采用五氟苯甲酰氯在注射器内衍生化后，通过气相色谱-质谱法测定脂肪胺。
Determination of aliphatic amines by gas chromatography-mass spectrometry after in-syringe derivatization with pentafluorobenzoyl chloride.
机构信息
Advanced Materials and Processes Research Institute, Bhopal 462026, India.
出版信息
J Chromatogr A. 2011 Aug 19;1218(33):5683-7. doi: 10.1016/j.chroma.2011.06.022. Epub 2011 Jun 17.
A simple and highly sensitive gas chromatographic method has been developed for the determination of low molecular weight short-chain aliphatic amines (SCAAs) after their simultaneous extraction and in-syringe derivatization with pentafluorobenzoyl chloride (PFBOC). Derivatization of the low molecular weight aliphatic amines in bicarbonate buffer of pH 10.5 with PFBOC was followed by immersed solvent microextraction. Derivatization conditions, including reagent concentration, reaction pH, ionic concentration of buffer, reaction time, stirring rate, reaction temperature and extraction solvent, have been investigated for method optimization. Linearity was studied within range of 0.15 pg ml⁻¹-50 ng ml⁻¹. The correlation coefficients were between 0.9934 and 0.9999. Detection limit of derivatized amines proved to be in the range of 0.117-1.527 pg ml⁻¹, and the intraday and interday relative standard deviation (RSD) values were less than 8% with respect to peak area. The method was applied for analysis of lake, river and industrial waste water. The recoveries of extraction from lake, river and industrial waste water samples, which have been spiked with different levels of aliphatic amines, were in the range of 68-99%, 63-102% and 62-105%, respectively.
已经开发出一种简单且高度灵敏的气相色谱法，用于在低分子量短链脂肪胺（SCAAs）经五氟苯甲酰氯（PFBOC）同时提取和注射器衍生后进行测定。在 pH 值为 10.5 的碳酸氢盐缓冲液中，PFBOC 将低分子量脂肪胺衍生化，然后进行浸入溶剂微萃取。对衍生化条件（包括试剂浓度、反应 pH 值、缓冲液的离子浓度、反应时间、搅拌速度、反应温度和萃取溶剂）进行了考察，以优化方法。在线性范围内为 0.15 pg ml⁻¹-50 ng ml⁻¹。相关系数在 0.9934 至 0.9999 之间。衍生化胺的检测限被证明在 0.117-1.527 pg ml⁻¹范围内，日内和日间相对标准偏差（RSD）值相对于峰面积小于 8%。该方法已应用于湖泊、河流和工业废水的分析。从已加入不同水平脂肪胺的湖泊、河流和工业废水样品中提取的回收率分别为 68-99%、63-102%和 62-105%。
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