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Separation of phthalates by cyclodextrin modified micellar electrokinetic chromatography: Quantitation in perfumes
Authors:Virginia Pérez-Fernández  Maria José González  Maria Ángeles García  Maria Luisa Marina
Institution:1. Department of Analytical Chemistry, Faculty of Chemistry, University of Alcalá, Spain;2. Department of Instrumental Analysis and Environmental Chemistry, Institute of General Organic Chemistry, CSIC, Spain
Abstract:A new CE method has been developed for the simultaneous separation of a group of parent phthalates. Due to the neutral character of these compounds, the addition of several bile salts as surfactants (sodium cholate (SC), sodium deoxycholate (SDC), sodium taurodeoxycholate (STDC), sodium taurocholate (STC)) to the separation buffer was explored showing the high potential of SDC as pseudostationary phase. However, the resolution of all the phthalates was not achieved when employing only this bile salt as additive, being necessary the addition of neutral cyclodextrins (CD) and organic modifiers to the separation media. The optimized cyclodextrin modified micellar electrokinetic chromatography (CD-MEKC) method consisted of the employ of a background electrolyte (BGE) containing 25 mM β-CD-100 mM SDC in a 100 mM borate buffer (pH 8.5) with a 10% (v/v) of acetonitrile, employing a voltage of 30 kV and a temperature of 25 °C. This separation medium enabled the total resolution of eight compounds and the partial resolution of two of the analytes, di-n-octyl phthalate (DNOP) and diethyl hexyl phthalate (DEHP) (Rs ~ 0.8), in only 12 min. The analytical characteristics of the developed method were studied showing their suitability for the determination of these compounds in commercial perfumes. In all the analyzed perfumes the most common phthalate was diethyl phthalate (DEP) that appeared in ten of the fifteen analyzed products. Also dimethyl phthalate (DMP), diallyl phthalate (DAP), dicyclohexyl phthalate (DCP), and di-n-pentyl phthalate (DNPP) were found in some of the analyzed samples.
Keywords:Ac  corrected peak areas  Ac-β-CD  acetyl-β-CD  BGE  background electrolyte  BBP  benzyl butyl phthalate  CD  cyclodextrin  CD-MEKC  cyclodextrin modified micellar electrokinetic chromatography  CHES  n-cyclohexyl-2-aminoethanesulfonic acid  DAD  diode array detector  DAP  diallyl phthalate  DCP  dicyclohexyl phthalate  DBP  di-n-butyl phthalate  DEHP  diethyl hexyl phthalate  DEP  diethyl phthalate  DiBP  diisobutyl phthalate  DM-β-CD  dimethyl-β-CD  DMP  dimethyl phthalate  DNPP  di-n-pentyl phthalate  DNOP  di-n-octyl phthalate  DPP  di-n-propyl phthalate  DPhP  diphenyl phthalate  EOF  electroosmotic flow  HP-β-CD  hydroxypropyl-β-CD  k  capacity factor  LOD  limit of detection  LOQ  limit of quantitation  Me-β-CD  methyl-β-CD  PVC  polyvinyl chloride plastics  SC  sodium cholate  SDC  sodium deoxycholate  SDS  sodium dodecyl sulfate  STDC  sodium taurodeoxycholate  STC  sodium taurocholate  SPE  solid phase extraction  TM-β-CD  trimethyl-β-CD
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