The molecular weight, the purity, and the degree ofsubstitution for several newly synthesized single-isomer,heptasulfated
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-cyclodextrin derivatives,he
ptakis-6-sulfato-
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-cyclodextrin,he
ptakis(2,3-diacetyl-6-sulfato)-
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-cyclodextrin, andhe
ptakis(2,3-dimethyl-6-sulfato)-
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-cyclodextrin, were determined by electrospray ionization massspectrometry and indirect UV detection capillary electrophoresis. The main fragmentation mechanism of thesesingle-isomer, fully sulfated cyclodextrins involves dissociation of the sulfate groups. The extent ofdesulfationincreases with the skimmer-collimator voltage bias andthe number of charges on the electrospray ions. Byreducing the skimmer-collimator voltage bias, the lossof sulfate groups could be reduced, though not completelyeliminated, for the doubly charged molecular ions.Thus,ESI-MS can be used to confirm the degree of substitutionfor the most sulfated isomer, but not to determine theexact concentration distribution for the lower substitutedisomers in a mixture.