CAJ | 학술논문

采用3种不同衍生方法对胺类化合物进行标记,比较衍生效率的差别,给出最优方法:5-(2-羟乙基)-(苯并吖啶酮与N,N-羰基双咪唑(CDI)缩合形成的双敏感探针2-(苯并吖啶酮)-乙基咪唑酸酯(BAEIC)与胺的衍生效率最高,产物稳定.BAEIC在N,N-二甲基甲酰胺(DMF)溶剂中以4-二甲氨基吡啶(DMAP)为催化剂,在80℃条件下与胺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.估算了衍生物在乙腈和甲醇水溶液中百分离子化值δ在5.62%～58.08%和2.14%～56.58%范围内.本方法具有良好的重现性,激发和发射波长为λ_(ex)/λ_(em)=280/510 nm,荧光检出限为0.12～0.59 μg/L(8.6～79 fmol);在线APCI-MS检出限为1.9～14 μg/L(544～825 fmol).
채용3충불동연생방법대알류화합물진행표기,비교연생효솔적차별,급출최우방법:5-(2-간을기)-(분병아정동여N,N-탄기쌍미서(CDI)축합형성적쌍민감탐침2-(분병아정동)-을기미서산지(BAEIC)여알적연생효솔최고,산물은정.BAEIC재N,N-이갑기갑선알(DMF)용제중이4-이갑안기필정(DMAP)위최화제,재80℃조건하여알반응생성적친핵취대물,불부표현출강렬적형광,동시구유흔강적질보리자화능력.고산료연생물재을정화갑순수용액중백분리자화치δ재5.62%～58.08%화2.14%～56.58%범위내.본방법구유량호적중현성,격발화발사파장위λ_(ex)/λ_(em)=280/510 nm,형광검출한위0.12～0.59 μg/L(8.6～79 fmol);재선APCI-MS검출한위1.9～14 μg/L(544～825 fmol).
With comparison of three different methods for the marking of amines compound, an optimal deri vatization method was selected.5-(2-Hydroxyethyl) benzoacridine (HBA) reacts with coupling agent N,N'-carbonyldiimidazole(CDI) to form an activated amide intermediate 2-(benzoacridin) ethyl-imidazole-1-carbox-ylate(BAEIC).BAEIC, which is dual-sensitive probe, reacts preferably with amino compounds 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 λ_(ex) of 280 nm and an emis sion maximum at λ_(em) of 510 nm.BAEIC-amine derivatives simultaneously exhibited high ionization potential with percent ionization (changing from 5.62% to 58.08% in aqueous acetonitrile and from 2.14% to 56.58% in aqueous methanol.Derivatives were not only sensitive to fluorescence but also to MS ionizable potential.The fluorescence detection limits(5/iV = 3) were 0.12-0.59 μg/L.The online APCI-MS detection limits were 1.9-14 μg/L(S/N=5).