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以吖啶酮-9-乙基对甲苯磺酸酯(AETS)作荧光衍生化试剂,建立了灵敏、简单的游离脂肪酸反相高效液相色谱测定方法。在Ec lipse XDB-C8色谱柱上,实现了19种游离脂肪酸(FFA)衍生物的完全基线分离。选取AETS摩尔数为脂肪酸的6倍,以DMF作溶剂,在85℃条件下以K2CO3作催化剂可获得稳定的荧光产物,条件温和、衍生产率高。利用柱后在线串联质谱以APC I大气压化学电离源正离子模式实现了各组分的质谱定性。对土壤和3种苔藓植物中(树藓、狭叶绢藓、曲尾藓)FFA组分定量结果表明,苔藓植物从土壤中富集了大量的游离脂肪酸。荧光检测的激发和发射波长分别为404 nm和440 nm。绝大多数脂肪酸的线性相关系数大于0.9996,检出限为12.3~43.7 fmol。本方法具有良好的重现性,用于实际样品测定,结果满意。
A sensitive and simple method for the determination of free fatty acids by reversed-phase high performance liquid chromatography was developed with acridone-9-ethyl-p-toluenesulfonate (AETS) as a fluorescent derivatization reagent. A complete baseline separation of 19 free fatty acid (FFA) derivatives was achieved on the Ec lipse XDB-C8 column. The molar ratio of AETS to fatty acid was 6 times, DMF as solvent and K2CO3 as catalyst at 85 ℃, the stable fluorescent product was obtained under mild conditions with high yield. The mass spectral characterization of each component was achieved by in-line tandem mass spectrometry using APC I atmospheric pressure chemical ionization source positive ion mode. Quantitative analysis of FFA components in soils and three bryophytes (Physcomitrella patens, Phaeophyceae, Tail moss) showed that bryophytes were enriched in large amounts of free fatty acids from soil. Fluorescence detection excitation and emission wavelengths were 404 nm and 440 nm. The linear correlation coefficient of most fatty acids was greater than 0.9996 with a detection limit of 12.3 ~ 43.7 fmol. The method has a good reproducibility, for the actual sample determination, the results are satisfactory.