应用化学 ›› 2011, Vol. 28 ›› Issue (10): 1202-1207.DOI: 10.3724/SP.J.1095.2011.00658

• 研究论文 • 上一篇    下一篇

1-乙基-3-丁基苯并咪唑六氟化磷离子液体液相微萃取剂的制备与应用

申书昌*,李飞,郑建华   

  1. (齐齐哈尔大学分析测试中心 齐齐哈尔 161006)
  • 收稿日期:2010-11-05 修回日期:2010-12-31 出版日期:2011-10-10 发布日期:2011-10-10
  • 通讯作者: 申书昌,教授; Tel/Fax:0452-2738202; E-mail:sscfxzx@163.com; 研究方向:色谱分析样品前处理技术
  • 基金资助:
    黑龙江省教育厅科学技术研究项目(11531410)

Preparation of C4eBimPF6 Ionic Liquid and its Application as a liquid-phase microextraction extractant

SHEN Shuchang*, LI Fei, ZHENG Jianhua   

  1. (Analytical and Testing Center of Qiqihar University,Qiqihar 161006)
  • Received:2010-11-05 Revised:2010-12-31 Published:2011-10-10 Online:2011-10-10

摘要:

合成了1-乙基苯并咪唑(eBim)、1-乙基-3-丁基苯并咪唑溴(C4eBimBr)中间体和1-乙基-3-丁基苯并咪唑六氟化磷(C4eBimPF6)离子液体。 通过红外光谱和核磁共振波谱表征了各步反应产物的结构。 基于离子液体分散液相微萃取-高效液相色谱法分析了水中邻苯二甲酸辛酯(DOP)和邻苯二甲酸壬酯(DNP)。 考察了萃取温度、萃取时间和离子液体用量对DOP和DNP萃取效果的影响。 在1.0~10 μg/L范围内,DOP和DNP的色谱峰高与质量浓度分别呈线性关系,相关系数(r2)分别为0.984 7和0.987 2。 DOP和DNP的最低检出限分别为0.018和0.052 μg/L,加标回收率分别为94.3%~102%和93.5%~103%。

关键词: 苯并咪唑离子液体, 分散液相微萃取, 高效液相色谱法, 邻苯二甲酸酯

Abstract:

1-Ethylbenzimidazolium(eBim), 1-ethyl-3-butyl-benzimi dazoliumbromine(C4eBimBr) intermediates, and 1-ethyl-3-butyl-enzimidazoliumhexafluorophosphate(C4eBimPF6) ionic liquid were synthesized. The structures of the intermediates and the ionic liquid were analyzed with IR and nuclear magnetic resonance spectroscopies. An analytical method for the determination of dioctyl phthalate(DOP) and dinonyl phthalate(DIP) in water using ionic liquid-based microextraction coupled with high performance liquid chromatography was developed. The influence of the extraction parameters including the extraction temperature, extraction time, and amount of ionic liquid was investigated. In the range from 1.0~10 μg/L, the relationship between the peak height and concentration of DOP and DNP was linear, and the correlative coefficients were 0.9847 and 0.9872 respectively. The limits of detection of the DOP and DNP were 0.018 and 0.052 μg/L, recoveries of DOP and DNP were 94.3%~102% and 93.5%~103%, respectively.

Key words: Benzimidazole ionic liquid, dispersive liquid-phase microextraction, high performance liquid chromatography, phthalate

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