色谱

色谱 ›› 2013, Vol. 31 ›› Issue (2): 155-161.DOI: 10.3724/SP.J.1123.2012.09003

• 技术与应用 • 上一篇    下一篇

超声辅助分散液液微萃取-高效液相色谱测定水样中的4种邻苯二甲酸酯类增塑剂

马燕玲1,2, 陈令新1,2*, 丁养军1, 明永飞3, 李金花2   

  1. 1. 曲阜师范大学化学与化工学院, 山东 曲阜 273165; 2. 中国科学院烟台海岸带研究所, 中国科学院海岸带环境过程重点实验室, 山东 烟台 264003; 3. 鲁东大学生命科学学院, 山东 烟台 264025
  • 收稿日期:2012-09-03 修回日期:2012-10-11 出版日期:2013-02-28 发布日期:2013-02-05
  • 通讯作者: 李金花
  • 基金资助:

    国家自然科学基金项目(21275158, 21105117)；山东省自然科学基金项目(ZR2010BQ027)；山东省优秀中青年科学家奖励基金项目(BS2009CL055)；烟台市科技发展项目(2010158).

Simultaneous determination of four phthalate esters in water samples using ultrasound-assisted dispersive liquid-liquid microextraction coupled with high performance liquid chromatography

MA Yanling1,2, CHEN Lingxin1,2*, DING Yangjun1, MING Yongfei3, LI Jinhua2   

  1. 1. College of Chemistry and Chemical Engineering, Qufu Normal University, Qufu 273165, China; 2. Key Laboratory of Coastal Zone Environmental Processes, Yantai Institute of Coastal Zone Research, Chinese Academy of Sciences, Yantai 264003, China; 3. College of Life Science, Ludong University, Yantai 264025, China
  • Received:2012-09-03 Revised:2012-10-11 Online:2013-02-28 Published:2013-02-05
  • Contact: Jin-Hua LI

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438

被引次数

117

摘要： 建立了采用超声辅助分散液液微萃取技术结合高效液相色谱法(UA-DLLME-HPLC)对4种邻苯二甲酸酯(PAEs)进行富集、检测的方法,并成功应用于实际水样分析。实验中采用富集因子来评价萃取效率,考察并优化了影响萃取效率的主要因素,包括萃取剂类型和用量、分散剂类型和用量、超声时间、离子强度、萃取时间和pH值等。结果表明: 在最佳萃取条件下,该法对4种PAEs（邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯和邻苯二甲酸二正辛酯）具有较高的富集能力,富集因子分别为71、144、169和159;检出限分别为3.78、1.77、3.07和3.30 μg/L。对实验室自来水、某品牌矿泉水以及湖水分别加标50、200及500 μg/L的回收率为82.99%～114.47%,相对标准偏差为1.93%～8.31%。该法简便、快速、环保,可以用于测定实际水样中的PAEs类增塑剂。

关键词: 超声辅助, 分散液液微萃取, 高效液相色谱, 邻苯二甲酸酯, 水样

Abstract: Ultrasound-assisted dispersive liquid-liquid microextraction coupled with high performance liquid chromatography(UA-DLLME-HPLC)was developed for the determination of four typical phthalate esters (PAEs). The analyzed PAEs included dimethyl phthalate(DMP), diethyl phthalate(DEP), dibutyl phthalate(DBP)and di-n-octyl phthalate(DnOP). The UA-DLLME parameters such as types/volumes of extraction/dispersion solvents, ultrasonic time, ionic strength and extraction time, were investigated. Enrichment factor (EF)was employed to evaluate the extraction efficiency. The conditions were finally chosen: CCl4 (40 μL)/acetonitrile (1.0 mL) as extraction/dispersion solvents; 30 g/L NaCl; ultrasound/centrifugation of 5 min. Under the optimized extraction conditions, UA-DLLME exhibited strong enrichment ability for the four PAEs. The EFs for DMP, DEP, DBP and DnOP obtained were 71, 144, 169 and 159, respectively. The limits of detection were 3.78, 1.77, 3.07 and 3.30 μg/L for DMP, DEP, DBP and DnOP, respectively. The satisfactory recoveries for three water samples at three spiked levels ranged from 82.99%-114.47%, with the relative standard deviations of 1.93%-8.31%. It is a convenient, speedy, environmentally benign method for the routine analysis of PAEs in water samples.

Key words: high performance liquid chromatography (HPLC), phthalate esters (PAEs), ultrasound-assisted (UA), water sample, dispersive liquid-liquid microextraction (DLLME)