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Experiences with chlorpropamide with reference to its intermittent use.

F FULEIHAN·C H PLIMPTON
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ChlorpropamideHypoglycemic AgentsANTIDIABETICS/therapeutic useJournal Article

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F FULEIHAN, C H PLIMPTON. 1959-03-30. Experiences with chlorpropamide with reference to its intermittent use.. https://doi.org/10.1111/j.1749-6632.1959.tb39595.x

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PubMed2006

Effect of pressure up to 5.5GPa on dry powder samples of chlorpropamide form-A.

The effect of pressure up to 5.5GPa on a dry powder sample of chlorpropamide (4-chloro-N-((propylamino)-carbonyl)-benzenesulfonamide), form-A (sp. gr. P2(1)2(1)2(1), a=9.066A, b=5.218A, c=26.604A), was studied in situ in a Merrill-Bassett diamond anvil cell using high-resolution X-ray powder diffraction (a synchrotron radiation source at SNBL ESRF, Grenoble). No evidence of the polymorphic transformation of chlorpropamide form-A to form-C was observed. The A-C polymorphic transition on tabletting previously reported by is therefore likely to be due to local heating effects. Similarly, the phase transitions of form-A reported by to be induced by pressure applied to a sample in its saturated ethanol solution (at 0.9 and at 2.0GPa) would appear to be solvent-mediated. In the dry sample, a phase transition may be supposed to occur at pressures above 4GPa, but this requires further studies.

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PubMed2005

Quantitative determination of polymorphic composition in intact compacts by parallel-beam X-ray powder diffractometry II. Data correction for analysis of phase transformations as a function of pressure.

An analytical, non-destructive method using parallel-beam transmission powder X-ray diffractometry (PXRD) is presented for in situ whole compact detection and quantification of solid-state phase transformations in powder compacts. Accurate quantification of analyte in intact compacts using PXRD requires a mathematical correction prior to interpolation of calibration data to account for sample differences that result as a function of pressure; namely, compact thickness and solid fraction. Chlorpropamide is examined as a model system, selected because of its susceptibility to polymorphic transformations when consolidated using moderately low pressures. The results indicate that quantification of the transformed phase of chlorpropamide without corrections for solid fraction and thickness, underestimates the extent of transformation by 2.4%. Although the magnitude of the correction for this particular system of polymorphs is small, more significant values are expected for other compounds, particularly those with sufficient compactibility to allow the formation of low solid fraction calibration samples.

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