Beruflich Dokumente
Kultur Dokumente
Centro de Ciências Naturais e Humanas (CCNH), Universidade Federal do ABC (UFABC), Santo André, SP CEP: 09210-580, Brazil
ABSTRACT: With the use of X-ray powder diffraction data and the Rietveld method, we verified that both microcrystalline cellulose PH-
101 and PH-102 presented differences in the crystallinity degree. The results revealed these samples are semicrystalline in nature and via
Rietveld refinements, it was possible, adding a known amount of an internal standard of corundum to the samples, to perform quantitative
phase analyses, which allowed us to determine the amorphous amount of the studied samples: 63.7(11) wt % in microcrystalline cellulose
PH-101 and 51.0(11) wt % in microcrystalline cellulose PH-102. An important contribution of this work refers to the attempt of using
this simple method, permitting to evaluate the degree of crystallinity of microcrystalline cellulose.
C 2014 Wiley Periodicals, Inc. and the
The crystal and molecular structures of the cellulose I" have Structure Database (ICSD) were used; the structural char-
R
been established using synchrotron and neutron diffraction acterization of samples and the evaluation of the amorphous
data recorded from oriented fibrous samples prepared by align- amount were carried out by means of the Rietveld method21,22
ing cellulose microcrystals from the cell wall of fresh water alga using XRPD data and the Topas-Academic v. 523 software pro-
Glaucocystis nostochinearum.20 Cellulose I" crystallizes in a tri- gram. First, we refined the unit cell parameters and the zero
clinic unit cell: a = 10.400(10) Å; b = 6.717(6) Å; c = 5.962(7) Å; point of the diffractometer. The background was fitted using
" = 80.37(5)◦ ; $ = 118.08(5)◦ ; and ( = 114.80(5)◦ , having space a 12-term Chebyshev polynomial. The peak asymmetry was
group P1. adjusted using the simple axial divergence model of Cheary
It should be mentioned that the determination of the crys- and Coelho.24,25 The peak profiles were modeled using the
tal structure of cellulose by X-ray diffraction played an impor- fundamental-parameter approach25 and the preferred orienta-
tant role in the polymer science and the concept of long-chain tion of the crystals were corrected with a fourth-order spherical
molecules. In order to verify such statements and information, harmonics function. The isotropic atomic displacements (Biso )
which may serve as a subsidy for the pharmaceutical industries, of all nonhydrogen atoms were fixed to 2.8. For the hydrogen
quantitative phase analyses by means of X-ray powder diffrac- atoms, the Biso values were assumed to be 1.2 times larger than
tion (XRPD) data and the Rietveld method were used to eval- the values of the nonhydrogen atoms.
uate the amorphous amount of both microcrystalline cellulose
PH-101 and microcrystalline cellulose PH-102. Also, FTIR was
used to follow their possible differences in absorption bands. RESULTS AND DISCUSSION
Fourier Transform Infrared Spectroscopy
MATERIALS AND METHODS
The FTIR spectra for microcrystalline cellulose PH-101 and
Powdered samples of microcrystalline cellulose PH-101 and microcrystalline cellulose PH-102 samples are shown in
PH-102 (Avicel from FMC BioPolymers) were kindly provided
R
Figure 3.
DOI 10.1002/jps.23909 De Figueiredo and Ferreira, JOURNAL OF PHARMACEUTICAL SCIENCES 103:1394–1399, 2014
1396 RESEARCH ARTICLE – Pharmaceutics, Drug Delivery and Pharmaceutical Technology
De Figueiredo and Ferreira, JOURNAL OF PHARMACEUTICAL SCIENCES 103:1394–1399, 2014 DOI 10.1002/jps.23909
RESEARCH ARTICLE – Pharmaceutics, Drug Delivery and Pharmaceutical Technology 1397
DOI 10.1002/jps.23909 De Figueiredo and Ferreira, JOURNAL OF PHARMACEUTICAL SCIENCES 103:1394–1399, 2014
1398 RESEARCH ARTICLE – Pharmaceutics, Drug Delivery and Pharmaceutical Technology
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DOI 10.1002/jps.23909 De Figueiredo and Ferreira, JOURNAL OF PHARMACEUTICAL SCIENCES 103:1394–1399, 2014