Analysis of polymorphic contamination in meloxicam raw materials and its effects

on the physicochemical quality of drug product

Jennifer T. Jacon Freitasa; Olimpia M. M. Santos Vianaa,b; Rudy Bonfilioa; Antônio Carlos Doriguettoa,b*;

Magali Benjamim de Araújoa.

aFaculty of Pharmaceutical Sciences, Federal University of Alfenas (UNIFAL-MG), 37130-001, Alfenas-

MG, Brazil; Phone number: +55 35 3701-9520bInstitute of Chemistry, Federal University of Alfenas (UNIFAL-MG), 37130-001, Alfenas-MG, Brazil;

Phone number: +55 35 3701-9717

* Corresponding author doriguetto@unifal-mg.edu.br

E-mail addresses: jenniferjaconfreitas@gmail.com (J. Freitas), olimpia_martins@yahoo.com.br (O.

Viana), rudy@unifal-mg.edu.br (R. Bonfilio), doriguetto@unifal-mg.edu.br (A. Doriguetto),

magali@unifal-mg.edu.br (M. Araújo).

SUPPLEMENTAL MATERIAL

(a)

(b)

Fig. S1 Experimental PXRD patterns of the residual solid materials in equilibrium with the solution

prepared from (a) MLX B01 and (b) MLX B04 in the media used to probe their equilibria solubility. The

diffractograms are compared to the calculated PXRD pattern of the MLX Forms I and the experimental

PXRD pattern of the MLX B04 (mixture of the MLX Forms I and III).

FIG.S2 Experimental PXRD patterns of the residual solid material remaining in the discs used to probe

the intrinsic dissolution of the MLX B01 and MLX B04. The diffractograms are compared to the

calculated PXRD pattern of the MLX Forms I and the experimental PXRD pattern of the MLX B04

(mixture of the MLX Forms I and III).

(a)

(b)

Fig. S3 Experimental PXRD patterns of the MLX APIs B01, B02, B03 and B05 after (a) three months

and (b) six months of wrapping in a climatic chamber under controlled humidity and temperature

conditions compared to the calculated PXRD pattern of the MLX Forms I. The diffractograms are

compared to the calculated PXRD pattern of the MLX Forms I and IV (hydrated form reported by Luger

et al., 1996); and to the experimental PXRD pattern of the MLX B04 (mixture of the MLX Forms I and

III).

(a)

(b)

Fig. S4 ATR-FTIR spectra of APIs meloxicam after (a) three months and (b) six months in a study of

polymorphic stability.

(a)

(b)

Fig. S5 DSC curves APIs meloxicam after (a) three months and (b) six months stability study under

conditions of 40 °C and relative humidity of 75%.

Fig. S6 Experimental PXRD patterns of the residue filtered from the slurry prepared with MLX B01

(pure MLX Forms I) in pH 7.5 phosphate buffer.