摘要
在HypersilODS2色谱柱上,利用新型荧光试剂1,2-苯并-3,4-二氢咔唑-9-乙基肼基甲酸酯(BCEC)作柱前衍生化试剂,采用梯度洗脱对5种中性糖荧光衍生物进行了优化分离.65℃下在乙腈溶剂中以冰乙酸作催化剂,衍生反应6.5h后获得稳定的荧光产物,衍生反应完全.激发和发射波长分别为λex=333nm,λem=390nm.线性回归系数均在0.999以上,检测限为24.3~62.1fmol.
On a reversed -phased Hypersil ODS2 column, using the novel fluorescence reagent 1, 2 - benzo-3, 4-dihydrocarbazole-9-ethyl-carbonylhydazine (BCEC) as pre-column derivatization reagent, 5 neutral saeeharide derivatives were successively separated with a good baseline resolution by high per- formanee liquid chromatography in conjunction with a gradient elution. The optimum derivatization was obtained by the reaction of neutral saccharides with BCEC at 65℃ in acetonitrile for 6.5 h in the pres- ence of acetic acid. The fluorescence excitation and emission wavelengths were set at λex333 and λcm 390 nm, respectively. Correlation coefficients for neutral saccharide derivatives are 〉0.999, and the detection limits ( at signal to noise of 3: 1) are 24.3 - 62.1 fmol for the labeled neutral saccharides.
出处
《化学研究》
CAS
2007年第4期62-65,共4页
Chemical Research
基金
国家自然科学基金资助项目(20075016)
关键词
HPLC
荧光检测
柱前衍生
糖类化合物
HPLC
fluorescence detection
pre-column derivatization
saccharide