Analysis of non-phthalates plasticizers on porous graphitic carbon by supercritical fluid chromatography using evaporative light scattering detection

摘要

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 CO_2 supercritical fluid. The effect of alkyl chain (pentane, hexane, heptane) and chlorinated (CH_2Cl_2, CHCl_3, CCl_4) solvents was studied on the retention and on the ELSD detection of plasticizers. A co-solvent mixture composed of CHCl_3 /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 CHCl_3/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.