Abstract

Use of a TG/DTA/Raman system enabled real time collection of Raman spectra during the dehydration of Risedronate, the active pharmaceutical ingredient in the osteoporosis drug Actonel. Raman spectra collected during the dehydration of this material show a crystal lattice adjustment below the boiling point of water facilitating interpretation of the TG/DTA thermal profile. Raman spectra also revealed recrystallization processes subsequent to loss of lattice water that were not evident in the thermal analysis profile. Spectral evidence showing the formation and disappearance of a second hydrate form are observed during the dehydration of this material. In addition, spectral evidence indicating the presence of an anhydrate form of this material are observed prior to thermal induced degradation of this material.

References

1.
Szekely
,
G.
, et al
,
Thermochimica Acta
 0040-6031, Vol.
196
,
1992
, pp.
511
-
532
.
2.
Kinoshita
,
R.
, et al
,
Thermochimica Acta
 0040-6031, Vol.
222
,
1993
, pp.
45
-
52
.
3.
Giron
,
D.
,
Journal of Thermal Analysis and Calorimetry
 1418-2874, Vol.
68
,
2002
, pp.
335
-
357
.
4.
Vora
,
A.
, et al
,
29th NATAS Conference Proceedings
,
2001
, pp.
101
-
105
.
5.
Loridant
,
S.
,
Bonnat
,
M.
, and
Siebert
,
E.
,
Applied Spectroscopy
 0003-7028, Vol.
49
,
1995
, pp.
1193
-
1196
.
6.
Chang
,
H.
and
Huang
,
P. J.
,
Raman Spectroscopy
, Vol.
29
,
1998
, pp.
97
-
102
.
7.
Murgan
,
R.
,
Hhule
,
A.
, and
Chang
,
H. J.
,
Applied Physics
 0340-3793, Vol.
86
,
1999
, p. 6779.
8.
Chang
,
H.
, et al
,
Reviews in Analytical Chemistry
, Vol.
20
, No.
3
,
2001
, pp.
207
-
238
.
9.
Chang
,
H.
and
Huang
,
P. J.
,
Analytical Chemistry
 0003-2700 https://doi.org/10.1021/ac960881l, Vol.
69
,
1997
, pp.
1485
-
1491
.
10.
Huang
,
P. J.
, et al
,
Thermochimica Acta
 0040-6031 https://doi.org/10.1016/S0040-6031(97)00168-8, Vol.
297
,
1997
, pp.
85
-
92
.
11.
Ghule
,
A.
, et al
,
Thermochimica Acta
 0040-6031, Vol.
371
,
2001
, pp.
127
-
135
.
12.
Chang
,
H.
, et al
,
Materials Chemistry and Physics
 0254-0584 https://doi.org/10.1016/S0254-0584(98)00239-9, Vol.
58
,
1999
, pp.
12
-
19
.
13.
Ghule
,
A.
, et al
,
Inorganic Chemistry
 0020-1669, Vol.
40
,
2001
, pp.
5917
-
5923
.
14.
Baskaran
,
N.
and
Chang
,
H.
,
Materials Chemistry and Physics
 0254-0584 https://doi.org/10.1016/S0254-0584(02)00213-4, Vol.
77
,
2003
, pp.
889
-
894
.
15.
Murugan
,
R.
, et al
,
Journal of Physics: Condensed Matter
 0953-8984 https://doi.org/10.1088/0953-8984/12/5/315, Vol.
12
,
2000
, pp.
677
-
700
.
16.
Ghule
,
A.
, et al
,
Spectrochimica Acta
 0038-6987, Vol.
Part A 59
,
2003
, pp.
1529
-
1539
.
17.
Chang
,
H.
, et al
,
Thermochimica Acta
 0040-6031 https://doi.org/10.1016/S0040-6031(01)00488-9, Vol.
374
,
2001
, pp.
45
-
49
.
18.
Murugan
,
R.
, et al
,
Thermochimica Acta
 0040-6031 https://doi.org/10.1016/S0040-6031(99)00364-0, Vol.
346
,
2000
, pp.
83
-
90
.
19.
Dubois
,
C. D.
, et al
,
30th NATAS Conference Proceedings
,
2002
, pp.
214
-
219
.
20.
Ghule
,
A. V.
,
Lo
,
B.
,
Tzing
,
S. H.
,
Hhule
,
K.
,
Chang
,
H.
, and
Ling
,
Y. C.
,
Chem. Phys. Letters
, Vol.
381
,
2003
, pp.
262
-
270
.
21.
Jager
,
H. J.
and
Prinsloo
,
L. C.
,
Thermochimica Acta
 0040-6031, Vol.
376
,
2001
, pp.
187
-
196
.
22.
Ghule
,
A.
,
Baskaran
,
N.
,
Murugan
,
R.
,
Chang
,
H.
,
Solid State Ionics
 0167-2738, Vol.
161
,
2003
, pp.
291
-
299
.
23.
Redman-Furey
,
N. L.
, et al
,
30th NATAS Conference Proceedings
,
2002
, pp.
733
-
738
.
24.
Analytical Applications of Raman Spectroscopy
,
M. J.
Pelletier
, Ed.,
1999
, pp.
1
-
97
.
25.
Wang
,
F.
, et al
,
Organic Process Research & Development
, Vol.
4
,
2000
, pp.
391
-
395
.
26.
Collins
,
W. J.
, et al
, “
Development and Evaluation of a TG/DTA/Raman System
,”
31st NATAS Conference Proceedings
,
2003
.
27.
Redman-Furey
,
N. L.
, et al
,
Journal of Pharmaceutical Sciences
 0022-3549 https://doi.org/10.1002/jps.20308, Vol.
94
, No.
4
,
2005
, pp.
893
-
911
.
This content is only available via PDF.
You do not currently have access to this content.