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The hydroxyethyl substitution along and among the polymer chains of respective cellulose ethers (HEC and HEMC) can be analyzed by ESI-IT-MS after permethylation of the free OH-groups, partial hydrolysis, and mABA labeling. This method requires the correct quantification of the molar ratios of the constituents belonging to a particular degree of polymerization (DP) with respect to their numbers of MeOEt and Me groups without any discrimination along the MS analysis pathway. The influence of the chemistry on the ionization and the impact of the voltages controlling the ion transport (Cap Exit, Octopoles) and the ion storage efficiency (Trap Drive, TD) on a relative quantification were studied using binary equimolar mixtures of cellobiose with increasing number of methoxyethyl and decreasing number of methyl groups (Δ m/z 88, 2× MeOEt). No suppression effects were observed in concentration-dependent measurements. Choice of Cap Exit is especially crucial for low m/z with less MeOEt residues. An equation describing the relationship between Oct 2 DC, m/z, and TD max (TD at maximum intensity) was established from the experimental data and applied to calculate TD max for higher DPs (larger COS). Optimized conditions allowed to determine the correct molar ratio of binary mixtures. Measurements of overlapping m/z segments and subsequent interrelation of the data gave complete substitution profiles for MeOEt/Me celluloses in accordance with reference data. The study generally makes aware of potential erroneous quantification in ESI-IT-MS analysis using internal standards of similar chemistry or in relative quantification of analytes, even for those with related structures.

analytical and bioanalytical chemistry/analytical and bioanalytical chemistry

Impact of instrumental settings in electrospray ionization ion trap mass spectrometry on the analysis of O-methoxyethyl-O-methyl cellulose: a comprehensive quantitative evaluation