Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore.
J Chromatogr A. 2013 Nov 22;1317:217-22. doi: 10.1016/j.chroma.2013.04.014. Epub 2013 Apr 12.
Ionic liquid-dispersive liquid-liquid microextraction combined with micro-solid phase extraction (IL-DLLME-μ-SPE), and high-performance liquid chromatography (HPLC) was developed for the determination of tricyclic antidepressants (TCAs) in water samples. Two hundred microliters of an organic solvent (as disperser solvent) and 20 μl of 1-hexyl-3-methylimidazolium tris(pentafluoroethyl)trifluorophosphate were injected into a 5.0 ml sample for sonication-assisted DLLME. After this, a μ-SPE device, containing a novel material zeolite imidazolate framework 4 (ZIF-4), was added into the sample solution and 1 min of vortex-assisted extraction was performed. After 5 min of sonication-assisted desorption, 10 μl of desorption solvent was injected into a HPLC system for analysis. A characteristic property of DLLME-VA-μ-SPE is that any organic solvent and solid sorbent immiscible with water can be used. Special apparatus, or conical-bottom test tubes, and tedious procedures conventionally associated with DLLME such as centrifugation, or refrigeration of solvent are not necessary in the present approach. A novel material, ZIF-4 was employed as μ-SPE sorbent. Under the optimized conditions, the calibration curves were linear in the range of 1-1000 μg/L. The relative standard deviations and the limits of detection were in the range of 1.5% and 7.8% and 0.3 and 1 μg/L, respectively. The relative recoveries of canal water samples, spiked with drugs, were in the range of 94.3% and 114.7%. The results showed that IL-DLLME-μ-SPE was suitable for the determination of TCAs in water samples.
离子液体分散液液微萃取结合微固相萃取(IL-DLLME-μ-SPE),与高效液相色谱(HPLC)相结合,用于测定水样中的三环类抗抑郁药(TCAs)。将 200μL 有机溶剂(作为分散溶剂)和 20μL 1-己基-3-甲基咪唑六氟磷酸盐注入 5.0ml 样品中,进行超声辅助 DLLME。之后,将一种新型材料沸石咪唑酯骨架 4(ZIF-4)的 μ-SPE 装置加入到样品溶液中,并进行 1 分钟的涡旋辅助萃取。超声辅助解吸 5 分钟后,将 10μL 解吸溶剂注入 HPLC 系统进行分析。DLLME-VA-μ-SPE 的一个特点是可以使用任何与水不混溶的有机溶剂和固体吸附剂。本方法不需要 DLLME 通常需要的特殊仪器或锥形底试管,以及繁琐的溶剂离心或冷藏程序。新型材料 ZIF-4 被用作 μ-SPE 吸附剂。在优化条件下,校准曲线在 1-1000μg/L 范围内呈线性。相对标准偏差和检出限分别在 1.5%和 7.8%以及 0.3 和 1μg/L 的范围内。加标运河水样的相对回收率在 94.3%和 114.7%之间。结果表明,IL-DLLME-μ-SPE 适用于水样中 TCAs 的测定。