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
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,5 μm)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.
荧光检测
质谱鉴定
柱前衍生
脂肪醛
酒
High-performance liquid chromatography
Fluorimetric detection
Mass spectrometric identification
Precolumn derivatization
Fatty aldehydes
Wine
Abstract
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 C8 chromatographic column (4.6 mm×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 3.75-16.65 fmol.
中图分类号 O657.37
所属栏目 试验与研究
基金项目 国家自然科学基金资助项目(20075016)
收稿日期 2006/1/19
修改稿日期
网络出版日期
作者单位点击查看
备注张海峰(1978-),男,山东济宁人,硕士研究生,主要从事荧光试剂开发及色谱分析.
引用该论文: ZHANG Hai-feng,LIU Ling-jun,WANG Ying-ying,YOU Jin-mao. HPLC-Fluorimetric Determination and Mass Spectrometric Detection of Fatty Aldehydes in Wine[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2007, 43(8): 617～620
张海峰,刘凌君,王影影,尤进茂. 高效液相色谱-荧光光度测定及质谱鉴定酒中脂肪醛[J]. 理化检验－化学分册, 2007, 43(8): 617～620
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参考文献
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【3】Gamiz-Gracia L,Luque de Castro M D.Determination of formaldehyde in liquid,solid and semisolid pharmaceuticals and cosmetics by flow injection-pervaporation[J].Analyst,1999,124:1119-1121．
【4】Zhan X Q,Li D H,Zhu Q Z.et al.Sensitive fluorimetric determination of formaldehyde by the co-quenching effect of formaldehyde and sulfite on the fluorescence of tetra-substituted amino aluminium phthalocyanine[J].Analyst,2000,125:1330-2334．
【5】Darlene M,Persson P,Skarping G.Determination of Formatdehyde in Air bu Chemisorption on Glass Filters Impregnated with 2,4-Dinitrophenylhydrazine Using Gas Chromatography with Therionmic Specific Detection[J].J Chromatogr,1992,626:284-288．
【6】Magin D F.Preparation and Gag Chromatographic Characterization of Benzyloximes and p-Nitrobenzyoximes of Short-Chian (C1-C7) Carbonyls[J].J Chromatogr,1979,178:219-227．
【7】Magin D F.Gas Chromatography of Simple Monocarbonyls in Cigarette Whole Smoke as the Benzyloxime Derivatives[J].J Chromatogr,1980,202:255-261．
【8】Levine S P,Harvey T M,Waeghe T J,et al.O-alkyloxime derivatives for gas chromatographic and gas chromatographic-mass spectrometric determination of aldehydes[J].Anal Chem,1981,53:805-809．
【9】Nambara T,Kigasawa K,Iwata T,et al.A New Type of Derivative for Flectron Capture-Gas Chromatography of Ketosteroids[J].J Chromatogr,1975,114:81．
【10】Iwata T,Hirose T,Nakamura M,et al.6,7-Dime-thoxy-1-methyl-2-oxo-1,2-dihydroquinoxalin-3-ylpro-piono-hydrazide as a fluorescence derivatization reagent for aldehydes in high-performance liquid chromatography[J].Analyst,1993,118:517．
【11】Zhang R E,Cao Y,Hearn W M.Synthesis and Application of Fmoc-Hydrazine for the Quantitative Determiantion of Saccharides by Reversed-Phase High-Performance Liquid Chromatography in the Low ang Subpicomole Range[J].Anal Biochem,1991,195:160．
【12】Goto J,Saisho Y,Nambara T.Sensitive Fluorescence Labeling Reagents for High Performance Liquid Chromatography of Carbonyl Compounds[J].Anal Sci,1989,5:399．
【13】Uzu S,Kanda S,Imai K,et al.Fluorogenic reagents: 4-aminosulphonyl-7-hydrazino-2,1,3-benzoxadiazole,4-(N,N-dimethylaminosulphonyl)-7-hydrazino-2,1,3-benzoxadiazole and 4-hydrazino-7-nitro-2,1,3-benzoxadiazole hydrazine for aldehydes and ketones[J].Analyst,1990,115:1477．
【14】Gubitz G,Wintersteiger R,Frei R W.Toroidal Coil Countercurrent Chromatography in Affinity Partitioning of Nicotinic Cholinergic Receptor Enriched Membranes[J].J Liq Chromatogr,1984,7:389．
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