高效液相色谱-荧光光度测定及质谱鉴定酒中脂肪醛  

HPLC-Fluorimetric Determination and Mass Spectrometric Detection of Fatty Aldehydes in Wine

作　　者：张海峰[1] 刘凌君[2] 王影影[2] 尤进茂[2] 

机构地区：[1]济宁师范专科学校化学系,曲阜273155 [2]曲阜师范大学化学科学学院,曲阜273165

出　　处：《理化检验（化学分册）》2007年第8期617-620,631,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家自然科学基金资助项目(20075016)

摘　　要：合成了一种新的荧光试剂[1,2-苯并-3,4-二氢咔唑-9-乙基肼基甲酸酯(以下简写作BCEC)]并在酒中脂肪醛高效液相色谱(HPLC)分离及测定中作为柱前衍生试剂。衍生反应在乙腈溶剂中,用三氯乙酸作催化剂并在60℃条件下进行,并能在10 min后获得稳定的荧光产物。用Zorbax Eclipse XDB C8(4.6 mm×150 mm,5μm)作色谱柱,并以不同浓度的乙腈-水溶液作流动相进行梯度淋洗。采用荧光检测,检测的激发波长为333 nm,发射波长为390 nm。采用在线质谱检测对10种脂肪醛进行定性鉴定,醛的物质的量在0.166 5～83.3 fmol之间与其色谱峰面积呈线性关系,相关系数均优于0.999 9,被测各醛的检出限(S/N=3)在3.75～16.65 fmol之间。A new fluorescence reagent, 1,2-benzo-3,4-dihydrocarbazole-9-ethylcarbonylhydrazine （abbreviated as BCEC here after） was synthesized and used as pre-column derivatization reagent in the HPLC separation and determination of fatty aldehydes in wine. Stable fluorescence products were obtained in 10 min by the reaction in acetonitrile solvent with trichloroacetic acid as catalyst at 60 ℃. The Zorbax Eclipse XDB C4 chromatographic col- umn （4. 6 min× 150 mm, 5 μm） was used in HPLC, with gradient elution using acetonitrile water solution （pH 3.5） as moblie phase. Fluorimetric detection was made at 333 nm （λex） and 390 nm （λem）On-line mass spectrometric identification of the aldehydes was made with positive iron model of APCI source. Linear relationship between the chromatographic peak area and concentration of the aldehydes in the range of 0. 166 5-81.3 fmol, with correlation coefficients around 0. 999 9. Detection limits of the aldehydes were in the range of 3.75-16. 65μmol. tiom

关 键 词：高效液相色谱 荧光检测 质谱鉴定 柱前衍生 脂肪醛 酒 

分 类 号：O657.37[理学—分析化学]