-(2,4-dichlorophenyl)-1, 3-dioxolan-4-yl)methyl benzoate diastereoisomers by supercritical fluid chromatography.
The study of the separation and determination of the two 2-bromomethyl-2-(2,4-dichlorophenyl)-1,3-dioxolan-4-yl-methyl benzoate diastereoisomers is presented in this work. The separation was achieved using packed column supercritical fluid chromatography. Three stationary phases were checked, the C(18) packing providing the best results. The influence of several parameters (nature and percentage of modifier, temperature and pressure) on the separation were also evaluated. The baseline separation (R(s)=1.78) of the compounds was obtained in only 2 min, using a C(18) column, a pressure of 100 bar, a temperature of 35 degrees C, a flow-rate of 2. 5 ml/min and 5% of 2-propanol as organic modifier. Under these conditions the unwanted diastereoisomer (trans) was eluted before the main compound (cis), so the determination of the purity was more accurate.
Toribio
L
L
Department of Analytical Chemistry, Faculty of Sciences, University of Valladolid, Prado de la Magdalena s/n, E-47005, Valladolid, Spain.
Bernal
J L
JL
del Nozal
M J
MJ
Jimenez
J J
JJ
Serna
M L
ML
D019840:2-Propanol / Q000737:chemistry; D001565:Benzoates / Q000737:chemistry / Q000302:isolation & purification*; D002845:Chromatography / Q000295:instrumentation / Q000379:methods*; D002851:Chromatography, High Pressure Liquid; D004148:Dioxolanes / Q000302:isolation & purification*; D000431:Ethanol / Q000737:chemistry; D000432:Methanol / Q000737:chemistry; D011312:Pressure; D013237:Stereoisomerism; D013696:Temperature
C413285:2-bromomethyl-2-(2,4-dichlorophenyl)-1,3-dioxolan-4-yl; D001565:Benzoates; D004148:Dioxolanes; D000431:Ethanol; C044605:methyl benzoate; D019840:2-Propanol; D000432:Methanol