Development of a gas chromatography mass spectrometry method for the analysis of aminoglycoside antibiotics using experimental design for the optimisation of the derivatisation reactions
Development of a gas chromatography mass spectrometry method for the analysis of aminoglycoside antibiotics using experimental design for the optimisation of the derivatisation reactions
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DOI：
10.1016/s0021-9673(98)00537-8
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发表时间：
1998-08-28
影响因子：
4.1
通讯作者：
Petz, M
中科院分区：
文献类型：
--
作者：
Preu, M;Guyot, D;Petz, M
用于分析氨基糖苷类抗生素卡那霉素和庆大霉素的填充柱 GC 电子捕获检测方法适用于毛细管 GC-MS。使用两步程序对分析物进行衍生化，包括用三甲基甲硅烷基咪唑对羟基进行三甲基甲硅烷基化以及用七氟丁酰咪唑对氨基进行酰化。给出并解释了所得卡那霉素A和庆大霉素C-1、C-1a和C-2衍生物的电子轰击质谱。使用实验设计优化衍生化程序。这种化学计量方法考虑了主要影响以及影响参数的相互作用，因此比常见的分步方法对该方法进行了更彻底的研究。使用分数阶乘和 Box Behnken Designs 进行优化产生了一种衍生方法，其产率比之前公布的方法更高，同时在许多情况下需要更少的试剂和更短的反应时间。 (C) 1998 Elsevier Science B.V. 保留所有权利。
A packed column GC-electron-capture detection method for the analysis of the aminoglycoside antibiotics kanamycin and gentamicin was adapted to capillary GC-MS. The analytes were derivatised using a two-step procedure involving trimethylsilylation of the hydroxyl groups with trimethylsilylimidazole and acylation of the amino groups with heptafluorobutyrylimidazole. Electron impact mass spectra of the resulting derivatives of kanamycin A and gentamicins C-1, C-1a and C-2 are given and interpreted. The derivatisation procedure was optimised using experimental design. This chemometrical approach considers main effects as well as interactions of the influential parameters, thus conducting a more thorough investigation of the method than the common step-by-step approach. Optimisation using fractional factorial and Box Behnken Designs produced a derivatisation method featuring better yield than previously published methods while in many cases requiring less reagents and shorter reaction times. (C) 1998 Elsevier Science B.V. All rights reserved.