著者
桑野 晴光 田村 千尋
出版者
公益社団法人 日本薬学会
雑誌
YAKUGAKU ZASSHI (ISSN:00316903)
巻号頁・発行日
vol.81, no.5, pp.764-767, 1961-05-25 (Released:2010-02-19)
参考文献数
5
被引用文献数
2 2

Polymorphism of chloramphenicol was examined by the X-ray diffraction method and quantitative relationship between the two crystal forms was examined. In general, proportionation of concentration to diffraction intensity can be quantitated in polymorphs but the method was inconvenient for use with organic compounds due to strict packing conditions. In the binary system (α- and β-forms) of chloramphenicol palmitate, specific intensity and specific concentration of the component were in proportion and quantitative straight line independent of packing codition was obtained. This was found to be effective in the range of over 3% of the β-form and precision is within 1%. As the quantitative linear equation: the following was obtained: xβ/xα=(0.347±0.005)⋅Iβ/Iα, where x is the concentration of the component and I is the intensity of reflection.
著者
田村 千尋 桑野 晴光
出版者
公益社団法人 日本薬学会
雑誌
YAKUGAKU ZASSHI (ISSN:00316903)
巻号頁・発行日
vol.81, no.5, pp.759-764, 1961-05-25 (Released:2010-02-19)
参考文献数
6
被引用文献数
1 1

From the consideration of X-ray diffraction, infrared absorption spectra, and various transition conditions of long-chain esters of chloramphenicol, and some assumptions were made on their crystal structure.1) According to X-ray diffraction, all-trans configuration for the long-chain portion of the β-form molecule results in good agreement between the molecular models and the long axis by X-ray measurement. In the case of α-form, the long axis of the crystal cannot be explained unless the molecule is assumed to have some cis linkages or the long chain part is a trans structure but deeply twined with each other.2) Infrared absorption spectra suggest that the α-form is closely resembled to a solution state and crystals with a cis configuration, having distorted molecule, may be assumed. The β-form is considered to have a higher order molecular arrangement as a crystal and it is convenient to assume an all-trans configuration by X-ray measurement.3) Stability of the β-form can be assumed form the measurement of melting point and specific gravity. On the other hand, similarity to the α-form and solution state (or amorphous state) as found from transition conditions and these agree well with the above two measurements.
著者
田村 千尋 桑野 晴光
出版者
公益社団法人 日本薬学会
雑誌
YAKUGAKU ZASSHI (ISSN:00316903)
巻号頁・発行日
vol.81, no.5, pp.755-759, 1961-05-25 (Released:2010-02-19)
参考文献数
6
被引用文献数
13 19

It was found that chloramphenicol palmitate, myristate, and caprylate come in two kinds of crystalline form and one amorphous form. These compounds were prepared and their transition conditions were examined.1) When the crystals is dissolved in a solvent and crystallized out, optional form of crystals can be obtained by controlling crystallization rate and this form is not affected by polarity or pH of the solvent. Crystals of α-form is obtained by rapid crystallization while the β-form is obtained by gradual crystallization. When a small amount is fused and cooled rapidly in a refrigerator, a vitrious substance is obtained.2) Transition between the solids occur only in the direction of amorphous to α-form to β-form, and there is no reverse progress. The transition rate is faster, the nearer the melting point. The mechanism of such a transition is thought to be the transition to a stable form by the heat motion of the molecule itself. The transition rate becomes suddenly rapid after formation of β-form crystal and this is considered to be due to added effect of catalytic transition.
著者
津田 恭介 生熊 晋 河村 正朗 太刀川 隆治 酒井 浄 田村 千尋 甘粕 治
出版者
The Pharmaceutical Society of Japan
雑誌
Chemical and Pharmaceutical Bulletin (ISSN:00092363)
巻号頁・発行日
vol.12, no.11, pp.1357-1374, 1964-11-25 (Released:2008-03-31)
被引用文献数
126 208

The structures of both tetrodonic acid hydrobromide and 6, 11-diacetylanhydrotetrodotoxin hydroiodide were established by chemical and X-ray crystallographical research. Based upon structures of both these salts and upon other chemical information, we determined that tetrodotoxin and anhydrotetrodotoxin have zwitterionic hemilactal structures.