MIL-101(Cr)/SiO2涂层搅拌棒吸附萃取-超高效液相色谱测定环境中的邻苯二甲酸酯类

Determination of phthalates in environment by ultra performance liquid chromatography with MIL-101(Cr)/SiO2 coated stir bar adsorption extraction

采用MIL-101(Cr)/SiO2材料作为搅拌棒吸附萃取涂层,运用溶胶凝胶技术制备出有效吸附极性有机物的搅拌棒。通过XRD,SEM,FT-IR对搅拌棒涂层材料进行了表征,并将所制得搅拌棒与超高效液相色谱联用,建立了MIL-101(Cr)/SiO2涂层搅拌棒吸附萃取-超高效液相色谱法测定环境样品中5种邻苯二甲酸酯。对提取时间、搅拌速率、pH、离子强度和解吸时间等萃取条件进行了优化,富集倍数最高可达到98.8倍。在最优条件下,该方法的线性范围为10.00~4375μg/L,R^2范围为0.9880~0.9998,检出限为0.05~0.095μg/L。该方法成功应用于环境水和土壤中5种邻苯二甲酸酯的检测。

Phthalate esters in environmental samples were determined by the stir bar adsorption extraction combined with ultra-performance liquid chromatography,using MIL-101(Cr)/SiO2 composite as the stir bar adsorption extraction coating.The coating of stir bars was prepared by sol-gel method with high efficiency.Characterization of MIL-101(Cr)/SiO2 composite was accomplished by X-ray diffraction(XRD),field emission scanning electron microscope(SEM),and fourier transform infrared spectrum(FT-IR).The extraction time,stirring rate,pH,ionic strength and desorption time of SBSE for detection of five phthalates were optimized,and the as-prepared MIL-101(Cr)/SiO2 composite exhibited very good stability and showed excellent adsorption and extraction behavior for phthalates.The method performances were satisfying under the optimal conditions,with a linear range of 10-4375μg/L,the linear correlation coefficient of 0.9880-0.9998,the enrichment factor of 98.8,and the detection limit of 0.05-0.095μg/L.The method exhibits great promise in detection of phthalates in environmental application.