采用中空纤维液相微萃取与高效液相色谱联用技术测定了尿液样品中的痕量己烯雌酚；考察了样品相酸度、中间相种类、接收相浓度、搅拌速度、萃取时间等对液-液-液三相微萃取效率的影响,进而确定了最佳萃取条件.结果表明,当样品相pH为2.5,中间相为甲苯,接收相为3μL 0.25 mol/L氢氧化钠溶液,搅拌速度为800r/min,萃取时间为50 min时,萃取效率最佳.在最佳萃取条件下,样品的回收率为76.4％,相对标准偏差为3.8％.%Trace diethylstilbestrol in urine samples was determined by combining hollow fiber membrane/liquid-phase microextraction with high performance liquid chromatography. The effects of donor phase pH, intermediate type, acceptor phase concentration, stirring rate, and extraction time on liquid-liquid-liquid tri-phase microextraction efficiency were investigated, and the optimal microextraction condition was established accordingly. Results indicate that, when toluene is used as the intermediate phase and 3 μL of 0. 25 mol/L NaOH solution as the acceptor phase, the best microextraction efficiency is obtained after 50 min of extraction under a stirring rate of 800 r/min. The recovery of the tested urine samples is 76. 4% and the relative standard deviation is 3. 8% under the optimized microextraction condition.
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