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利用新型荧光试剂1,2-苯并-3,4-二氢咔唑-9-乙基氯甲酸酯(BCEOC)作为柱前衍生化试剂,在EclipseXDB-C8色谱柱上,梯度洗脱对12种游离脂肪胺进行了优化分离。40℃下在乙腈溶剂中以硼酸盐缓冲溶液作催化剂,衍生反应10min后获得稳定的荧光产物。激发和发射波长分别为λex=333nm,λem=390nm。采用大气压化学电离源(APCI)正离子模式,实现了土壤和造纸污水中脂肪胺的定性测定。采用荧光法进行分析物的定量测定。多数脂肪胺的线性回归系数大于0.999,检出限在18.65~38.82×10-15mol。方法具有稳定良好的重现性,对实际样品测定结果满意。
A novel fluorescent reagent, 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate (BCEOC), was used as a pre-column derivatization reagent on EclipseXDB-C8 column. 12 kinds of free fatty amine were optimized. Borate buffer solution was used as a catalyst in acetonitrile solvent at 40 ℃ for 10min to obtain a stable fluorescent product. Excitation and emission wavelengths were λex = 333 nm, λem = 390 nm, respectively. Atmospheric pressure chemical ionization (APCI) positive ion mode was used to achieve the qualitative determination of fatty amines in soil and papermaking wastewater. Quantitative determination of analyte by fluorescence method. The linear regression coefficients of most fatty amines were greater than 0.999 and the detection limits were between 18.65 and 38.82 × 10-15 mol. The method has stable and good reproducibility and is satisfactory to the actual sample measurement results.