巻号一覧
10 巻, 4 号
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富山 新一1964 年 10 巻 4 号 p. 219-229
発行日: 1964/12/30
公開日: 2008/05/30
ジャーナル フリーPDF形式でダウンロード (1655K) -
菅野 三郎, 屋宮 妙子, 詫摩 真澄1964 年 10 巻 4 号 p. 230-235
発行日: 1964/12/30
公開日: 2008/05/30
ジャーナル フリーThe differential determination of aminopyrine and sulpyrin in pharmaceutical preparations were investigated. The determination is based on the principle that aminopyrine and sulpyrin are colored with ferric ferricyanate solution. Aminopyrine and sulpyrin were separated by treatment with chloroform because the former is soluble in chloroform while the later insoluble. Aminopyrine dissolved in 0.01% sulfuric acid solution after the evaporation of chloroform was colored with ferric ferricyanate. Sulpyrin insoluble in chloroform was hydrolyzed to monomethylaminoantipyrine, extracted with chloroform and treated in the same manner as aminopyrine. Each of the colored solutions obtained from the sample and the standard solution (aminopyrine or sulpyrin 10 μg/ml), after ethanol was added for the prevention of precipitation of the pigment, were allowed to stand for about 60 minutes at 20∼30° and then determined respectively at 710 mμ. The recoveries of aminopyrine and sulpyrin in pharmaceutical preparations were 93∼103%.抄録全体を表示PDF形式でダウンロード (706K) -
辻 章夫, 中村 晃忠, 和田 秋枝, 加藤 せえ, 沢田 弘1964 年 10 巻 4 号 p. 236-241
発行日: 1964/12/30
公開日: 2008/05/30
ジャーナル フリーA spectrophotometric method for determination of N-Acetyl-p-aminophenol (NAAP) in pharmaceutical preparations is described. NAAP was oxidized by HNO2 in acidic solution to give an yellow color which was changed to orange-yellow by addition of strongly alkaline solution and determined spectrophotometrically at 437 mμ. With this method, NAAP in the range 7∼28 μg/ml could be determined within a standard deviation of ±0.77%. Because of its simplicity and rapidity, this method is well suited for analysis of NAAP in complex pharmaceutical preparations of antipyretic analgesics. Influences of about forty compounds, which are used with NAAP, were examined. Aminopyrine and sulpyrine interfer this method, but aminopyrine can be separated by extraction and a sample containing sulpyrine can be successfully determined by extracting with CHCl3 after heating with diluted hydrochloric acid.抄録全体を表示PDF形式でダウンロード (726K) -
辻 章夫, 北條 正躬1964 年 10 巻 4 号 p. 241-246
発行日: 1964/12/30
公開日: 2008/05/30
ジャーナル フリーSpectrophotometric methods for determination of N-Acetyl-p-aminophenol (NAAP) in pharmaceutical preparations are described. NAAP was hydrolysed by refluxing with HCl to produce p-aminophenol which reacts with Na3 [Fe (CN)5NH3] in alkaline solution to give a blue-green color (λmax : 700 mμ), or condenses with phenol in alkaline solution to produce a blue indophenol dye (λmax : 620 mμ). NAAP in pharmaceutical preparations could be determined by these methods within a standard deviation of ±0.6%. Influences of about forty compounds, which are used with NAAP, were examined. Sulpyrine interferes this method but its interference can be eliminated by using the standard solution containing the same amount of sulpyrine.抄録全体を表示PDF形式でダウンロード (728K) -
呉地 伝夫, 加藤 昌宏, 荻野 喜文1964 年 10 巻 4 号 p. 247-251
発行日: 1964/12/30
公開日: 2008/05/30
ジャーナル フリーIn the previous paper the separation analysis of antioxidants by thin-layer chromatography was reported. The present report deals with the gas chromatographic analysis of BHA and BHT. Separation and simultaneous determination of BHA and BHT were investigated by using commercial thermo 1-1 (Shimadzu) as a stationary liquid and methyl caprate as a internal standard. Average recovery rates of BHA and BHT from edible oil were 98.4 and 92.9 per cent, and the standard deviations were 1.9 and 1.2 per cent respectively.抄録全体を表示PDF形式でダウンロード (635K) -
山根 靖弘, 本宮 幸子, 馬場 紀子1964 年 10 巻 4 号 p. 251-253
発行日: 1964/12/30
公開日: 2008/05/30
