PMCCPMCCPMCC

Search tips
Search criteria 

Advanced

 
Logo of aapspharmspringer.comThis journalToc AlertsSubmit OnlineOpen Choice
 
AAPS PharmSciTech. 2006 March; 7(1): E72–E78.
Published online 2006 February 10. doi:  10.1208/pt070111
PMCID: PMC2750718

Quantitative measurement of indomethacin crystallinity in indomethacin-silica gel binary system using differential scanning calorimetry and X-ray powder diffractometry

Abstract

Differential scanning calorimetry (DSC) and X-ray powder diffractometry (XRPD) methods were developed for the quantitative analysis of the crystallinity of indomethacin (IMC) in IMC and silica gel (SG) binary system. The DSC calibration curve exhibited better linearity than that of XRPD. No phase transformation occurred in the IMC-SG mixtures during DSC measurement. The major sources of error in DSC measurements were inhomogeneous mixing and sampling. Analyzing the amount of IMC in the mixtures using high-performance liquid chromatography (HPLC) could reduce the sampling error. DSC demonstrated greater sensitivity and had less variation in measurement than XRPD in quantifying crystalline IMC in the IMC-SG binary system.

Keywords: Differential scanning calorimetry, X-ray powder diffractometry, crystallinity, quantitative analysis, indomethacin, silica gel, amorphization

Full Text

The Full Text of this article is available as a PDF (214K).

