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Free Amino Acid Analysis in Honey Samples by Hydrophilic Interaction Liquid Chromatography with UV Detection Using Precolumn Derivatization with Dansyl Chloride
Chromatographia ( IF 1.7 ) Pub Date : 2021-01-03 , DOI: 10.1007/s10337-020-03991-z
Ertuğ Kırkan , Cemil Aydoğan

A new hydrophilic interaction chromatography (HILIC) method was developed for free amino acid analysis in honey samples after pre-column derivatization of amino acids with dansyl chloride (Dns-Cl). This method consisted of the sample pretreatment with a modified QuEChERS extraction and liquid chromatographic analysis with UV detection. The derivatized amino acids were separated on a HILIC column (NH 2 -HILIC 150 × 4.6 mm). The separation of 9 derivatized amino acids was successfully achieved with gradient elution. The derivatization process allowed high sensitivity for the amino acids while the rapid analysis in the HILIC mode within 17 min of elution time was obtained. Full separation and determination of the Dns-amino acids were achieved in relevant honey samples. Mean percentage recoveries of Dns-amino acids from the samples were 82.4% or higher with a good standard deviation of < 4%.

中文翻译:

使用柱前衍生化丹磺酰氯通过亲水相互作用液相色谱结合紫外检测分析蜂蜜样品中的游离氨基酸

开发了一种新的亲水相互作用色谱 (HILIC) 方法,用于分析用丹磺酰氯 (Dns-Cl) 对氨基酸进行柱前衍生化后的蜂蜜样品中的游离氨基酸。该方法包括使用改进的 QuEChERS 萃取进行样品预处理和使用 UV 检测的液相色谱分析。衍生的氨基酸在 HILIC 柱(NH 2 -HILIC 150 × 4.6 mm)上分离。通过梯度洗脱成功实现了 9 种衍生氨基酸的分离。衍生化过程允许对氨基酸具有高灵敏度,同时在洗脱时间的 17 分钟内在 HILIC 模式下获得快速分析。在相关蜂蜜样品中实现了Dns-氨基酸的完全分离和测定。样品中 Dns-氨基酸的平均回收率为 82。
更新日期:2021-01-03
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