HPLC-APCI-MS Determination of Free Fatty Acids in Tibet Folk Medicine Lomatogonium rotatum with Fluorescence Detection and Mass Spectrometry Identification
会议名称：《首届中国中西部地区色谱学术交流会暨仪器展览会》
会议日期：2006年
学科分类：1008[医学-中药学(可授医学、理学学位)] 1006[医学-中西医结合] 081704[工学-应用化学] 07[理学] 08[工学] 0817[工学-化学工程与技术] 070302[理学-分析化学] 0703[理学-化学] 100602[医学-中西医结合临床] 10[医学]
关 键 词：HPLC-APCI-MS FFAs AETS fluorescence detection derivatization Lomatogonium rotatum
摘 要：A simple and sensitive method for the determination of free fatty acids (FFAs) using acridone-9-ethyl-p-toluenesulfonate (AETS) as fluorescence derivatization reagent by high-performance liquid chromatography (HPLC) has been developed. Free fatty acid derivatives were separated on Eclipse XDB-Cs column with a good baseline resolution and detected with the fluorescence which excitation and emission wavelengths of derivatives were set at λex=404 and λem=440nm, respectively. Identification of 19 fatty acid derivatives was carried out by online post-column mass spectrometry with atmospheric pressure chemical ionization (APCI) source under positive-ion detection mode. 19 FFAs from the extract of Lomatogonium rotation are sensitively determined. The results indicate that the plant Lomatogonium rotatum enriches an abundance of FFAs and FFAs of higher contents mainly focus on that of even carbon atoms C14, C16 and C18. The validation of the method including linearity, repeatability, and detection limits was examined. Most linear correlation coefficients for fatty acid derivatives are 0.9989, and detection limits (at signal-to-noise of 3:1) are 12.3-43.7 fmol. The relative standard deviations (RSDs) of the peak areas and retention times for 19 FFAs standards are 2.24 % and 0.45 %, respectively. The established method is rapid and reproducible for the separation determination of FFAs from the extract of Lomatogonium rotatum with satisfactory results.