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色谱

• 研究论文 • 上一篇    下一篇

三相中空纤维液相微萃取在羟基苯甲酸类化合物分析中的应用

朱颖, 陈璇, 郑飞浪, 白小红   

  1. School of Pharmaceutical Science, Shanxi Medical University, Taiyuan 030001, China
  • 收稿日期:2009-03-12 修回日期:2009-05-19 出版日期:2009-11-30 发布日期:1981-12-25
  • 通讯作者: 白小红

Application of three-phase hollow fiber liquid-phase microextraction for analysis of hydroxybenzoic acids

ZHU Ying, CHEN Xuan, ZHENG Feilang, BAI Xiaohong*   

  1. School of Pharmaceutical Science, Shanxi Medical University, Taiyuan 030001, China
  • Received:2009-03-12 Revised:2009-05-19 Online:2009-11-30 Published:1981-12-25
  • Contact: BAI Xiaohong

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摘要： 在优化的三相中空纤维液相微萃取(3p-HFLPME)条件下,研究了6种羟基苯甲酸类化合物(HBAs)的3p-HFLPME行为;揭示了HBAs的富集因子(EF)与其正庚醇/水条件分配系数(log Pn-heptanol/5 mmol/L HCl)、pKa和羟基数目(N)的相关性,初步阐明了聚偏氟乙烯中空纤维对HBAs的电荷转移传递机理以及有机溶剂对HBAs的选择性萃取机理。优化的3p-HFLPME条件: 以MOF 503聚偏氟乙烯中空纤维为有机溶剂支持体,正庚醇为有机相,5 mmol/L HCl体系为给体,80 mmol/L NH3·H2O为接受相,搅拌速度为1200 r/min,萃取35 min。该方法的精密度（以相对标准偏差计）小于3%,检出限为0.09~30.00 μg/L,加标回收率为93.3%~107.1%,HBAs质量浓度为5 mg/L时的富集因子最高达107.6倍。

关键词: 电荷转移化合物 , 富集因子, 聚偏氟乙烯中空纤维, 羟基苯甲酸, 三相中空纤维液相微萃取

Abstract: Under the optimal experimental conditions of three-phase hollow fiber liquid-phase microextraction (3p-HFLPME), the behaviors of hydroxybenzoic acids (HBAs) were investigated. The correlativities between the enrichment factor (EF) of HBAs and their n-heptanol/water conditional distribution coefficients (log Pn-heptanol/5 mmol/L HCl), pKa and the number of ~OH (N); the extraction mechanism that polyvinylidene difluoride hollow fiber contributed to promote the extraction efficiency by forming charge transfer compound with HBAs and the organic solvents showed notable selectivity for HBAs were elucidated. The optimal 3p-HFLPME conditions were: MOF 503 polyvinylidene difluoride hollow fiber as organic solvent supporter, n-heptanol as organic phase, 5 mmol/L HCl in the donor phase and 80 mmol/L NH3·H2O as the acceptor phase, the HBAs were extracted for 35 min under an agitation of 1200 r/min. It was found that the relative standard deviations were lower than 3%, the detection limits were 0.09~30.00 μg/L, the average recoveries of HBAs in Calyx Kaki were 93.3%~107.1% and the EF of HBAs at 5 mg/L was up to 107.6 fold.

Key words: charge transfer compound , enrichment factor, hydroxybenzoic acids, polyvinylidene difluoride hollow fiber, three-phase hollow fiber liquid-phase microextraction