Abstract
The dehydration mechanism of α-lactose monohydrate was investigated by several techniques and interpreted on the basis of structural data. Whatever the dehydration conditions (heating or use of hygroscopic organic solvents), the departure of water molecules occurs cooperatively in channels parallel to the c axis of the initial structure. Subsequently, the reorganization leads to the closest packing (hygroscopic metastable form, LαH) under heating or to the stable anhydrous form (LαS), probably via a nucleation and growth process in ethanol. The use of acetone as dehydrating solvent on single crystals of α-lactose monohydrate led to the unexpected formation of single crystals of the anomeric β-lactose at room temperature, from which the crystal structure of β-lactose could be accurately re-determined. Recrystallization experiments of anhydrous lactose allowed to prepare N-methylpyrrolidinone and DMSO solvates of α-lactose.
Similar content being viewed by others
References
J. K. Guillory, Polymorphism in pharmaceutical solids (ed. H. G. Brittain), Marcel Dekker Inc., New York 1999, p. 183.
E. Garcia, S. Veesler, R. Boistelle and C. Hoff, J. Cryst. Growth, 198/199 (1999) 1360.
N. Rodriguez-Hornedo and D. Murphy, J. Pharm. Sci., 88 (1999) 651.
S. R. Byrn, R. R. Pfeiffer, G. Stephenson, D. J. W. Grant and W. B. Gleason, Chem. Mater., 6 (1994) 1148.
J. Bernstein, R. J. Davey and J.-O. Henck, Angew. Chem. Int. Ed. Engl., 38 (1999) 3440.
D. Giron, Thermochim. Acta, 248 (1995) 1.
K. R. Morris, S. L. Nail, G. E. Peck, S. R. Byrn, U. J. Griesser, J. G. Stowell, S.-J. Hwang and K. Park, Pharm. Sci. & Techn. Tod., 1 (1998), 235.
T. L. Threlfall, Analyst, 120 (1995) 2435.
S. R. Byrn, R. R. Pfeiffer, M. Ganey, C. Hoiberg and G. Poochikian, Pharm. Res., 12 (1995) 945.
J. D. Dunitz and J. Bernstein, Acc. Chem. Res., 28 (1995) 193.
J. Bernstein and J.-O. Henck, Cryst. Eng., 1 (1998) 119.
N. Blagden, R. J. Davey, R. Rowe and R. Roberts, Int. J. Pharm., 172 (1998) 169.
J.-O. Henck, J. Bernstein, A. Ellern and R. Boese, J. Am. Chem. Soc., 123 (2001) 1834.
F. J. J. Leusen, J. Cryst. Growth, 166 (1996) 900.
A. Gavezzotti, Faraday Discuss., 106 (1997) 63.
G. R. Desiraju, Science, 278 (1997) 404.
B. P. van Eijck and J. Kroon, Acta Cryst., B56 (2000) 535.
S. Petit and G. Coquerel, Chem. Mater., 8 (1994) 2247.
F. W. Goodhart, Handbook of Pharmaceutical Excipients (2nd ed.), Ed. A. Wade and P. J. Weller, The Pharmaceutical Press, London 1994, p. 252.
T. J. Buma and G. A. Wiegers, Neth. Milk & Dairy J., 21 (1967) 208.
E. Berlin, P. G. Kliman, B. A. Anderson and M. J. Pallansch, Thermochim. Acta, 2 (1971) 143.
Y. Roos and M. Karel, J. Food Sci., 57 (1992) 775.
T. D. Dincer, G. M. Parkinson, A. L. Rohl and M. I. Ogden, J. Cryst. Growth, 205 (1999) 368.
T. A. Nickerson and E. E. Moore, J. Dairy Sci., 57 (1974) 1315.
C. F. Lerk, A. C. Andreae, A. H. de Boer, P. de Hoog, K. Kussendrager and J. van Leverink, J. Pharm. Sci., 73 (1984) 856.
S. L. Raghavan, R. I. Ristic, D. B. Sheen and J. N. Sherwood, J. Pharm. Sci., 90 (2001) 823.
T. Itoh, M. Satoh and S. Adachi, J. Dairy Sci., 60 (1977) 1230.
L. O. Figura and M. Epple, J. Thermal Anal., 44 (1995) 45.
S. G. Lim and T. A. Nickerson, J. Dairy Sci., 56 (1973) 843.
T. J. Buma, Neth. Milk & Dairy J., 32 (1978) 258.
D. C. Fries, S. T. Rao and M. Sundaralingam, Acta Cryst., B27 (1971) 994.
C. A. Beevers and H. N. Hansen, Acta Cryst., B27 (1971) 1323.
J. H. Noordik, P. T. Beurskens, P. Bennema, R. A. Visser and R. O. Gould, Z. Kristallogr., 168 (1984) 59.
P. Walstra and R. Jenness, Dairy Chemistry and Physics, ‘Carbohydrates’, Chap. 3, John Wiley and Sons Ltd., New York 1984, p. 27.
G. M. Sheldrick, SHELXTL, Release 5.10, (Program for the determination and the refinement of crystal structures), Bruker Analytical X-ray Instruments Inc., Madison, Wisconsin, USA.
A. K. Galwey, Thermochim. Acta, 355 (2000) 181.
K. Shankland, W. I. F. David and T. Csoka, Z. Kristallogr., 212 (1997) 550.
G. A. Stephenson, J. Pharm. Sci., 89 (2000) 958.
A. Altomare, J. Foadi, C. Giacovazzo, A. G. G. Moliterni, M. C. Burla and G. Polidori, J. Appl. Cryst., 31 (1998) 74.
C. Gervais and G. Coquerel, Acta Cryst. A, submitted (2001).
S. Nordhoff and J. Ulrich, J. Therm. Anal. Cal., 57 (1999) 181.
E. Laine, V. Tuominen, P. Ilvessalo and P. Kahela, Int. J. Pharm., 20 (1984) 307.
C. C. Evans, Whiskers, Mills and Boon, London 1972, p. 19
K. Hirotsu and A. Shimada, Bull. Chem. Soc. Japan, 47 (1974) 1872.
R. Docherty, G. Clydesdale, K. J. Roberts and P. Bennema, J. Phys. D: Appl. Phys., 24 (1991) 89.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Garnier, S., Petit, S. & Coquerel, G. Dehydration Mechanism and Crystallisation Behaviour of Lactose. Journal of Thermal Analysis and Calorimetry 68, 489–502 (2002). https://doi.org/10.1023/A:1016087702409
Issue Date:
DOI: https://doi.org/10.1023/A:1016087702409