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Solid-state phase behaviour of dodecylglycosides

Ericsson, Caroline LU ; Ericsson, Louise C and Ulvenlund, Stefan LU (2005) In Carbohydrate Research 340(8). p.1529-1537
Abstract
The solid-state phase behaviour of lyophilised n-dodecyl-beta-D-glucoside (beta-C(12)G(1)), n-dodecyl-beta-D-maltoside (beta-C(12)G(2)) and n-dodecyl-beta-D-maltotrioside (beta-C(12)G(3)) has been investigated by differential scanning calorimetry (DSC) and X-ray techniques. For beta-C(12)G(1), lyophilisation results in a formation of a crystalline anhydrate. The lamellar spacing (37 angstrom) is consistent with an alkyl chain packing in which the chains are not interdigitated. At 80 degrees C, the material melts into a lamellar liquid crystal with a lamellar spacing of 32 angstrom, which suggests that the non-interdigitated chain packing of the crystalline state is retained in the liquid crystal. In contrast, lyophilisation of... (More)
The solid-state phase behaviour of lyophilised n-dodecyl-beta-D-glucoside (beta-C(12)G(1)), n-dodecyl-beta-D-maltoside (beta-C(12)G(2)) and n-dodecyl-beta-D-maltotrioside (beta-C(12)G(3)) has been investigated by differential scanning calorimetry (DSC) and X-ray techniques. For beta-C(12)G(1), lyophilisation results in a formation of a crystalline anhydrate. The lamellar spacing (37 angstrom) is consistent with an alkyl chain packing in which the chains are not interdigitated. At 80 degrees C, the material melts into a lamellar liquid crystal with a lamellar spacing of 32 angstrom, which suggests that the non-interdigitated chain packing of the crystalline state is retained in the liquid crystal. In contrast, lyophilisation of beta-C(12)G(2) and beta-C(12)G(3) results in the formation of a glassy state, best described as a frozen version of the lamellar liquid crystal. For beta-C(12)G(2), the lamellar spacing in the glass and liquid crystal suggests interdigitation of the alkyl chains. The glass transition temperature was found to be 65 degrees C for beta-C(12)G(3), and 100 degrees C for K12G3, which compares favourably with the glass transition of the parent carbohydrates. A second crystalline modification of beta-C(12)G(1) was prepared by precipitation from an aqueous solution at temperatures below the Krafft point (38 degrees C). For this modification, the lamellar distance (24 angstrom) is consistent with interdigitated alkyl chains. At 50 degrees C, the crystalline material melts into a liquid crystalline phase. The material also readily loses water and rapidly re-crystallises to the anhydrate. The amount of water lost upon drying is consistent with the idea that the material is a monohydrate of beta-C(12)G(1). The drying and re-crystallisation processes give rise to 'pre-transitions' in the DSC thermograms and illustrate the importance of careful control of water in any analysis of the phase behaviour of alkylglycosides. (c) 2005 Elsevier Ltd. All rights reserved. (Less)
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author
organization
publishing date
type
Contribution to journal
publication status
published
subject
in
Carbohydrate Research
volume
340
issue
8
pages
1529 - 1537
publisher
Elsevier
external identifiers
  • pmid:15882846
  • wos:000229684500011
  • scopus:19344369519
ISSN
1873-426X
DOI
10.1016/j.carres.2005.03.015
language
English
LU publication?
yes
id
50811514-feee-4433-a8cf-481789f3616b (old id 157347)
date added to LUP
2007-07-11 11:19:13
date last changed
2017-07-23 03:53:07
@article{50811514-feee-4433-a8cf-481789f3616b,
  abstract     = {The solid-state phase behaviour of lyophilised n-dodecyl-beta-D-glucoside (beta-C(12)G(1)), n-dodecyl-beta-D-maltoside (beta-C(12)G(2)) and n-dodecyl-beta-D-maltotrioside (beta-C(12)G(3)) has been investigated by differential scanning calorimetry (DSC) and X-ray techniques. For beta-C(12)G(1), lyophilisation results in a formation of a crystalline anhydrate. The lamellar spacing (37 angstrom) is consistent with an alkyl chain packing in which the chains are not interdigitated. At 80 degrees C, the material melts into a lamellar liquid crystal with a lamellar spacing of 32 angstrom, which suggests that the non-interdigitated chain packing of the crystalline state is retained in the liquid crystal. In contrast, lyophilisation of beta-C(12)G(2) and beta-C(12)G(3) results in the formation of a glassy state, best described as a frozen version of the lamellar liquid crystal. For beta-C(12)G(2), the lamellar spacing in the glass and liquid crystal suggests interdigitation of the alkyl chains. The glass transition temperature was found to be 65 degrees C for beta-C(12)G(3), and 100 degrees C for K12G3, which compares favourably with the glass transition of the parent carbohydrates. A second crystalline modification of beta-C(12)G(1) was prepared by precipitation from an aqueous solution at temperatures below the Krafft point (38 degrees C). For this modification, the lamellar distance (24 angstrom) is consistent with interdigitated alkyl chains. At 50 degrees C, the crystalline material melts into a liquid crystalline phase. The material also readily loses water and rapidly re-crystallises to the anhydrate. The amount of water lost upon drying is consistent with the idea that the material is a monohydrate of beta-C(12)G(1). The drying and re-crystallisation processes give rise to 'pre-transitions' in the DSC thermograms and illustrate the importance of careful control of water in any analysis of the phase behaviour of alkylglycosides. (c) 2005 Elsevier Ltd. All rights reserved.},
  author       = {Ericsson, Caroline and Ericsson, Louise C and Ulvenlund, Stefan},
  issn         = {1873-426X},
  language     = {eng},
  number       = {8},
  pages        = {1529--1537},
  publisher    = {Elsevier},
  series       = {Carbohydrate Research},
  title        = {Solid-state phase behaviour of dodecylglycosides},
  url          = {http://dx.doi.org/10.1016/j.carres.2005.03.015},
  volume       = {340},
  year         = {2005},
}