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Crystallinity evaluation of tacrolimus solid dispersions by chemometric analysis.
Int J Pharm. 2012 Feb 28; 423(2):341-50.IJ

Abstract

Different destructive and nondestructive analytical methods, namely powder X-ray diffractometry (PXRD), differential scanning calorimetry (DSC), Raman and near-infrared (NIR) spectroscopy and imaging, to detect and characterize tacrolimus trace crystallinity in an amorphous solid dispersion (SD) using chemometric analysis were developed. The SD was spiked with different percentages of the crystalline drug to construct an array of SDs with different crystallinity percentages. Partial least square (PLS) regression analysis was employed to compare the performance of the calibration models created using these analytical methods. The obtained results indicated a significant interaction between tacrolimus and the employed polymer and a drug dissolution dependency on the crystalline fraction within the SDs. Using two PLS factors, these analytical methods were ranked according to its specificity to detect the trace crystallinity of SDs as NIR>PXRD>Raman>DSC. Through the application of PLS, root-mean-squared error of calibration values of 2.91%, 5.36%, 7.07% and 11.58% were calculated for the calibration models constructed by NIR, PXRD, Raman and DSC, respectively. Having a prediction error of 2.1% and a correlation coefficient of 0.99, it is demonstrated that combined NIR imaging and chemometric analysis outperformed the other methods in detecting trace crystallinity in tacrolimus amorphous systems. The spatial distributions of amorphous and crystalline drug were also obtained in order to allow for studying the crystallization dissemination in the solid dispersions. Consequently, NIR and NIR imaging coupled with chemometry was shown to be a powerful tool for the prediction of drug crystallinity within SDs.

Authors+Show Affiliations

Center for Drug Evaluation and Research, Food and Drug Administration, Silver Spring, MD, USA.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Comparative Study
Journal Article
Research Support, U.S. Gov't, Non-P.H.S.

Language

eng

PubMed ID

22100517

Citation

Zidan, Ahmed S., et al. "Crystallinity Evaluation of Tacrolimus Solid Dispersions By Chemometric Analysis." International Journal of Pharmaceutics, vol. 423, no. 2, 2012, pp. 341-50.
Zidan AS, Rahman Z, Sayeed V, et al. Crystallinity evaluation of tacrolimus solid dispersions by chemometric analysis. Int J Pharm. 2012;423(2):341-50.
Zidan, A. S., Rahman, Z., Sayeed, V., Raw, A., Yu, L., & Khan, M. A. (2012). Crystallinity evaluation of tacrolimus solid dispersions by chemometric analysis. International Journal of Pharmaceutics, 423(2), 341-50. https://doi.org/10.1016/j.ijpharm.2011.11.003
Zidan AS, et al. Crystallinity Evaluation of Tacrolimus Solid Dispersions By Chemometric Analysis. Int J Pharm. 2012 Feb 28;423(2):341-50. PubMed PMID: 22100517.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Crystallinity evaluation of tacrolimus solid dispersions by chemometric analysis. AU - Zidan,Ahmed S, AU - Rahman,Ziyaur, AU - Sayeed,Vilayat, AU - Raw,Andre, AU - Yu,Lawrence, AU - Khan,Mansoor A, Y1 - 2011/11/12/ PY - 2011/09/05/received PY - 2011/11/01/revised PY - 2011/11/03/accepted PY - 2011/11/22/entrez PY - 2011/11/22/pubmed PY - 2012/6/16/medline SP - 341 EP - 50 JF - International journal of pharmaceutics JO - Int J Pharm VL - 423 IS - 2 N2 - Different destructive and nondestructive analytical methods, namely powder X-ray diffractometry (PXRD), differential scanning calorimetry (DSC), Raman and near-infrared (NIR) spectroscopy and imaging, to detect and characterize tacrolimus trace crystallinity in an amorphous solid dispersion (SD) using chemometric analysis were developed. The SD was spiked with different percentages of the crystalline drug to construct an array of SDs with different crystallinity percentages. Partial least square (PLS) regression analysis was employed to compare the performance of the calibration models created using these analytical methods. The obtained results indicated a significant interaction between tacrolimus and the employed polymer and a drug dissolution dependency on the crystalline fraction within the SDs. Using two PLS factors, these analytical methods were ranked according to its specificity to detect the trace crystallinity of SDs as NIR>PXRD>Raman>DSC. Through the application of PLS, root-mean-squared error of calibration values of 2.91%, 5.36%, 7.07% and 11.58% were calculated for the calibration models constructed by NIR, PXRD, Raman and DSC, respectively. Having a prediction error of 2.1% and a correlation coefficient of 0.99, it is demonstrated that combined NIR imaging and chemometric analysis outperformed the other methods in detecting trace crystallinity in tacrolimus amorphous systems. The spatial distributions of amorphous and crystalline drug were also obtained in order to allow for studying the crystallization dissemination in the solid dispersions. Consequently, NIR and NIR imaging coupled with chemometry was shown to be a powerful tool for the prediction of drug crystallinity within SDs. SN - 1873-3476 UR - https://www.unboundmedicine.com/medline/citation/22100517/Crystallinity_evaluation_of_tacrolimus_solid_dispersions_by_chemometric_analysis_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0378-5173(11)01039-8 DB - PRIME DP - Unbound Medicine ER -