Abstract

In this paper, we evaluated the use of a silylation reagent N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide in the microwave-assisted derivatization method to replace a traditional prolonged heating method for the determination of 12 amino acids. Several parameters, including the kind of extraction solvent, extraction time, microwave power and microwave time, were optimized. The experiment showed that the optimal derivatization time was 3 min with a microwave power of 240 W. The calibration curves were linear with the correlation coefficients ranging from 0.995 to 1.000 in the concentration levels between 0.1–20 μg/mL and the relative standard deviations were between 4.4 and 18%. The limits of detection were 0.1–2.4 μg/mL and the recoveries of those compounds were 62–115%. A comparison of this method to other methods has demonstrated that the proposed method is a rapid and reliable sample-treatment procedure for amino acids determination in real tobacco samples.

中文翻译：

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气相色谱-质谱法测定烟草中氨基酸的衍生化方法

摘要

在本文中，我们评估了甲硅烷基化试剂N-甲基-N-（叔-丁基二甲基甲硅烷基）三氟乙酰胺在微波辅助衍生化方法中代替了传统的长时间加热方法来测定12个氨基酸。优化了几种参数，包括萃取溶剂的种类，萃取时间，微波功率和微波时间。实验表明，最佳衍生时间为3分钟，微波功率为240W。校准曲线呈线性关系，浓度水平在0.1–20μg/ mL之间时，相关系数为0.995至1.000，相对标准偏差为在4.4％和18％之间。检测限为0.1–2.4μg/ mL，这些化合物的回收率为62–115％。