Characterization of crystal forms of -estradiol – thermal analysis, Raman microscopy, X-ray analysis and solid-state NMR

拉曼光谱 化学 结晶学 材料科学 X射线 拉曼散射 分析化学(期刊) Crystal(编程语言) 单晶 晶体结构 结晶 相变 晶体生长 X射线晶体学
作者
Narayan Varíankaval,Karl I. Jacob,Steven M. Dinh
出处
期刊:Journal of Crystal Growth [Elsevier BV]
卷期号:217 (3): 320-331 被引量:24
标识
DOI:10.1016/s0022-0248(00)00442-5
摘要

The structure and select crystalline properties of a common drug (estradiol) used in a transdermal drug delivery system are investigated. Four different crystal forms of estradiol (EA, EC, ED and EM) were prepared in the laboratory and characterized by thermal analysis, optical microscopy, Raman microspectroscopy, and solid-state NMR. Variable temperature X-ray studies were carried out on form A (EA) to determine whether the crystal structure changed as a function of temperature. These four forms exhibited different thermal behavior. EA and EC had similar melting points. This study clearly shows that water cannot be released from the crystal lattice of EA unless melting is achieved, and exposing EA to temperatures below the melting point only results in a partial release of hydrogen bonded water. EC was prepared by melting EA and subsequently cooling it to room temperature. Form EC was anhydrous, as it did not exhibit water loss, as opposed to EA, which had about 3.5% water in its crystal structure. ED was very difficult to prepare and manifested itself only as a mixture with EC. Its melting point was about 10°C lower than that of EC. It is thought to be an unstable form due to its simultaneous occurrence with EC and the inability to isolate it. EM is a solvate of methanol, not a polymorph. Its melting point was similar to EA and EC. From thermogravimetry/differential thermal analysis and differential scanning calorimetry data, it was apparent that estradiol formed a hemisolvate with methanol. All four forms had different morphologies. Raman microscopy was carried out on the different crystal forms. The spectra of EC and ED were almost identical. Thermal analysis revealed that this is due to the highly unstable nature of ED and its tendency to either convert spontaneously to EC or occur in mixtures with it.
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