Rietveld Method in the Analysis of Polymorphism in Mebendazole Tablets Acquired in Brazil’s Drugstores

Salvi, Simone T. B.; Antonio, Selma G.; Ferreira, Fabio F.; Paiva-Santos, Carlos O.

doi:10.5935/0103-5053.20150151

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Journal of the Brazilian Chemical Society

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Articles • J. Braz. Chem. Soc. 26 (9) • Sept 2015 • https://doi.org/10.5935/0103-5053.20150151 copy

Rietveld Method in the Analysis of Polymorphism in Mebendazole Tablets Acquired in Brazil’s Drugstores

Authorship SCIMAGO INSTITUTIONS RANKINGS

Mebendazole (MBZ) is an anthelmintic medicine known to exhibit the polymorphs A, B and C, where polymorph C is the one indicated for tablets. Mebendazole commercial tablets (references, generics and similars) were analyzed in this work using X-ray powder diffraction data and the Rietveld method (RM) aiming at characterizing and quantifying crystal phases. Form C was found in mixture with form A in formulations of 500 mg (reference and generic). One of the generics presented a batch with form B and another one with form C. All the other tablets presented form A.

Keywords:
X-ray powder diffractometry; polymorphism; mebendazole; Rietveld method

Drug class	Sample code	Date of manufacture	Date of expiration	Presentation / mg
Reference	R-01	11/2008	11/2013	500
Reference	R-02	7/2008	7/2011	100
Generic	G-01	10/2009	10/2012	100
Generic	G-02 batch L1	5/2009	5/2011	100
Generic	G-02 batch L2	2/2010	2/2012	100
Generic	G-02 batch L3	5/2010	5/2012	100
Generic	G-03	11/2007	11/2010	500
Generic	G-04	8/2008	8/2010	100
Generic	G-05	10/2009	10/2012	100
Similar	S-01 batch M1	6/2009	6/2011	100
Similar	S-01 batch M2	8/2009	8/2011	100
Similar	S-01 batch M3	12/2009	12/2011	100
Similar	S-02	7/2008	7/2011	100

Unit cell parameter	Form A¹²	Form C¹³	Lactose^a a α-Lactose monohydrate. ²⁹	β-D-Mannitol³⁰	Talc
a	5.5044(2) Å	5.1480(9) Å	7.982(2)Å	8.672(8)Å	5.293(3)Å
b	11.2872(2) Å	7.8779(15) Å	21.562(3)Å	16.875(1)Å	9.179(3)Å
c	12.5276(5) Å	17.907(3) Å	4.824(1)Å	5.560(5)Å	9.469(3)Å
α	66.694(2)°	82.425(6)°	90°	90°	90°
β	82.959(2)°	82.743(7)°	109.57(3)°	90°	90°
γ	78.444(2)°	71.091(13)°	90°	90°	90°
Z	2	–	2	4	2
Space group	P 1	P 1	P2₁	P2₁2₁2₁	C 1

Form B⁸
Diameter / Å	Intensity (I100) / %
14.62	60
9.36	83
7.26	42
7.08	47
4.65	100
4.55	42
4.21	46
4.11	63
3.92	46
3.62	67
3.52	50
3.11	40
3.09	43

	R_wp / %	χ²	Form A [RP]^a a The relative percentage of API in the tablets can be found in square brackets: [RP]; / %	Form C [RP]^a a The relative percentage of API in the tablets can be found in square brackets: [RP]; / %	Mannitol / %	Talc / %	Lactose / %	Mg St^b b Mg St: magnesium stearate; / %
R-01	10.84	1.56	.5(3) [4.5]	95.5(3) [95.5]	−	−	−	−
R-02	15.52	3.75	50 (3) [100]	−	43.79(3)	5.8(6)	−	−
G-01	12.04	2.02	65.6(7) [100]	−	28.8(6)	5.6(2)	−	N.Q.^c c N.Q.: identified, but not quantified.
G-02-L1	12.69	2.69	3.9(3) [42.4]	5.3(3) [57.6]	90.72(5)	−	−	−
G-02-L2	9.67	.36	−	66.2(3) [100]	33.8(3)	−	−	−
G-02-L3	11.17	3.71	−	68.7(6) [100]	31.3(5)	−	−	−
G-03	11.68	2.91	4.5(3) [5]	84.4(7) [95]	−	2.1(2)	8.9(6)	−
G-04	9.84	1.37	94.1(4) [100]	−	−	5.9(4)	−	−
G-05	12.00	2.46	100 [100]	−	N.Q.^c c N.Q.: identified, but not quantified.	−	−	N.Q.^c c N.Q.: identified, but not quantified.
S-01-M1	9.38	3.86	90.7(3) [100]	−	−	−	9.3(3)	−
S-01-M2	6.75	1.56	85(1) [100]	−	−	2(1)	13(1)	−
S-01-M3	11.47	2.75	100 [100]	−	−	−	−	−
S-02	10.30	1.46	93.7(4) [100]	−	6.3(4)	−	−	−

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