柱前荧光衍生脂肪醇的高效液相色谱分离及质谱鉴定  

Determination of aliphatic alcohols by high-performance liquid chromatography coupled to mass spectrometry (HPLC/MS) with fluorescence and atmospheric pressure chemical ionization (APCI) detection

作　　者：陈向明[1] 刘德胜[1] 

机构地区：[1]滨州医学院烟台校区药物化学教研室,烟台264003

出　　处：《分析试验室》2008年第10期76-79,共4页Chinese Journal of Analysis Laboratory

摘　　要：利用新型荧光试剂1,2-苯并-3,4-二氢咔唑-9-乙酸（BCAA）作为柱前衍生化试剂,以乙腈为溶剂,1-乙基-3-（3-二甲氨基丙基）环己碳二亚胺（EDAC）作为缩合剂,4-二甲氨基吡啶（DMAP）为催化剂,55℃下衍生反应25 min后获得稳定的荧光产物。在Eclipse XDB-C8色谱柱上,通过梯度洗脱对12种游离脂肪醇进行了分离和在线质谱定性。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,对洗发水（含十二烷基硫酸钠）中游离脂肪醇进行定性及测定。脂肪醇的线性回归相关系数大于0.9997,检出限在9.40-25.32 fmol。A simple and highly sensitive method based on the derivatization of aliphatic alcohols utilizing 1,2-benzo-3,4- dihydrocarbazole-9-acetic acid （BCAA） as the novel pre-column derivatization reagent followed by high-performance liquid chromatography with fluorescence detection and online mass spectrometric identification was developed. Optimum derivatization was obtained by the reaction of aliphatic alcohols with BCAA at 55℃ for 25min in the presence of EDAC and DMAP in acetonitrile solvent. The condition of derivation was mildness. Derivatives were sufficiently stable to be efficiently analyzed by high-performance chromatography without pretreatment. On a reversed-phase Eclipse XDB-Cs column, twelve kinds of aliphatic alcohol （C1 - C12 ） derivatives were separated in conjunction with a gradient elution with a good baseline resolution. The precise determination results of aliphatic alcohols from shampoo were obtained by postcolumn online mass spectrometric identification with atmospheric pressure chemical ionization（APCI） source under positive mode detection. The established method exhibited excellent reproducibility and sensitivity. Linear responses were observed with correlation coefficients above 0.9997, detection limits （at signal-to-noise of 3：1） 9.40- 25.32 fmol.

关 键 词：高效液相色谱-质谱 荧光检测 柱前衍生 脂肪醇 

分 类 号：O657.7[理学—分析化学]