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Characterization of single-isomer, heptasulfated beta-cyclodextrins by electrospray ionization mass spectrometry and indirect UV detection capillary electrophoresis

机译:电喷雾电离质谱和间接紫外检测毛细管电泳对单异构体七硫酸化β-环糊精的表征

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The molecular weight, the purity, and the degree of substitution for several newly synthesized single-isomer, heptasulfated beta-cyclodextrin derivatives, heptakis-6-sulfato-beta-cyclodextrin, heptakis(2,3-diacetyl-6-sulfato)-beta-cyclodextrin, and heptakis(2,3-dimethyl-6-sulfato)-beta-cyclodextrin, were determined by electrospray ionization mass spectrometry and indirect UV detection capillary electrophoresis. The main fragmentation mechanism of these single-isomer, fully sulfated cyclodextrins involves dissociation of the sulfate groups. The extent of desulfation increases with the skimmer-collimator voltage bias and the number of charges on the electrospray ions. By reducing the skimmer-collimator voltage bias, the loss of sulfate groups could be reduced, though not completely eliminated, for the doubly charged molecular ions. Thus, ESI-MS can be used to confirm the degree of substitution for the most sulfated isomer, but not to determine the exact concentration distribution for the lower substituted isomers in a mixture. [References: 35]
机译:几种新合成的单一异构体,七硫酸化β-环糊精衍生物,庚七-6-硫酸盐-β-环糊精,庚七(2,3-二乙酰基-6-硫酸盐)-β的分子量,纯度和取代度通过电喷雾电离质谱和间接紫外检测毛细管电泳法测定β-环糊精和七(2,3-二甲基-6-硫酸根)-β-环糊精。这些单一异构体,完全硫酸化的环糊精的主要断裂机理涉及硫酸酯基团的解离。脱硫程度随分离器-准直器的电压偏置和电喷雾离子上的电荷数量而增加。通过减少撇渣器-准直器的电压偏差,可以减少(尽管没有完全消除)双电荷分子离子的硫酸盐基团的损失。因此,ESI-MS可以用于确认最硫酸化的异构体的取代度,但不能确定混合物中较低取代的异构体的确切浓度分布。 [参考:35]

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