Selected References

These references are in PubMed. This may not be the complete list of references from this article.
1. Vippagunta SR, Brittain HG, Grant DJW. Crystalline Solids. Adv Drug Deliv Rev. 2001;48:3–26. doi: 10.1016/S0169-409X(01)00097-7. [PubMed] [Cross Ref]
2. Morris KR, Griesser UJ, Eckhardt CJ, Stowell JG. Theoretical approaches to physical transformations of active pharmaceutical ingredients during manufacturing processes. Adv Drug Deliv Rev. 2001;48:91–114. doi: 10.1016/S0169-409X(01)00100-4. [PubMed] [Cross Ref]
3. Zhang GG, Law D, Schmitt EA, Qiu YH. Phase transformation considerations during process development and manufacture of solid oral dosage forms. Adv Drug Deliv Rev. 2004;56:371–390. doi: 10.1016/j.addr.2003.10.009. [PubMed] [Cross Ref]
4. Hanawa T, Ikoma R, Watanabe A, Hidaka M, Sugihara M. Preparation and characterization of sealed heated mixture of ethenzamide and porous calcium silicate. Chem Pharm Bull (Tokyo) 1996;44:1367–1371.
5. Taylor LS, Zografi G. The quantitative analysis of crystallinity using FT-Raman spectroscopy. Pharm Res. 1998;15:755–761. doi: 10.1023/A:1011979221685. [PubMed] [Cross Ref]
6. Jalsovszky G, Egyed O, Holly S, Hegedus B. Investigation of the morphological composition of cimetidine by FT-Raman spectroscopy. Appl Spectrosc. 1995;49:1142–1145. doi: 10.1366/0003702953965164. [Cross Ref]
7. Forbes RA, McGarvey BM, Smith DR. Measurement of residual isopropyl alcohol in loracarbef by near-infrared reflectance spectroscopy. Anal Chem. 1999;71:1232–1239. doi: 10.1021/ac981135e. [Cross Ref]
8. Andersen KV, Bildsoe H, Jakobsen HJ. Determination of enantiomeric purity from solid-state 31P MAS NMR of organophosphorus compounds. Magn Reson Chem. 1990;28:S47–S51. doi: 10.1002/mrc.1260281310. [Cross Ref]
9. Kamat MS, Osawa T, DeAngelis RJ, Koyama Y, Deluca PP. Estimation of the degree of crystallinity of cefazolin sodium by X-ray and infrared methods. Pharm Res. 1988;5:426–429. doi: 10.1023/A:1015984300692. [PubMed] [Cross Ref]
10. Otsuka M, Kaneniwa N. A kinetic study of the crystallization process of non-crystalline indomethacin under isothermal conditions. Chem Pharm Bull (Tokyo) 1988;36:4026–4032. [PubMed]
11. Seyer JJ, Luner PE. Determination of indomethacin crystallinity in the presence of excipients using diffuse reflectance near-infrared spectroscopy. Pharm Dev Technol. 2001;6:573–582. doi: 10.1081/PDT-120000295. [PubMed] [Cross Ref]
12. Yoshioka M, Hancock BC, Zografi G. Inhibition of indomethacin crystallization in poly(vinylpyrrolidone) coprecipitates. J Pharm Sci. 1995;84:983–986. doi: 10.1002/jps.2600840814. [PubMed] [Cross Ref]
13. Clas SD, Faizer R, O’Connor RE, Vadas EB. Quantification of crystallinity in blends of lyophilized and crystalline MK-0591 using X-ray powder diffraction. Int J Pharm. 1995;121:73–79. doi: 10.1016/0378-5173(95)00008-7. [Cross Ref]
14. Suryanarayanan R, Herman CS. Quantitative analysis of the active ingredient in a multi-component tablet formulation by powder X-ray diffractometry. Int J Pharm. 1991;77:287–295. doi: 10.1016/0378-5173(91)90329-M. [Cross Ref]
15. Konno T. Physical and chemical changes of medicinals in muxtures with adsorbents in the solid state. 4. Study on reduced-pressure mixing for practical use of amorphous mixtures of flufenamic acid. Chem Pharm Bull (Tokyo) 1990;38:2003–2007. [PubMed]
16. Nakai Y, Yamamoto K, Izumikawa S. Interaction of medicinals and porous powder. 3. Effects of pore diameter of porous glass powder on crystalline properties. Chem Pharm Bull (Tokyo) 1989;37:435–438.
17. Vippagunta SR, Maul KA, Tallavajhala S, Grant DJW. Solid-state characterization of nifedipine solid dispersions. Int J Pharm. 2002;236:111–123. doi: 10.1016/S0378-5173(02)00019-4. [PubMed] [Cross Ref]
18. Park A, Cima LG. In vitro cell response to differences, in poly-lactide crystallinity. J Biomed Mater Res. 1996;31:117–130. doi: 10.1002/jbm.1996.820310102. [PubMed] [Cross Ref]
19. Liggins RT, Burt HM. Paclitaxel-loaded poly(L-lactic acid) microspheres. 3. Blending low and high molecular weight polymers to control morphology and drug release. Int J Pharm. 2004;282:61–71. doi: 10.1016/j.ijpharm.2004.05.026. [PubMed] [Cross Ref]
20. Alsaidan SM, Alsughayer AA, Eshra AG. Improved dissolution rate of indomethacin by adsorbents. Drug Dev Ind Pharm. 1998;24:389–394. doi: 10.3109/03639049809085635. [PubMed] [Cross Ref]
21. Gupta MK, Goldman D, Bogner RH, Tseng YC. Enhanced drug dissolution and bulk properties of solid dispersions granulated with a surface adsorbent. Pharm Dev Technol. 2001;6:563–572. doi: 10.1081/PDT-120000294. [PubMed] [Cross Ref]
22. Konno T, Kimuno K. Physical and chemical changes of medicinals in mixtures with adsorbents in the solid state. 2. Application of reduced pressure treatment for the improvement of dissolution of flufenamic acid. Chem Pharm Bull (Tokyo). 1989;37:2481–2484. [PubMed]
23. Nakai Y, Yamamoto K, Terada K. Interaction of medicinals and porous powder. 1. Anomalous thermal behavior of porous glass mixtures. Chem Pharm Bull (Tokyo) 1984;32:4566–4571. [PubMed]
24. Hanawa T, Ikoma R, Watanabe A, Hidaka M, Sugihara M. Preparation and characterization of sealed heated mixture of ethenzamide and porous calcium silicate. Chem Pharm Bull (Tokyo) 1996;44:1367–1371.
25. Otsuka M, Kato F, Matsuda Y. Determination of indomethacin polymorphic contents by chemometric near-infrared spectroscopy and conventional powder X-ray diffractometry. Analyst. 2001;126:1578–1582. doi: 10.1039/b103498g. [PubMed] [Cross Ref]
26. O’Brien M, McCauley J, Cohen E, editors. Indomethacin. Analytical Profiles of Drug Substances. London, UK: Academic Press; 1984.

Articles from AAPS PharmSciTech are provided here courtesy of American Association of Pharmaceutical Scientists