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| 黄金蝉若虫体蛋白水解液的荧光标记及电喷雾质谱鉴定 | |
| 引用本文： | 李肖燕,尤进茂,孙志伟,付艳艳,秦雪芹,丁明州,李玉林.黄金蝉若虫体蛋白水解液的荧光标记及电喷雾质谱鉴定[J].分析化学,2010,38(7). |
| 作者姓名： | 李肖燕 尤进茂 孙志伟 付艳艳 秦雪芹 丁明州 李玉林 |
| 作者单位： | 1. 曲阜师范大学,山东省生命有机分析重点实验室,曲阜,273165 2. 曲阜师范大学,山东省生命有机分析重点实验室,曲阜,273165;中国科学院西北高原生物研究所,西宁,810008 3. 曲阜师范大学,山东省生命有机分析重点实验室,曲阜,273165;中国科学院研究生院,北京,100049 4. 中国科学院西北高原生物研究所,西宁,810008 |
| 基金项目： | 国家自然科学基金，中国科学院"百人计划" |
| 摘 要： | 采用2-2-(7H-二苯并a,g]咔唑-乙氧基)-乙基]氯甲酸酯(DBCEC-Cl)作为柱前衍生试剂, 于室温下,在硼酸钠缓冲液(pH 9.0)中,金蝉若虫体蛋白水解液中氨基酸的完全衍生化在5 min即可完成.在Hypersil BDS C18色谱柱 (200 mm×4.6 mm, 5 μm) 上, 采用梯度洗脱实现了各衍生物的完全基线分离.最佳荧光检测为λex/λem=300/395 nm.在线串联的ESI/MS正离子质谱数据显示:所有衍生物均给出m/z 338 5,294.5的特征碎片离子峰.荧光条件下的线性回归系数大于0.9992; 检出限为2.6～24 fmol.本方法灵敏、可靠、重现性好.对实际黄金蝉若虫体蛋白水解液中氨基酸的测定,结果满意. |
| 关 键 词： | 高效液相色谱-离子阱/质谱 荧光检测 柱前衍生 2-[2-(7H-二苯并[a g]咔唑-乙氧基)-乙基]氯甲酸酯 氨基酸 |
Application of 2-[2-(7H-Dibenzo[a,g]-carbazol-7-yl)-ethoxyl]ethyl Chloroformate as A Pre-column Derivatization Reagent for Determination of Amino Acids from Hydrolyzed Cicada by High Performance Liquid Chromatography with Fluorescence Detection and Mass S |
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| LI Xiao-Yan,YOU Jin-Mao,SUN Zhi-Wei,FU Yan-Yan,QIN Xue-Qin,DING Ming-Zhou,LI Yu-Lin.Application of 2-[2-(7H-Dibenzo[a,g]-carbazol-7-yl)-ethoxyl]ethyl Chloroformate as A Pre-column Derivatization Reagent for Determination of Amino Acids from Hydrolyzed Cicada by High Performance Liquid Chromatography with Fluorescence Detection and Mass S[J].Chinese Journal of Analytical Chemistry,2010,38(7). | |
| Authors: | LI Xiao-Yan YOU Jin-Mao SUN Zhi-Wei FU Yan-Yan QIN Xue-Qin DING Ming-Zhou LI Yu-Lin |
| Institution: | LI Xiao-Yan1,YOU Jin-Mao1,2,SUN Zhi-Wei1,3,FU Yan-Yan1,QIN Xue-Qin1,DING Ming-Zhou1,LI Yu-Lin2 1(College of Chemistry,Qufu Normal University,the Key Laboratory of Life-Organic Analysis,Qufu 273165) 2(Northwest Plateau Institute of Biology,Chinese Academy of Sciences,Xining 810001) 3(Graduate School of Chinese Academy of Sciences,Beijing 100039) |
| Abstract: | By using 2-2-(7H-dibenzoa,g]carbazole-ethoxy)-ethyl chloroformate (DBCEC-Cl) as a sensitive pre-column derivatization reagent,a simple method for evaluating the chemical compositions of protein amino acids from the hydrolyzed cicada sample has been developed.Studies on derivatization conditions indicated that the labeling reaction proceeded rapidly and smoothly in the presence of a base catalyst (pH 9.0) in acetonitrile to give the corresponding sensitively fluorescent derivatives with an excitation maxim... |
| Keywords: | High performance liquid chromatography-ion trap mass spectrometry Fluorescence detection Pre-column derivatization 2-[2-(7H-Dibenzo[a g]carbazol-7-yl)-ethoxy]ethyl chloroformate Amino acids |
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