Solid Phase Extraction - Capillary Gas Chromatography Analysis Of Six Trace Phthalate Esters

In the recent years, considerable attention has been paid to the human exposure to Phthalic acid esters (Phthalates, PAEs), one of environmental hormones. An efficient analysis of phthalates becomes necessary for better monitoring them. The solid-phase extraction (SPE) procedure is an new less time-consuming and economical sample pretreatment technique. The purpose of our optimization study was to develop a multi-residual SPE method coupled to capillary GC-ECD encompassing six most common phthalates in pond water at GuangZhou pearl river fisheries research institute and to proceed preliminary study about SPE for aquatic products.Firstly, the influence of split ratio and the temperature rise rates on chromatogram peak heights of analytes was investigated with the aid of uniform design. The splitless injection was selected ultimately and the optional oven temperature was programmed from 50℃ held 2 min, then increased to 200℃ at 25℃min^-1, held 2 min before increasing to 280℃ at 40℃min^-1, held 5min, the total GC run time is 17 min.Secondly, depended on C₁₈ cartridge, uniform design method was again employed toexamine four SPE factors affecting the partition of analytes——eluentcomponent(hexane:acetone), elution volume(ml), elution rate(mlmin^-1), sampling rate(mlmin^-1). The influence of four factors for individual analytes were expressed as mathematic models and optimized by computer pattern recognition(CRP) technology. The final SPE method employing eluent component(hexane:acetone)35:1, elution volume 2 ml , elution rate 1 mlmin^-1 , sampling rate 9 mlmin' enabled the determination of all six phthalates in water sample.Thirdly, the SPE—GC—ECD method for the determination of six phthalates was validated. The results showed linear response over four orders of magnitude, that were DMP, DEP, DOP 0.1¹00mg/l, DBP, BEHP 0.02¹0mg/l, BBP 0.001 ¹0mg/l. The determined compounds of DMP, DEP, DBP, DEHP, DOP, BBP were 0.4ng/l, 0.3ng/l, 0.1ng/l, 0. 02ng/l, 0.04 ng/l, 0.01 ng/1, respectively. The precisions of six...