On-line determination of carboxylic acids, aldehydes and ketones by high-performance liquid chromatography-diode array detection-atmospheric pressure chemical ionisation mass spectrometry after derivatization with 2-nitrophenylhydrazine
On-line determination of carboxylic acids, aldehydes and ketones by high-performance liquid chromatography-diode array detection-atmospheric pressure chemical ionisation mass spectrometry after derivatization with 2-nitrophenylhydrazine
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DOI：
10.1016/j.chroma.2003.10.100
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发表时间：
2004-03-26
影响因子：
4.1
通讯作者：
Van der Wal, S
中科院分区：
文献类型：
--
作者：
Peters, R;Hellenbrand, J;Van der Wal, S
2-硝基苯肼 (2-NPH) 广泛用于工业和生物样品中羧酸、醛和酮的衍生化。这些化合物与 2-NPH 反应形成衍生物，通过高效液相色谱 (HPLC) 进行分离，并通过二极管阵列检测 (DAD) 进行检测。紫外光谱提供有关化合物功能的信息：羧酸或酮/醛。 “已知”样品中的大多数洗脱化合物可以通过 2-NPH 衍生物的保留时间（与标准品相比）及其 UV 光谱来很好地表征。基于保留时间和/或紫外光谱来鉴定工业或生物样品中不同的未知的羧酸、酮和/或醛的2-NPH衍生物是不够的。这些未知的 2-NPH 化合物可以根据分子质量或/和衍生物的碎片，通过在线大气压化学电离质谱 (APCI-MS) 进行鉴定。描述了一种新颖且特异的在线 HPLC-DAD-APCl(-)-MS 方法，用于在用 2-NHP 在线柱前衍生化后测定羧酸、酮和醛。研究了不同 2-NPH 衍生物的裂解情况，并通过在线鉴定未知衍生物证明了 APCI(-)-MS 检测的可能性，该衍生物是 1-乙基-3(3-二甲基氨基丙基)碳二亚胺盐酸盐与 2-NPH 在样品溶液中存在高浓度环状反肽时产生的副产物。 (C) 2003 Elsevier B.V. 保留所有权利。
2-Nitrophenylhydrazine (2-NPH) is widely used for the derivatization of carboxylic acids, aldehydes and ketones, in industrial and biological samples. These compounds react with 2-NPH to form derivatives, which are separated by high-performance liquid chromatography (HPLC) and detected with diode array detection (DAD). The UV spectra give information about the functionality of the compounds: carboxylic acid or ketone/aldehyde. Most of the eluting compounds in "known" samples are well characterised by the retention time (comparison with those of standards) of the 2-NPH derivative and their UV spectrum. The identification of different unknown 2-NPH derivatives of carboxylic acids, ketones and/or aldehydes, in industrial or biological samples, based on retention time and/or UV spectrum is not sufficient. These unknown 2-NPH compounds can be identified with on-line atmospheric pressure chemical ionisation mass spectrometry (APCI-MS) based on the molecular mass or/and the fragmentation of the derivative. A novel and specific on-line HPLC-DAD-APCl(-)-MS method is described for the determination of carboxylic acids, ketones and aldehydes, after on-line pre-column derivatization with 2-NHP. The fragmentation of different 2-NPH derivatives were investigated and the possibilities of APCI(-)-MS detection were demonstrated by the on-line identification of an unknown derivative, which turned out to be a side product between 1-ethyl-3(3-dimethylaminopropyl)carbodiimide hydrochloride and 2-NPH in the presence of high concentrations of a cyclic an-tide in the sample solution. (C) 2003 Elsevier B.V. All rights reserved.