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Preparation and crystallographic analysis of gliclazide polymorphs.

Rajamma AJ, Sateesha SB, Narode MK, Prashanth VR, Karthik AM - Indian J Pharm Sci (2015 Jan-Feb)

Bottom Line: Polymorph Form-I is found to exist in centro-symmetric triclinic P-1 space group and has endothermic peak at 162.93°.Form-II and Form-III are relatively most stable and least soluble.However, there was no remarkable difference in their aqueous solubility under the conditions in which study was conducted.

View Article: PubMed Central - PubMed

Affiliation: Department of Pharmacognosy, KLEU's College of Pharmacy, Bangalore-560 010, India.

ABSTRACT
Since the introduction of gliclazide in the pharmaceutical industry, a large number of research groups have been engaged in various investigations aiming to enhance its biomedical application. But, very limited efforts have been made to study polymorphism of gliclazide. Therefore, this study focuses on solvent-induced polymorphism of gliclazide and its characterization by thermal methods. Three polymorphs namely, Form-I, II and III and an amorphous powder were produced from different solvents and solvent mixtures. Crystals were analyzed using infrared spectroscopy, differential scanning calorimetry, X-ray powder diffraction and single crystal x-ray diffraction. Polymorph Form-I is found to exist in centro-symmetric triclinic P-1 space group and has endothermic peak at 162.93°. Form-II has endothermic peak from 171.2° to 172.35° and exists in centro-symmetric monoclinic P21/a space group while Form-III has endothermic peak from 168.93° to 169.86° and exists in centro-symmetric monoclinic P21/n space group. The equilibrium solubility values of Form-I, II, III and the amorphous form were 0.4825±0.025, 0.2341±0.042, 0.2581±0.038 and 0.5213±0.072 mg/ml, respectively. The Form-I has relatively higher solubility and similar to that of amorphous gliclazide. Form-II and Form-III are relatively most stable and least soluble. However, there was no remarkable difference in their aqueous solubility under the conditions in which study was conducted.

No MeSH data available.


DSC curves of gliclazide crystals.(a) Crystal prepared from chloroform, (b) crystal prepared from acetone, and (c) amorphous form of gliclazide.
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Figure 3: DSC curves of gliclazide crystals.(a) Crystal prepared from chloroform, (b) crystal prepared from acetone, and (c) amorphous form of gliclazide.

Mentions: DSC is an extremely important analytical tool for measuring the wide variety of transitions in pharmaceutical materials[15]. DSC data can derive useful information in identifying the polymorphs. The DSC scans of all the crystals and raw material are shown in figs. 2 and 3. The DSC endothermic details of gliclazide crystals are presented in Table 1. The DSC curve of the gliclazide crystal prepared from ethanol shows a sharp endothermic peak at 162.93° with an insignificant peak at 124.80°. This form is designated here as the polymorph-I. The DSC curve of the polymorph-II, which is obtained by crystallization from methanol, exhibits a single sharp endotherm at 171.20°. This polymorph can also be obtained from acetone, it shows melting endothermic peak at 172.35°.


Preparation and crystallographic analysis of gliclazide polymorphs.

Rajamma AJ, Sateesha SB, Narode MK, Prashanth VR, Karthik AM - Indian J Pharm Sci (2015 Jan-Feb)

DSC curves of gliclazide crystals.(a) Crystal prepared from chloroform, (b) crystal prepared from acetone, and (c) amorphous form of gliclazide.
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC4355880&req=5

Figure 3: DSC curves of gliclazide crystals.(a) Crystal prepared from chloroform, (b) crystal prepared from acetone, and (c) amorphous form of gliclazide.
Mentions: DSC is an extremely important analytical tool for measuring the wide variety of transitions in pharmaceutical materials[15]. DSC data can derive useful information in identifying the polymorphs. The DSC scans of all the crystals and raw material are shown in figs. 2 and 3. The DSC endothermic details of gliclazide crystals are presented in Table 1. The DSC curve of the gliclazide crystal prepared from ethanol shows a sharp endothermic peak at 162.93° with an insignificant peak at 124.80°. This form is designated here as the polymorph-I. The DSC curve of the polymorph-II, which is obtained by crystallization from methanol, exhibits a single sharp endotherm at 171.20°. This polymorph can also be obtained from acetone, it shows melting endothermic peak at 172.35°.

Bottom Line: Polymorph Form-I is found to exist in centro-symmetric triclinic P-1 space group and has endothermic peak at 162.93°.Form-II and Form-III are relatively most stable and least soluble.However, there was no remarkable difference in their aqueous solubility under the conditions in which study was conducted.

View Article: PubMed Central - PubMed

Affiliation: Department of Pharmacognosy, KLEU's College of Pharmacy, Bangalore-560 010, India.

ABSTRACT
Since the introduction of gliclazide in the pharmaceutical industry, a large number of research groups have been engaged in various investigations aiming to enhance its biomedical application. But, very limited efforts have been made to study polymorphism of gliclazide. Therefore, this study focuses on solvent-induced polymorphism of gliclazide and its characterization by thermal methods. Three polymorphs namely, Form-I, II and III and an amorphous powder were produced from different solvents and solvent mixtures. Crystals were analyzed using infrared spectroscopy, differential scanning calorimetry, X-ray powder diffraction and single crystal x-ray diffraction. Polymorph Form-I is found to exist in centro-symmetric triclinic P-1 space group and has endothermic peak at 162.93°. Form-II has endothermic peak from 171.2° to 172.35° and exists in centro-symmetric monoclinic P21/a space group while Form-III has endothermic peak from 168.93° to 169.86° and exists in centro-symmetric monoclinic P21/n space group. The equilibrium solubility values of Form-I, II, III and the amorphous form were 0.4825±0.025, 0.2341±0.042, 0.2581±0.038 and 0.5213±0.072 mg/ml, respectively. The Form-I has relatively higher solubility and similar to that of amorphous gliclazide. Form-II and Form-III are relatively most stable and least soluble. However, there was no remarkable difference in their aqueous solubility under the conditions in which study was conducted.

No MeSH data available.