An examination of the kinetics of the solution-mediated polymorphic phase transformation between α- and β-forms of L-glutamic acid as determined using online powder X-ray diffraction

被引:35
作者
Dharmayat, Spoorthi [1 ]
Hammond, Robert B. [1 ]
Lai, Xiaojun [1 ]
Ma, Caiyun [1 ]
Purba, Elida [1 ]
Roberts, Kevin J. [1 ]
Chen, Zeng-Ping [2 ]
Martin, Elaine [2 ]
Morris, Julian [2 ]
Bytheway, Richard [3 ]
机构
[1] Univ Leeds, Sch Proc Environm & Mat Engn, Inst Particle Sci & Engn, Leeds LS2 9JT, W Yorkshire, England
[2] Newcastle Univ, Sch Chem Engn & Adv Mat, Ctr Proc Analyt & Control Technol, Newcastle Upon Tyne NE1 7RU, Tyne & Wear, England
[3] Bede Xray Metrol, Durham DH1 1TW, England
关键词
D O I
10.1021/cg0706215
中图分类号
O6 [化学];
学科分类号
0703 ;
摘要
Online powder X-ray diffraction, employing a flow-through cell [Hammond et al. Cryst. Growth Des. 2004, 4, 943] and a previously developed cheuaometric method [Chen et al. Anal. Chem. 2005, 77, 6563], was applied for quantitative analysis of the polymorphic phase transformation from the metastable alpha-form to the stable beta-form of L-glutamic acid (LGA). The process of interconversion was monitored in aqueous slurries, using a jacketed 400 mL magnetically stirred reactor as a function of temperature. Calibration studies revealed that the current detection limits are.ca. 0.8 and 0.2 wt%, respectively, for alpha- and beta-forms of LGA as determined for slurries of LGA in methanol and good signal detection can be accomplished using a data acquisition time of 10 s albeit with increased noise levels. Compositions of slurries, in terms of the amounts of the individual solid phases present, were calculated from the areas of individual, discriminating peaks associated with the phases. Analysis of the diffraction peaks arising from the (111) reflection, 2 theta = 18 degrees for the a-forth and (102) reflection, 2 theta = 31 degrees for the beta-form, was used to obtain the rates of phase interconversion. Phenomenologically, the rate law observed for dissolution of the alpha-form was -D-alpha = k(d alpha) and the rate law observed for growth of the beta-form was D-beta = k(g beta)C(beta) where C-beta is the concentration of the beta-form expressed in weight percent. At 45 degrees C, the values of the rate constants k(d alpha) and k(g beta) were 18 x 10(-4) wt% s(-1) and 3 x 10(-4) s(-1), respectively. Activation energies calculated, using the Arrhenius relationship, were found to be 43.9 kJ/mol with k(d alpha 0) calculated to be 25.9 x 10(3) wt% s(-1) for the dissolution of alpha-form and 47.0 kJ/mol with k(g beta 0) calculated to be 16.2 x 10(30) s(-1) for the growth of the beta-form. The activation energy calculated from a different, characteristic peak of the beta-form at 2 theta = 21 degrees corresponding to the reflection from (101) planes, was 32.1 kJ/mol suggesting that there might be some texture effects manifested in the flow field of the crystalline slurry. The overall quantitative accuracy of this method together with potential for improvement is also discussed.
引用
收藏
页码:2205 / 2216
页数:12
相关论文
共 41 条
[1]   In situ measurement of solvent-mediated phase transformations during dissolution testing [J].
Aaltonen, Jaakko ;
Heinanen, Paula ;
Peltonen, Leena ;
Kortejarvi, Hanna ;
Tanninen, Veli Pekka ;
Christiansen, Leena ;
Hirvonen, Jouni ;
Yliruusi, Jouko ;
Rantanen, Jukka .
JOURNAL OF PHARMACEUTICAL SCIENCES, 2006, 95 (12) :2730-2737
[2]   Crystal chemistry and solvent effects in polymorphic systems - Sulfathiazole [J].
Blagden, N ;
Davey, RJ ;
Lieberman, HF ;
Williams, L ;
Payne, R ;
Roberts, R ;
Rowe, R ;
Docherty, R .
JOURNAL OF THE CHEMICAL SOCIETY-FARADAY TRANSACTIONS, 1998, 94 (08) :1035-1044
[3]   THE KINETICS OF SOLVENT-MEDIATED PHASE-TRANSFORMATIONS [J].
CARDEW, PT ;
DAVEY, RJ .
PROCEEDINGS OF THE ROYAL SOCIETY OF LONDON SERIES A-MATHEMATICAL PHYSICAL AND ENGINEERING SCIENCES, 1985, 398 (1815) :415-428
[4]   Control of polymorphism and crystal size of L-glutamic acid in the absence of additives [J].
Cashell, C ;
Corcoran, D ;
Hodnett, BK .
JOURNAL OF CRYSTAL GROWTH, 2004, 273 (1-2) :258-265
[5]  
CHAN HK, 1985, DRUG DEV IND PHARM, V11, P315, DOI 10.3109/03639048509056874
[6]   Enhancing the signal-to-noise ratio of X-ray diffraction profiles by smoothed principal component analysis [J].
Chen, ZP ;
Morris, J ;
Martin, E .
ANALYTICAL CHEMISTRY, 2005, 77 (20) :6563-6570
[7]   Modeling and comparison of dissolution profiles [J].
Costa, P ;
Manuel, J ;
Lobo, S .
EUROPEAN JOURNAL OF PHARMACEUTICAL SCIENCES, 2001, 13 (02) :123-133
[8]   Polymorphism in molecular crystals: Stabilization of a metastable form by conformational mimicry [J].
Davey, RJ ;
Blagden, N ;
Potts, GD ;
Docherty, R .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1997, 119 (07) :1767-1772
[9]   RATE CONTROLLING PROCESSES IN SOLVENT-MEDIATED PHASE-TRANSFORMATIONS [J].
DAVEY, RJ ;
CARDEW, PT ;
MCEWAN, D ;
SADLER, DE .
JOURNAL OF CRYSTAL GROWTH, 1986, 79 (1-3) :648-653
[10]   In situ monitoring of wet granulation using online X-ray powder diffraction [J].
Davis, TD ;
Morris, KR ;
Huang, HP ;
Peck, GE ;
Stowell, JG ;
Eisenhauer, BJ ;
Hilden, JL ;
Gibson, D ;
Byrn, SR .
PHARMACEUTICAL RESEARCH, 2003, 20 (11) :1851-1857