Selective Sample Pretreatmet Materials For Phthalate Esters In Drinking Water And Its Determination Method Development

Phthalate esters (PAEs) have become ubiquitous pollutants in the environment due to their widely use and persistent properties. The concentration of PAEs existing in the complicated environmental samples are in trace level and make sample pretreatment necessary for establishment of a reliable determination method of PAEs prior to chromatographic separation.Graphene nanoplatelet (GN) as solid-phase extraction (SPE) sorbent in combination with high performance liquid chromatography has been used for the determination of five phthalate esters (PAEs) in aqueous solutions. The operation parameters affecting the extraction efficiency were optimized. Comparative studies showed that GN was superior to other common SPE sorbents in terms of recovery and adsorption capacity. Under optimization conditions, detection limits of0.09-0.33ng/mL were achieved for five PAEs and402-711of enrichment factors for the analytes were obtained. The proposed method was successfully applied for the determination of PAEs in tap water and drink samples with recoveries ranging from87.7%to100.9%.PVA as glue with direct coating method was used to prepare GN coated SPME fiber. The DBP, DPeP and DCHP in water samples were determined by HPLC method. The influence factors of the SPME, such as solvent of desorption, extraction or desorption time, stir rate, salt effect were optimized. Method validation proved the feasibility of the developed GN as SPME sorbent for quantization of the investigated PAEs at trace levels obtaining linear range from100ng/mL to1000ng/mL. Average recoveries of individual PAE were over85.3%, and the SPME fiber could reuse about30times.Heat shrink tube (HST) acting as solid-phase microextraction (SPME) fiber coating has been firstly reported. A simple way to prepare HST-SPME was proposed to determine three Phthalate acid esters (PAEs) in bottled drinking water, coupling with high-performance liquid chromatography-ultraviolet (HPLC-UV). Under the optimized conditions, the maximum enrichment factor for the analytes reached to931, while the linear range varied between50ng/mL and5000ng/mL. The proposed method was successfully applied to the analysis of the bottled mineral water sample with recoveries ranging from90.1%to100.5%.