网络招聘分析报告.ppt

2-(苯并吖啶***)-乙基咪唑酸酯探针对荧光和质谱的双增敏作用
作者:付艳艳李肖燕孙志伟秦雪芹夏莲索有瑞李玉林尤进茂
【摘要】采用3种不同衍生方法对***类化合物进行标记,比较衍生效率的差别,给出最优方法:5-(2-羟乙基)-(苯并吖啶***与N,N-羰基双咪唑(CDI)缩合形成的双敏感探针2-(苯并吖啶***)-乙基咪唑酸酯(BAEIC)与***的衍生效率最高,产物稳定。BAEIC在N,N-二***甲酰***(DMF) 溶剂中以4-二甲氨基吡啶(DMAP) 为催化剂,在80 ℃条件下与***反应生成的亲核取代物,不仅表现出强烈的荧光,同时具有很强的质谱离子化能力。估算了衍生物在乙***%~%%~%范围内。本方法具有良好的重现性,激发和发射波长为λex/λem=280/510 nm,~ μg/L(~79 fmol); 在线APCI-~14 μg/L(544~825 fmol)。
【关键词】液相色谱-质谱; 脂肪***; 5-(2-羟乙基)-苯并吖啶***; 2-(苯并吖啶***)-乙基咪唑酸酯
Abstract parison of three different methods for the marking of pound,an optimal derivatization method was -(2-Hydroxyethyl)benzoacridine(HBA) reacts with coupling agent N,N′-carbonyldiimidazole(CDI) to form an activated amide intermediate 2-(benzoacridin)ethyl-imidazole-1-carboxylate(BAEIC).BAEIC,which is dual-sensitive probe,reacts preferably with pounds at 80 ℃ in the presence of 4-dimethylaminopyridine(DMAP) catalyst in N,N-dimethylformamide(DMF) solvent to give the corresponding sensitively fluorescent derivatives with an excitation maximum at λex of 280 nm and an emission maximum at λem of 510 -amine derivatives simultaneously exhibited high ionization potential with percent ionization( changing from % to % in aqueous acetonitrile and from % to % in aqueous were not only sensitive to fluorescence but also to MS ionizable fluorescence detection limits(S/N=3) were - μg/ online APCI-MS detection limits were -14 μg/L(S/N=5).
Keywords High performance liquid chromatography/mass spectrometry; Aliphatic amines; 5-(2-Hydroxyethyl)benzoacridine; 2-(Benzoacridin)ethyl-imidazole-1- carboxylate
1 引言
质谱和荧光技术广泛应用于环境科学、毒物学及生命科学等领域中,用于确定诸多生物活性分子的含量及化学结构[1~3]。环境中的***多是由蛋白质、氨基酸等含氮类有机化合物经生物降解而成。大多数***类化合物在亚硝化剂存在下可生成强致癌性的N-亚硝基化合物[4~8],因此,检测环境中的***具有重要意义。目前,检测***的方法主要有气相色谱法[9]和离子交换法[10]。尽管方法简便易行,但由于灵敏度低而受到限制。为提高检测灵敏度和改善选择性,采用柱前或柱后衍生化是一种行之有效的手段。但测定***类化合物所用试剂较多[11~14],如常用荧光试剂FMOC-Cl衍生化时,过量试剂易造成柱效降低。此外,试剂对脯氨酸和半胱氨酸衍