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首页> 外文期刊>Applied Magnetic Resonance >~(19)F-NMR Analysis of Primary and Secondary Amines Following Chemical Derivatization with Trifluoroacetic Anhydride
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~(19)F-NMR Analysis of Primary and Secondary Amines Following Chemical Derivatization with Trifluoroacetic Anhydride

机译：三氟乙酸酐化学衍生化后的伯胺和仲胺的〜（19）F-NMR分析

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摘要

Five amines were reacted with trifluoroacetic anhydride (TFAA) as derivatization reagent and subsequently analyzed via ~(19)F nuclear magnetic resonance (NMR) spectroscopy. The ~(19)F-NMR spectra of derivatives of aniline, 2,4-dimethyl aniline, and 2-methoxy aniline produce a signal that are very close to TFAA. The peaks resulting from the reaction of TFAA with N-ethyl aniline and N-methyl aniline are shifted much farther downfield than any of the other signals. Optimal ~(19)F-NMR sensitivity based upon T _1 relaxation time was investigated for derivatization compound and flurbiprofen as internal standard in toluene. The calibration curve was linear for amines over the range of 9.0-100.0 mg L ~(-1), with detection limit (S/N = 3) of 2.6-2.9 mg L ~(-1). Solid-phase extraction cartridges were investigated for preconcentration of water samples. The method was validated through spike and recovery for secondary amines from tap water sample.
机译：将五种胺与三氟乙酸酐（TFAA）作为衍生试剂反应，随后通过〜（19）F核磁共振（NMR）光谱进行分析。苯胺，2,4-二甲基苯胺和2-甲氧基苯胺的衍生物的〜（19）F-NMR光谱产生非常接近TFAA的信号。 TFAA与N-乙基苯胺和N-甲基苯胺反应产生的峰比其他任何信号都向远处偏移更远。研究了基于T _1弛豫时间的最佳〜（19）F-NMR灵敏度，用于衍生化化合物和氟比洛芬作为甲苯的内标。胺的校准曲线在9.0-100.0 mg L〜（-1）范围内呈线性，检出限（S / N = 3）为2.6-2.9 mg L〜（-1）。研究了固相萃取柱对水样品的预浓缩。通过加标和回收自来水样品中的仲胺对方法进行了验证。

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