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离子液体作为高效液相色谱-电化学检测中的流动相添加剂:应用于肉类婴儿食品中杂环芳香胺的测定。

Ionic liquids as mobile phase additives in high-performance liquid chromatography with electrochemical detection: application to the determination of heterocyclic aromatic amines in meat-based infant foods.

作者信息

Martín-Calero Aurora, Pino Verónica, Ayala Juan H, González Venerando, Afonso Ana M

机构信息

Department of Analytical Chemistry, Nutrition and Food Science, University of La Laguna, 38205 La Laguna, Spain.

出版信息

Talanta. 2009 Aug 15;79(3):590-7. doi: 10.1016/j.talanta.2009.04.032. Epub 2009 May 3.

Abstract

The beneficial effects of several ionic liquids (ILs) as mobile phase additives in high-performance liquid chromatography with electrochemical detection for the determination of six heterocyclic aromatic amines (HAs) have been evaluated for first-time. The studied ionic liquids were 1-butyl-3-methylimidazolium tetrafluoroborate (BMIm-BF(4)), 1-hexyl-3-methylimidazolium tetrafluoroborate (HMIm-BF(4)) and 1-methyl-3-octylimidazolium tetrafluoroborate (MOIm-BF(4)). Several chromatographic parameters have been evaluated in the presence or absence of ILs, or using ammonium acetate as the most common mobile phase additive, with three different C18 stationary phases. The effect of the acetonitrile content was also addressed. In general, best resolution, lower peak-widths (up to 72.1% lower) and lower retention factors are obtained when using ILs rather than ammonium acetate as mobile phase additives. The main improvement was obtained in the baseline noise, being 360% less noisy for BMIm-BF(4), 310% for HMIm-BF(4), and 227% for MOIm-BF(4), when compared to ammonium acetate at +1000 mV. Different chromatographic methods using the best conditions for each IL were also evaluated and compared. Finally, the best chromatographic conditions using 1mM of BMIm-BF(4) as mobile phase additive, the Nova-Pak C18 column, 19% (v/v) of acetonitrile content in the mobile phase, and +1000 mV in the ECD, have been applied for the chromatographic analysis of six HAs contained in meat-based infant foods. The whole extraction method of meat-based infant foods using focused microwave-assisted extraction and solid-phase extraction has also been optimized. Extraction efficiencies up to 89% and detection limits ranged between 9.30 and 0.165 ng g(-1) have been obtained under optimized conditions.

摘要

首次评估了几种离子液体(ILs)作为高效液相色谱电化学检测中流动相添加剂用于测定六种杂环芳香胺(HAs)的有益效果。所研究的离子液体为1-丁基-3-甲基咪唑四氟硼酸盐(BMIm-BF₄)、1-己基-3-甲基咪唑四氟硼酸盐(HMIm-BF₄)和1-甲基-3-辛基咪唑四氟硼酸盐(MOIm-BF₄)。在有或没有离子液体的情况下,或者使用乙酸铵作为最常用的流动相添加剂时,使用三种不同的C18固定相评估了几个色谱参数。还探讨了乙腈含量的影响。总体而言,与使用乙酸铵作为流动相添加剂相比,使用离子液体时可获得最佳分离度、更低的峰宽(降低幅度高达72.1%)和更低的保留因子。主要改进在于基线噪声,与在+1000 mV时的乙酸铵相比,BMIm-BF₄的噪声降低360%,HMIm-BF₄降低310%,MOIm-BF₄降低227%。还评估并比较了针对每种离子液体使用最佳条件的不同色谱方法。最后,以1 mM的BMIm-BF₄作为流动相添加剂、Nova-Pak C18柱、流动相中乙腈含量为19%(v/v)以及在电化学检测器中为+1000 mV的最佳色谱条件,已应用于肉基婴儿食品中六种杂环芳香胺的色谱分析。还优化了使用聚焦微波辅助萃取和固相萃取的肉基婴儿食品的整个萃取方法。在优化条件下获得了高达89%的萃取效率,检测限在9.30至0.165 ng g⁻¹之间。

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