title: Analysis of non-phthalates plasticizers on porous graphitic carbon by supercritical fluid chromatography using evaporative light scattering detection.
abstract: The analysis of several plasticizers, widely used in the production of medical devices, was investigated on porous graphitic carbon (PGC) stationary phase in supercritical fluid chromatography (SFC) with an evaporative light scattering detector (ELSD). Due to strong interaction of compounds with the PGC support, solvents of strong eluotropic strength were added to the CO2 supercritical fluid. The effect of alkyl chain (pentane, hexane, heptane) and chlorinated (CH2Cl2, CHCl3, CCl4) solvents was studied on the retention and on the ELSD detection of plasticizers. A co-solvent mixture composed of CHCl3/heptane, eluted under gradient mode, allowed a significant improvement of the ELSD response compared to the use of each solvent individually. Then, a central composite design (CCD) was implemented to optimize both the separation and the detection of plasticizers. The parameters involved were the outlet pressure, the gradient slope, the co-solvent composition and the drift tube temperature of the ELSD. After optimization, baseline separation of plasticizers was achieved in 7min and best signal-to-noise ratios were obtained with outlet pressure and drift tube temperature of ELSD set at 200bar and 31°C, respectively. The co-solvent mixture was also composed of CHCl3/heptane (35/65 v/v) and a gradient from 15 to 60% of co-solvent in 2.2min was employed. The results demonstrated that CCD is a powerful tool for the optimization of SFC/ELSD method and the response surface model analysis can provide statistical understandings of the significant factors required to achieve optimal separation and ELSD sensitivity.
authors.affiliation: Univ Lille Nord de France, UDSL, EA 4481, UFR Pharmacy, 59006 Lille, France.
authors.forename: Claude
authors.initials: C
authors.lastname: Vaccher
authors.affiliation: Univ Lille Nord de France, UDSL, EA 4481, UFR Pharmacy, 59006 Lille, France; Department of Pharmacy, University Hospital, Lille, France.
authors.forename: Bertrand
authors.initials: B
authors.lastname: Decaudin
authors.affiliation: Department of Pharmacy, University Hospital, Clermont-Ferrand, France; EA 4676 C-Biosenss, Auvergne University, Clermont-Ferrand, France.
authors.forename: Valérie
authors.initials: V
authors.lastname: Sautou
authors.affiliation: Univ Lille Nord de France, UDSL, EA 4481, UFR Pharmacy, 59006 Lille, France. Electronic address: marie.lecoeur@univ-lille2.fr.
authors.forename: Marie
authors.initials: M
authors.lastname: Lecoeur
mesh_terms: D025924:Chromatography, Supercritical Fluid / Q000295:instrumentation / Q000379:methods*; D006108:Graphite / Q000737:chemistry*; D010795:Phthalic Acids / Q000032:analysis; D010968:Plasticizers / Q000032:analysis*; D016062:Porosity; D059629:Signal-To-Noise Ratio; D013696:Temperature
chemical_list: D010795:Phthalic Acids; D010968:Plasticizers; C032279:phthalic acid; D006108:Graphite
keywords: Evaporative light scattering detector; Experimental design; Plasticizers; Porous graphitic carbon; Supercritical fluid chromatography