为实现对环境水样中污染物PBDEs(多溴联苯醚)的预富集和分析,利用溶胶-凝胶法制取了一种MOFs(金属有机骨架材料)凝胶膜片微固相萃取装置,结合GC-ECD(气相色谱-电子捕获检测器)检测方法测定环境水样中的7种PBDEs,考察了MOFs用量、萃取温度、萃取时间和解吸时间对于萃取效果的影响.结果表明,在MOFs用量为4 mg、萃取温度为70℃、萃取时间为50 min、解吸时间为15 min的条件下,7种PBDEs单体的加标回收率为74.9%~98.1%,相对标准偏差为3.3%~5.7%,方法检出限均小于4.7 ng/L.
A micro-solid-phase extraction device was developed using the sol-gel method by assembling with a metal-organic frameworks(MOFs) with the gel to form a 1 mm membrane.Subsequently,this device was applied for determination of seven polybrominated diphenyl ethers(PBDEs) in the water by coupling with the gas chromatography-electron capture detector.Variables affecting the extraction efficiency including the amount of the MOFs,extraction temperature,extraction time and desorption time were detected.Under the optimized conditions(MOF 4 mg,extraction temperature 70 ℃,evtraction time 50 min,and desorption time 15 min) recoveries of the seven PBDEs were in the range of 74.9% to 98.1%,and the relative standard deviations were between 3.3% and 5.7%.Limits of detection were less than 4.7 ng/L for all seven PBDEs.