利用离子液体双水相萃取-高效液相色谱(HPLC)法测定了水中痕量氯酚类内分泌干扰物。以2,4-二氯酚(2,4-DCP)、2,6-二氯酚(2,6-DCP)和对氯苯酚(4-CP)为目标分析物,考察了影响离子液体双水相萃取率的主要因素,如分相盐的浓度、水相pH值、萃取时间及离子液体加入量。当NaH2PO4的浓度为0.5 g/mL,水相pH值为4,萃取时间为4 min,离子液体加入量为2 mL时,3种氯酚的萃取效率最高。取离子液体相直接进行HPLC分析,2,4-DCP,2,6-DCP和4-CP的检出限(S/N=3)分别为2、11和5μg/L。将本方法应用于自来水、湖水及工业废水中2,4-DCP,2,6-DCP和4-CP的检测,相对标准偏差(RSD)为1.2%~5.2%;加标回收率为90.2%~107%,结果令人满意。
Determination of trace chlorophenols endocrine disrupting chemicals in water sample was carried out by utilizing ionic liquid aqueous two-phase extraction systems coupled with high-perfor-mance liquid chromatography(HPLC).The effects of salt concentration,pH value of aqueous phase,extraction time and the amount of ionic liquid on extraction efficiency were investigated.The highest extraction efficiency for these three target analytes were obtained when concentration of NaH2PO4 aqueous,pH value,extraction time and the amount of ionic liquid were 0.5 g/mL,4.0,4 min and 2 mL,respectively.Ionic liquid phase was directly analyzed by HPLC with the detection limits of 2,11 and 5 μg/L(S/N=3) for 2,4-dichlorophenol,2,6-dichlorophenol and 4-chlorophenol,respectively.Good recovery results(90.2%-107.0%) with relative standard deviation ranging from 1.2% to 5.2%(n=5) were obtained when this method was applied to determine these three chlorophenols in tap water,lake water,waste water of chemical industry.