PMID- 24723380
OWN - NLM
STAT- MEDLINE
DCOM- 20150330
LR  - 20141006
IS  - 1522-2683 (Electronic)
IS  - 0173-0835 (Linking)
VI  - 35
IP  - 19
DP  - 2014 Oct
TI  - Optimization of the enantioseparation of a diaryl-pyrazole sulfonamide derivative 
      by capillary electrophoresis in a dual CD mode using experimental design.
PG  - 2765-71
LID - 10.1002/elps.201300639 [doi]
AB  - A CE method using dual cationic and neutral cyclodextrins (CD) was optimized for 
      the enantiomeric separation of a compound presenting a diaryl sulfonamide group. 
      Preliminary studies were made to select the optimal CDs and pH of the BGE. Two 
      CDs (amino-beta-CD and beta-CD) were selected to separate the enantiomers in a 67 mM 
      phosphate buffer at pH 7.4. However, the repeatability of the analyses obtained 
      on bare-fused silica capillary was not acceptable owing to the adsorption of the 
      amino-beta-CD to the capillary. To prevent this, a dynamic coating of the capillary 
      was used employing five layers of ionic-polymer (poly(diallyldimethylammonium) 
      chloride (PDADMAC) and poly(sodium 4-styrenesulfonate). The efficiency of the 
      coating was assessed by measuring the EOF stability. Repeatability of the 
      injections was obtained when intermediate coating with PDADMAC was performed 
      between each run. Secondly, this enantioseparation method was optimized using a 
      central composite circumscribed design including three factors: amino-beta-CD and 
      beta-CD concentrations and the percentage of methanol. Under the optimal conditions 
      (i.e. 16.6 mM of amino-beta-CD, 2.6 mM of beta-CD, 0% MeOH in 67 mM phosphate buffer 
      (pH 7.4) as BGE, cathodic injection 0.5 psi, 5 s, separation voltage 15 kV and a 
      temperature of 15 degrees C), complete enantioresolution of the analyte was obtained. It 
      is worth mentioning that the design of experiments (DOE) protocol employed showed 
      a significant interaction between CDs, highlighting the utility of DOE in method 
      development. Finally, small variations in the ionic-polymer concentrations did 
      not significantly influence the EOF, confirming the robustness of the coating 
      method.
CI  - (c) 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
FAU - Rogez-Florent, Tiphaine
AU  - Rogez-Florent T
AD  - Universite Lille Nord de France, Lille, France; UDSL, Analytics chemistry 
      laboratory, Lille, France.
FAU - Foulon, Catherine
AU  - Foulon C
FAU - Six, Perrine
AU  - Six P
FAU - Goossens, Laurence
AU  - Goossens L
FAU - Danel, Cecile
AU  - Danel C
FAU - Goossens, Jean-Francois
AU  - Goossens JF
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
DEP - 20140605
PL  - Germany
TA  - Electrophoresis
JT  - Electrophoresis
JID - 8204476
RN  - 0 (Polymers)
RN  - 0 (Sulfonamides)
RN  - 0 (beta-Cyclodextrins)
SB  - IM
MH  - Electrophoresis, Capillary/*instrumentation/*methods
MH  - Polymers
MH  - Reproducibility of Results
MH  - Research Design
MH  - Stereoisomerism
MH  - Sulfonamides/*chemistry/*isolation & purification
MH  - beta-Cyclodextrins/*chemistry
OTO - NOTNLM
OT  - Arylsulfonamide
OT  - Capillary electrophoresis
OT  - Cationic and neutral dual CD mode
OT  - Central composite design
OT  - Multilayer coating
EDAT- 2014/04/12 06:00
MHDA- 2015/03/31 06:00
CRDT- 2014/04/12 06:00
PHST- 2013/12/18 00:00 [received]
PHST- 2014/03/27 00:00 [revised]
PHST- 2014/03/29 00:00 [accepted]
PHST- 2014/04/12 06:00 [entrez]
PHST- 2014/04/12 06:00 [pubmed]
PHST- 2015/03/31 06:00 [medline]
AID - 10.1002/elps.201300639 [doi]
PST - ppublish
SO  - Electrophoresis. 2014 Oct;35(19):2765-71. doi: 10.1002/elps.201300639. Epub 2014 
      Jun 5.