| Article ID | Journal | Published Year | Pages | File Type |
|---|---|---|---|---|
| 1199409 | Journal of Chromatography A | 2014 | 10 Pages |
•Non-phthalate plasticizers have been analyzed by SFC/ELSD using porous graphitic carbon.•The effect of various solvents on the ELSD detection of plasticizers was studied.•The ELSD response was improved using a co-solvent mixture composed of CHCl3/heptane.•An experimental design was used to optimize both separation and detection of plasticizers.
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 7 min and best signal-to-noise ratios were obtained with outlet pressure and drift tube temperature of ELSD set at 200 bar 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 2.2 min 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.