ジャーナル フリーThe reaction product from vitamin B1 and cupric ion was found to give a red fluorescence and this relatively sensitive and selective reaction was applied to the detection of vitamin B1. A few milligrams of sample containing vitamin B1 were dissolved in about 1 ml of water and added one drop of 0.1% thymolphthalein solution. To the sample solution, 0.1 N sodium hydroxide solution was added drop by drop until the solution turned blue and two more drops were added. The thiolized solution was prepared by heating the sample solution in a water bath at 50-90° for 30 seconds. One drop of 0.5% cupric sulfate solution was put on a filter paper and after drying the paper, one drop of the thiolized solution was added on the spot. After 1-2 minutes, the red fluorescence was observed. The limit of identification was 3 μg (60μg/ml). This reaction is interfered by mercury, iron, sulfur-bearing compounds and vitamin B2.抄録全体を表示PDF形式でダウンロード (470K) -
小山 隆1964 年 10 巻 4 号 p. 254-257
発行日: 1964/12/30
公開日: 2008/05/30
ジャーナル フリーThe reaction of acetylacetone reagent with hexamine (hexamethylenetetramine) was investigated. Hexamine dissolved in acetylacetone reagent is decomposed rapidly on heating in boiling water bath to liberate HCHO which reacts with the reagent, while the liberation of HCHO from hexamine at 60° is considerably slow. Aqeous solutions of hexamine and HCHO were individually reacted with acetylacetone reagent in boiling water bath for ten minutes and the extinctions at 425 mμ of the reaction mixtures were measured. The calibulation curve of hexamine is identical with that of HCHO. DDL (3, 5-diacetyl-1, 4-dihydrolutidine) produced in the reaction mixture is gradually decomposed on heating in boiling water bath, and then the extinction decreases slowly, but the decrease could be neglected for determining HCHO. Hexamine is obtainable in pure crystalline form, and is sufficiently stable in aqueous solution. Therefore, it is considered that hexamine is a excellent standard substance for determining HCHO by acetylacetone reaction. The results of the present investigation also indicate that hexamine itself can be determined by acetylacetone reaction.抄録全体を表示PDF形式でダウンロード (527K) -
菅野 三郎, 渡辺 重信, 村井 絢子1964 年 10 巻 4 号 p. 258-260
発行日: 1964/12/30
公開日: 2008/05/30
ジャーナル フリーThe gas chromatography was applied to the separation of phenacetin and acetanilide which are coexisting in the same pharmaceutical preparation. The calibration curves of phenacetin and acetanilide were obtained by adopting 2-naphthyl methyl ether as the internal standard substance. The recovery of phenacetin was 94∼100% and that of acetanilide 93∼102%.抄録全体を表示PDF形式でダウンロード (421K) -
呉地 伝夫, 荻野 喜文1964 年 10 巻 4 号 p. 261-265
発行日: 1964/12/30
公開日: 2008/05/30
ジャーナル フリーSeparation analysis of nine kinds of antioxidants and quantitative determination of BHA were investigated by means of silica gel thin-layer chromatography. Benzene-ether (1 : 2) and chloroform-ether (1 : 3) were found as suitable solvent systems for two dimensional chromatography, and the minimum amount for identification was 1 μg per ml. For determination of BHA, 2, 6-dichloroquinone 4-chlorimide were used as a color reagent and the colored spot was scraped off from the plate, extracted with ether and determined spectrophotometrically.抄録全体を表示PDF形式でダウンロード (525K) -
中澤 泰男, 中島 玲子1964 年 10 巻 4 号 p. 266-267
発行日: 1964/12/30
公開日: 2008/05/30
ジャーナル フリーThin-layer chromatography was applied to a simultaneous identification of 5-substituted barbituric acids which are used as hypnotics. Silver nitrate-impregnated silica gel layer was found to be adequate for this purpose and the suitable solvent systems were also investigated. Separative analysis of these compounds could be made by means of the silica gel layer with a combination of two or three kinds of the solvent systems.抄録全体を表示PDF形式でダウンロード (388K)
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