土壤和水中脂肪胺的高效液相色谱荧光测定及质谱鉴定  

Determination of aliphatic amines in solid and waste water samples by high-performance liquidchromatography/atmospheric pressure chemical ion-ization( APCI)-mass spectrometry and fluoremetry

作　　者：石运伟[1] 张海峰[1] 程燕[1] 白敏[1] 赵先恩[1] 陈向明[1] 尤进茂[1] 

机构地区：[1]曲阜师范大学化学科学学院

出　　处：《分析试验室》2005年第8期42-47,共6页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金资助项目(20075016)

摘　　要：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Eclipse XDB-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=333 nm,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.On a reverse-phase Eclipse XDB-C8 column, using the novel fluorescence reagent 1,2-benzo-3,4-dihydrocarbazole-9-ethyl chloroformate （BCEOC） as a precolumn derivatization reagent, C1 - C12 aliphatic amine derivatives were optimally separated with a good baseline resolution by high-performance liquid chromatography in conjunction with a gradient elution. The optimal derivatization was obtained by the reaction of aliphatic amines with BCEOC at 40 ~C in acetonitrile solvent for 10 min in the presence of basic catalyst sodium borate, and the derivatives were stable and able to be directly analyzed without pretreatment. The fluorescence excitation and emission wavelengths were set at λex = 333 nm and λem = 390 nm, respectively. The qualitative analysis of aliphatic amine derivatives from soil and wastewater samples was accomplished by post-column mass spectrum with atmospheric pressure chemical ionization （APCI） source detection under positive mode. Quantitative determination of the analytes was achieved by means of fluorescence detection. The established method has excellent reproducibilities and recoveries. The correlation coefficients for aliphatic amine derivatives are 〉 0. 999, and the detection limits （ signal ： noise and 3 ： 1 ） are 18.65 - 38.82 x 10^-15 mol for the labeled aliphatic amines.

关 键 词：高效液相色谱-质谱 荧光检测 柱前衍生:脂肪胺 

分 类 号：O658.1[理学—分析化学]