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Determination of free fatty acids from soil by LC-MS with fluorescence detection and atmospheric pressure chemical ionization identification

机译:液相色谱-质谱联用荧光检测-常压化学电离识别法测定土壤中的游离脂肪酸

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摘要

A simple and highly sensitive method for the determination of fatty acids using liquid chromatography with fluorescence detection is described. Fatty acids were derivatized by a new novel pre-column derivatization reagent 1,2-benzo-3,4-dihydrocarbazole-9-ethanol before injection. Derivatives were sufficiently stable for efficient analysis by LC without pre-treatment. On a reversed-phase XDB-C_8 column, 19 kinds of fatty acids (C _1-C_(19)) derivatives were separated in conjunction with gradient elution and good baseline resolution. The precise determination of fatty acids from soil sample was achieved by post-column online mass spectrometric identification with atmospheric pressure chemical ionization source in positive mode. The established method exhibited good selectivity and excellent repeatability. The RSD (n = 6) for each fatty acid derivative were <3%, detection limits (at signal-to-noise of 3:1) were 11.79-33.04 fmol.
机译:描述了一种使用液相色谱和荧光检测法测定脂肪酸的简单且高度灵敏的方法。注射前,用新的新型柱前衍生试剂1,2-苯并-3,4-二氢咔唑-9-乙醇对脂肪酸进行衍生。衍生物足够稳定,无需进行预处理即可通过LC进行有效分析。在反相XDB-C_8色谱柱上,结合梯度洗脱和良好的基线分辨率,分离了19种脂肪酸(C _1-C_(19))衍生物。通过柱后在线质谱鉴定和正压大气化学电离源可实现对土壤样品中脂肪酸的精确测定。所建立的方法表现出良好的选择性和优异的可重复性。每种脂肪酸衍生物的RSD(n = 6)小于3%,检出限(信噪比为3:1)为11.79-33.04 fmol。

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