HF-LPME-HPLC法测定水中4种邻苯二甲酸酯

Determination of 4 kinds of phthalate esters in water samples by hollow fibre liquid-phase micro-extraction and highly efficient liquid chromatography

研究建立一种中空纤维膜液相微萃取结合高效液相色谱(HF-LPME-HPLC)测定水中4种邻苯二甲酸酯(PAEs)的方法。考查了中空纤维膜的长度等参数对萃取效果的影响。结果表明,中空纤维膜长度为8 cm,1-丁基-3-甲基咪唑六氟磷酸盐([BMIm]PF6)为萃取剂,十二醇为支撑膜相,萃取时间为5 min时,萃取效果最好。该法中4种PAEs的线性范围为10~1 000 ng/m L(R2均大于0.999),检出限为1.67~7.38 ng/m L,相对标准偏差(RSD)为2.1%~5.7%(n=5)。实际样品测定中,加标回收率为89%~107%,因此,该法可用于水样中4种PAEs的测定。

A method for the determination of four kinds of phthalate esters（PAEs） by hollow fibre liquid-phase micro-extraction and highly efficient liquid chromatograph（HF-LPME-HPLC） has been developed and established.The influences of hollow fibre length and other factors on extraction effects have been investigated. The results show that the extraction effect is the best,when the length of hollow fibre membrane is 8 cm,1-butyl-3-methylimidazolium hexafluorophosphate（[BMIm]PF6） is used as extractant,1-dodecanol is used as membrane-supported phase,and extraction time 5 min. By this method,the linear relationship of the 4 kinds of PAEs is in the range of 10-1 000 ng/m L（R^2 are all higher than 0.999）,detection limits 1.67-7.38 ng/m L and relative standard deviations 2.1%-5.7%（n=5）. The labeled recovery rate of actual sample determination is in the range of 89%-107%,after spiked with PAEs.Therefore,this method could be applied to the determination of 4 kinds of PAEs in water samples.