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机构地区:[1]广东药学院药科学院,广东广州510006 [2]中山大学测试中心,广东广州510275 [3]中山大学化学与化学工程学院,广东广州510275
出 处:《分析测试学报》2008年第11期1225-1228,1232,共5页Journal of Instrumental Analysis
基 金:广东省自然科学基金资助项目(990209);广东药学院博士启动基金资助项目(43540128)
摘 要:首次以6种香豆素衍生物——3-氨基香豆素(3-AC)、3-羟基香豆素(3-HC)、3-羧基香豆素(3-CC)、4-甲基-7-羟基香豆素(4-M-7-HC)、3-乙酰氨基香豆素(3-AcAC)和3-苯基-7-乙酰氨基香豆素(3-ph-7-AcAC)为基质对聚乙二醇样品进行基质辅助激光解吸/电离飞行时间质谱(MALDI TOF-MS)分析。结果表明:3-AC、3-HC和3-CC均能有效解吸电离聚乙二醇样品,产生分辨率高、离子信号强、信噪比高的质谱图,不仅测定了聚乙二醇样品的数均相对分子质量、重均相对分子质量和聚合度分布,还能够准确地推测出样品的端基结构和重复单元,将为改善高分子合成反应条件和机理推导提供确凿依据。3-AC、3-HC和3-CC香豆素衍生物将为MALDI TOF-MS分析高分子聚合物提供新的基质选择。For the first time, six coumaric derivatives including 3-aminocoumarin (3-AC), 3- hydroxycoumarin ( 3 -HC ), 3-carboxycoumarin ( 3-CC ), 4-methyl-7-hydroxycoumarin ( 4-M-7 -HC ), 3 - acetylamino-coumarin(3-AcAC) and 3-phenyl-7-acetylaminocoumarin ( 3-ph-7-AcAC), were studied as matrices for determination of three polyethylene glycol samples by matrix-assisted laser desorption/ ionization time-of-flight mass spectrometry(MALDI TOF - MS ) method. The results showed that 3- AC, 3-HC and 3-CC could desorb and ionize effectively polyethylene glycol samples and produced the mass spectra with good resolution, strong molecular ion signals and high signal-to-noise(S/N). The number average (Mn), weight average (Mw ) and polydispersities were determined and the terminal group and repeating unit were analyzed clearly according to the mass data and the synthetic reaction. These coumarinic matrices would offer new light on MALDI TOF - MS analyse of complex polymer.
关 键 词:基质辅助激光解吸/电离飞行时间质谱 香豆素衍生物 基质 聚乙二醇
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