著者
武田 豊彦 鈴木 裕介 稲津 邦平 坂元 照男 前川 秀幸
出版者
公益社団法人日本薬学会
雑誌
薬学雑誌 (ISSN:00316903)
巻号頁・発行日
vol.109, no.6, pp.p395-401, 1989-06

Cephalothine sodium (CET-Na) in crystals can be obtained by freezing the aqueous solution and subsequent warming at a fixed temperature for facilitating crystallization prior to vacuum application for drying. The product has, however, been found to unavoidably contain traces of the amorphous CET-Na, which causes a rapid color development during storage. By using thermal analysis, differential scanning calorimetry (DSC), electric conductometry, and polarized light cryomicrographic techniques, the solubilities in water, freezing point, eutectic point, and melting behavior of CET-Na in aqueous solution were investigated. The investigation demonstrated that CET-Na in supersaturated aqueous solution is very stable, and that seeding with microcrystalline CET-Na to the supersaturated solution and subsequent cooling of the mixture till its freezing point gives neither any evidence for crystallization nor for growth of the seed crystals. The freeze-drying of CET-Na in the supersaturated solution after seeding has been demonstrated to give crystalline CET-Na contaning neither of amorphous nor of quasicrystalline form.
著者
武田豊四郎講演
出版者
日本講演協會
巻号頁・発行日
1942
著者
佐藤 邦夫 狩野 敦 濱島 ちさと 関 英政 加藤 博巳 田沢 義人 加藤 智恵子 猪股 正秋 佐藤 俊一 武田 豊
出版者
Japan Gastroenterological Endoscopy Society
雑誌
日本消化器内視鏡学会雑誌 (ISSN:03871207)
巻号頁・発行日
vol.29, no.2, pp.318-327, 1987-02-20 (Released:2011-05-09)
参考文献数
66

62歳男性のDouble Pylorus(以下DP)の1例を経験した.患者は心窩部痛を主訴として来院し,X線および内視鏡検査で,幽門の小彎側に十二指腸球部に通じる瘻孔と,これに接して十二指腸潰瘍を有するいわゆるDPが確認された.この患者の10年前の内視鏡所見では幽門前部小彎に変形は認めるものの,副交通路は形成されていない.本邦では近年本症の報告が相次ぎ,1985年末で本例を含め43例にのぼる.その内訳は男32例,女11例で,自覚症状は心窩部痛,吐下血が多い.平均年齢は61.4歳で,成因は先天性2例,後天性33例,いずれとも断定していないもの8例で,副交通路の位置は幽門の小彎側33例,大彎側6例,前壁側1例,部位記載不明3例である.治療法は外科的17例,保存的26例で,最近は保存的に治療されるものが多い.幽門近傍潰瘍の穿通によって形成されるとみられる後天性DPについてはPeripyloric gastroduodenal fistulaと呼ぶのが適切と考えられる.
著者
武田 豊彦 鈴木 裕介 稲津 邦平 坂元 照男 前川 秀幸
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.109, no.6, pp.395-401, 1989-06-25 (Released:2008-05-30)
参考文献数
13
被引用文献数
2 6

Cephalothine sodium (CET-Na) in crystals can be obtained by freezing the aqueous solution and subsequent warming at a fixed temperature for facilitating crystallization prior to vacuum application for drying. The product has, however, been found to unavoidably contain traces of the amorphous CET-Na, which causes a rapid color development during storage. By using thermal analysis, differential scanning calorimetry (DSC), electric conductometry, and polarized light cryomicrographic techniques, the solubilities in water, freezing point, eutectic point, and melting behavior of CET-Na in aqueous solution were investigated. The investigation demonstrated that CET-Na in supersaturated aqueous solution is very stable, and that seeding with microcrystalline CET-Na to the supersaturated solution and subsequent cooling of the mixture till its freezing point gives neither any evidence for crystallization nor for growth of the seed crystals. The freeze-drying of CET-Na in the supersaturated solution after seeding has been demonstrated to give crystalline CET-Na contaning neither of amorphous nor of quasicrystalline form.
著者
鈴木 裕介 武田 豊彦 稲津 邦平 坂元 照男
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.110, no.11, pp.858-868, 1990-11-25 (Released:2008-05-30)
参考文献数
7

