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采用 HPLC 荧光检测和在线大气压化学电离质谱鉴定法,用双敏探针 1-咪唑-2-(5-苯并吖啶酮)-乙酮测定环境水中的胺。

Dual-sensitive probe 1-imidazole-2-(5-benzoacridine)-ethanone for the determination of amines in environmental water using HPLC with fluorescence detection and online atmospheric chemical ionization-mass spectrometry identification.

机构信息

Northwest Plateau Institute of Biology, Chinese Academy of Sciences, Xining 810001, PR China.

出版信息

Talanta. 2010 Jan 15;80(3):1392-9. doi: 10.1016/j.talanta.2009.09.041.

DOI:10.1016/j.talanta.2009.09.041
PMID:20006104
Abstract

Dual-sensitive probe of 1-imidazole-2-(5-benzoacridine)-ethanone (IBAE) for the determination of free amines with fluorescence detection and online highly sensitive atmospheric chemical ionization-mass spectrometry identification (APCI-MS) has been developed. 2-(Benzoacridine)-5-acetic acid (BAAA) reacts with coupling agent N,N'-carbonyldiimidazole (CDI) to form a highly activated amide intermediate 1-imidazole-2-(5-benzoacridine)-ethanone (IBAE), which is dual-sensitive probe. The amide intermediate (IBAE) reacts preferably with amines in dimethylformamide (DMF) solvent to give the high yields of derivatives. IBAE-amine derivatives are not only sensitive to fluorescence but also to MS ionizable efficiency. The percent ionization delta values change from 0 to 57.32% in aqueous acetonitrile and from 0 to 62.14% in aqueous methanol. The relative standard deviations of the peak areas with fluorescence detection for each amine are <1.24% (40ng/ml, n=6). The fluorescence detection limits (at a signal-to-noise ratio of 3) are in the range of 0.15-0.50ng/ml. The online APCI-MS detection limits are in the range of 2.07-8.51ng/ml (at a signal-to-noise ratio of 3). Therefore, the facile IBAE intermediate derivatization allowed the development of a highly sensitive and specific method for the quantitative analysis of trace levels of amines in environmental water.

摘要

已经开发出了一种用于测定游离胺的双敏探针,该探针由 1-咪唑-2-(5-苯并吖啶基)乙酮(IBAE)和荧光检测以及在线高灵敏度大气压化学电离质谱鉴定(APCI-MS)组成。2-(苯并吖啶基)-5-乙酸(BAAA)与偶联剂 N,N'-羰基二咪唑(CDI)反应,形成高度活化的酰胺中间物 1-咪唑-2-(5-苯并吖啶基)乙酮(IBAE),这是双敏探针。酰胺中间物(IBAE)在二甲基甲酰胺(DMF)溶剂中与胺优先反应,生成高收率的衍生物。IBAE-胺衍生物不仅对荧光敏感,而且对 MS 可离子化效率敏感。在水-乙腈中,离子化百分数 delta 值从 0 变化到 57.32%,在水-甲醇中,从 0 变化到 62.14%。每个胺的荧光检测峰面积的相对标准偏差均小于 1.24%(40ng/ml,n=6)。荧光检测的检出限(信噪比为 3)在 0.15-0.50ng/ml 范围内。在线 APCI-MS 检测限在 2.07-8.51ng/ml 范围内(信噪比为 3)。因此,简便的 IBAE 中间物衍生化允许开发出一种用于痕量胺在环境水中定量分析的高灵敏度和特异性方法。

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