摘要
以4-(9-吖啶酮)-甲基苯甲酰肼作为荧光衍生化试剂,在EclipseXDB-C8色谱柱上,梯度洗脱实现了9种游离脂肪酸(FFA)衍生物的完全基线分离。85℃下在乙腈溶剂中用N-乙基-N′-[(3-二甲氨基)丙基]碳二亚胺盐酸盐(EDC)做催化剂,衍生反应60min后获得稳定的荧光产物。使用荧光检测器,激发和发射波长分别为333nm和390nm。采用大气压化学电离源(APCI)正离子模式,实现了土壤中游离脂肪酸的质谱鉴定。所有脂肪酸的线性相关系数均大于0.9994,检出限为45.52～133.72fmol。
On a reversed-phase Eclipse XDB-C8 chromatographic column, 9 fatty acids were derivatized using 4（9-acridone ketone）-methyl benzoyl hydrazine （AMBH） as precolumn derivatization reagent and separated by HPLC in conjunction with a gradient elution with fluorescence detection and MS identification. Optimum derivatization, giving the corresponding stable fluorescent derivatives, was obtained by reacting of fatty acids with AMBH 85 ℃ for 60 min in the prescence of N-ethyl-N’-（3-dimethylamino propyl） carbodiimide hydorchloride （EDC） catalyst in acetonitrile. The fluorescence excitation and emission wave lengths of derivatives were λex=333 nm and λem=390 nm, respectively. The identification of fatty acid derivatives in soil was performed by the online APCI/MS （ atmospheric pressure chemical ion ization source） in positive mode. All linear correlation coefficients for fatty acid derivatives are over 0.999 94, and detection limits are 45.52～133.72 fmol （signal-to-noise o f 3：1）.
出处
《化学传感器》
CAS
2013年第2期59-63,共5页
Chemical Sensors
关键词
高效液相色谱-质谱
荧光检测器
柱前衍生
脂肪酸
high performance liquid chromatography/mass spectrometry
fluorescence detector
derivatization
fatty acids
