Summary
The substitution patterns of methyl cellulose as well as of a thexyldimethylsilyl cellulose after permethylation were determined by hydrolysis and separation of the resulting partially methylated glucoses without further derivatization by h.p.l.c.. On an amine-modified silica column the solutes get separated into glucose, 2,3,6-tri-O-methyl glucose and the groups of mono-O-methyl-and di-O-methyl glucoses. A chromatographic run on a reversed-phase column enables the identification of the single mono-O-methyl- and di-O-methyl glucoses. In this way, a determination of both the average degree of substitution and the substitution pattern of cellulose derivatives is possible. Comparison of the results with those obtained by standard methylation analysis including g.l.c.-m.s. proves the correctnes of the method employed.
Similar content being viewed by others
References
Kowsaka K, Okajima K, Kamide K (1983) Polymer Journal 18: 843
Sei T, Ishitani K, Suzuki R (1985) Polymer Journal 17: 1065
Takahashi SI, Fujimoto T, Barua BM, Miyamoto T, Inagaki H (1986) J. Polym. Sci., Polym. Chem. Ed. 24: 2981
Tezuka Y, Imai K, Oshima M, Chiba T (1987) Macromolecules 20: 2413
Nehls I, Philipp B, Wagenknecht W, Klemm D, Schnabelrauch M, Stein A, Heinze T (1990) Papier (Darmstadt) 44: 633
Clemett CJ (1973) Anal. Chem. 45: 186
Ho FF, Klosziewicz DW (1980) Anal. Chem. 52: 913
Reuben J (1986) Carbohydr. Res. 157: 201
Reuben J (1987) Carbohydr. Res. 161: 23
Larm O, Larsson K, Theander O (1981) Starch/Stärke 33: 240
McNeil M, Albersheim P (1984) Carbohydr. Res. 131: 131
Lindberg B, Lindquist U, Stenberg O (1988) Carbohydr. Res. 176: 137
Rosell K-G (1988) Carbohydr. Res. 177: 289
Rosell K-G (1988) J. Carbohydr. Chem. 7: 525
Rolf D, Gray GR (1982) J. Am. Chem. Soc. 104: 3539
D'Ambra AJ, Rice MJ, Zeller SG, Gruber PR, Gray GR (1988) Carbohydr. Res. 177: 111
Mischnick-L. P, König WA (1989) Carbohydr. Res. 185: 113
Mischnick-L. P, Krebber R (1989) Carbohydr. Res. 187: 197
Mischnick P (1989) Carbohydr. Res. 192: 233
Mischnick P (1991) J. Carbohydr. Chem. 10: 711
Zeller SG, Griesgraber W, Gray GR (1991) Carbohydr. Res. 211: 41
Klemm D, Schnabelrauch M, Stein A, Heinze T, Erler U, Vogt, S (1991) Papier (Darmstadt) 45: 773
Cheetham NWH: Sirimanne P (1980) J. Chromatogr. 196: 171
Heyraud A, Salemis P (1982) Carbohydr. Research 107: 107
Sinner M (1976) J. Chromatogr. 121: 122
McGinnis GD, Fang P (1978) J. Chromatogr., 153: 107
Oshima R, Kumanotani J (1983) J. Chromatogr. 265: 335
Lehrfeld J (1976) J. Chromatogr. 120: 141
White CA, Kennedy JF, Golding BT (1979) Carbohydr. Res. 76: 1
Nachtmann F, Bunda KW (1977) J. Chromatogr. 136: 279
Thiem J, Karl H, Schwentner J, Reimer J (1978) J. Chromatogr. 147: 491
Sweet DP, Shapiro RH, Albersheim P (1975) Carbohydr. Res. 40: 217
Biermann CJ (1988) Adv. Carbohydr. Chem. Biochem. 46: 251
Micheel F, Klemer A (1956) Chemie der Zucker und Polysaccharide. Geest und Portig, Leipzig
Stein A, Erler U, Klemm D Carbohydr. Res. in preparation
Chaplin MF (1986) in Chaplin MF, Kennedy JF (ed) Carbohydrate analysis — a practical approach. IRL Press, Oxford Washington DC
Author information
Authors and Affiliations
Rights and permissions
About this article
Cite this article
Erler, U., Mischnick, P., Stein, A. et al. Determination of the substitution patterns of cellulose methyl ethers by HPLC and GLC-comparison of methods. Polymer Bulletin 29, 349–356 (1992). https://doi.org/10.1007/BF00944830
Accepted:
Issue Date:
DOI: https://doi.org/10.1007/BF00944830