Seeding and subsequent freeze-drying of aqueous cephalothin sodium (CET-Na) solution of supersaturated concentrations, which preliminarily received an excess of mechanical stress, have been reported to make the product unacceptable in pharmaceutical elegance and in chemical stability upon storage. In order to find out the cause, the CET-Na solution that preliminarily received mechanical stress has been examined as to its crystallization behavior during freezedrying process, by using polarizedlight cryomicroscopy, scanning electron microscopy, cryodifferential scanning calorimetry, refractometry, viscositometry, and surface tensiometry. Aqueous CET-Na solution of supersaturated concentrations, to which an excess of mechanical stress was given, has been demonstrated to exhibit the following features : in the process of seeding and subsequent freeze-drying, the solution shows an incomplete crystallization at -40°C ; in the crystal growth stage at -5°C, crystals are found to be difficult to grow sufficiently from the seeds as their nuclei. These findings indicate that the supersaturated solution has changed to an unusual state upon receiving such stress, the state being different from the state of untreated solution in that the solution thus treated shows physico-chemical properties capable of easy crystallization through a simple step of freezing. The change as such in physico-chemical properties has also been estimated to have resulted from a structural change of associated molecules of CET-Na in its supersaturated solution into a condensed state quite similarly to that of liquid crystals.
著者
鈴木 裕介 武田 豊彦 稲津 邦平 坂元 照男
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.110, no.11, pp.849-857, 1990-11-25 (Released:2008-05-30)
参考文献数
13
被引用文献数
1 2

A method of seeding and subsequent freeze-drying of aqueous cephalothin sodium (CET-Na) of supersaturated concentrations was employed in an experiment with a regular production scale. The freeze-dried plugs of non-uniformity in appearance were consequently obtained together with those of white in color and in high uniformity in appearance. Such plugs of irregular shape have been found to show a marked color development during storage, and the reconstitution time was also prolonged. Scanning electron microscopy, powder X-ray diffractometry, and thermogravimetry have all demonstrated that the plugs of irregular appearance show dense aggregates of fine crystals of a high non-crystallinity by an incomplete crystal growth. Investigation has then been made with supersaturated CET-Na solution, which has preliminarily received varying mechanical stresses in varying time courses of temperature, similarly to a regular production program, for the purpouse of achieving the reproducibility of such unacceptable plugs. It has been demonstrated that by a more prolonged storage at a lower temperature of CET-Na in supersaturated solution the plug may surely contain aggregates of more fine crystallites of a higher non-crystallinity, accordingly have a higher irregularity in appearance and exhibit a more marked deterioration in pharmaceutical qualities.
著者
鈴木 裕介 武田 豊彦 稲津 邦平 坂元 照男 前川 秀幸
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.109, no.6, pp.388-394, 1989-06-25 (Released:2008-05-30)
参考文献数
10
被引用文献数
1 1

Cephalothin sodium (CET-Na) prepared according to the conventional freeze-drying methods is known to easily develop color during storage. Since amorphous CET-Na has been reported to be markedly unstable, the color development is thought to be due to the presence of traces of CET-Na in an amorphous state observed with scanning electron microscopy. Quantitation by use of the powder X-ray diffractometry of such traces of amorphous CET-Na has proved to be of little use. Thermogravimetry (TG) and differential scanning calorimetry (DSC) have demonstrated that the freeze-dried CET-Na by the conventional methods contains three types of CET-Na : amorphous (unstable phase), quasi-crystalline (metastable phase). Pyrolysis initiation temperatures of these three types of CET-Na have been demonstrated to become higher in this order. A new parameter for the evaluation of non-crystallinity of CET-Na has been introduced, in which the ratio is calculated from the data of the total weight loss observed through the pyrolysis of both amorphous and quasi-crystalline CET-Na against the total weight loss of all components during the pyrolysis of sample specimen. The ratio thus calculated is defined as "non-crystallinity". This new parameter has successfully been introduced to establish a good correlation to the degree of increasing color intensity with aging of freeze-dried CET-Na.