Determination of carbonyls using liquid chromatography-mass spectrometry with atmospheric pressure chemical ionization
Determination of carbonyls using liquid chromatography-mass spectrometry with atmospheric pressure chemical ionization
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DOI：
10.1039/a902766a
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发表时间：
1999-08-01
影响因子：
--
通讯作者：
Karst, U
中科院分区：
文献类型：
--
作者：
Kempter, C;Zurek, G;Karst, U
描述了一种基于质谱检测的液相色谱测定醛和酮的方法。最近开发的模块化衍生剂用于分析。这些肼试剂，例如4-二甲氨基-6-(4-甲氧基-1-萘基)-1,3,5-三嗪-2-肼 (DMNTH) 与羰基化合物反应，形成相应的腙，并通过 HPLC-MS 在正离子模式下以常压化学电离进行分离。电喷雾电离也可用于分析。特别关注各种校准方法，包括使用标准溶液的外部校准和使用环丁酮腙标准品的内部校准，环丁酮是一种在实际样品中不太可能出现的醛。第二种内部校准方法是基于 C-13(2) 标记的乙醛腙标准品。然后可以使用不同的校准方法来分析真实样品。一系列腙的检测限范围为 2 x 10(-8) 至 5 x 10(-8) mol L-1，包括烷基链长度为 1 至 7 个碳原子的饱和醛腙、选定的不饱和醛和芳香醛腙以及酮腙。
A liquid chromatographic method for the determination of aldehydes and ketones based on mass spectrometric detection is described. Recently developed modular derivatizing agents are employed for analysis. These hydrazine reagents, e.g. 4-dimethylamino-6-(4-methoxy- 1-naphthyl)-1,3,5-triazine-2-hydrazine (DMNTH), react with the carbonyl compounds with the formation of the respective hydrazones, which are separated by HPLC-MS with atmospheric pressure chemical ionization in the positive mode. Electrospray ionization may also be used for analysis. Particular focus is directed on various calibration approaches, including external calibration with standard solutions and internal calibration with a hydrazone standard of cyclobutanone, an aldehyde not likely to occur in real samples. A second approach for internal calibration is based on the C-13(2)-labelled acetaldehyde hydrazone standard. Different calibration approaches may then be used for the analysis of real samples. Limits of detection range from 2 x 10(-8) to 5 x 10(-8) mol L-1 for a series of hydrazones, including hydrazones of saturated aldehydes with alkyl chain lengths from 1 to 7 carbon atoms, and hydrazones of selected unsaturated and aromatic aldehydes as well as ketone hydrazones.