臭化正ブチルスコポラミン中のスコポラミンの定量 : トロパンアルカロイドの分析研究(第7報)

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In order to examine the amount of scopolamine contained as inpurity in scopolamine-n-butyl bromide (BSB), determination method employing ultraviolet absorption was studied. About 2 g of BSB was accurately measured, and dissolved in 4 ml of water. The solution, to which 1 ml of ammonia test solution was added, was saturated with salt, and extracted five times with 10 ml of mixture of carbon tetrachloride and chloroform(1 : 2). After dehydration with anhydrous sodium sulphate, the extract was evaporated to remove the solvent on a water bath under reduced pressure. The residue was extracted five times with successive 10 ml of carbon tetrachloride. The extract was filtered and the filtrate was evaporated on a water bath under reduced pressure to remove the solvent as complete as possible. The residue, dissolved in about 10 ml of ethanol, was evaporated again to remove the solvent under reduced pressure. Another 10.0 ml of ethanol accurately measured was added to the residue, 1.5 ml of the resultant solution was accurately measured and water was added to it to make 100 ml. This was served as test solution. In another place, about 10.00 mg of reference standard of scopolamine was measured and dissolved in 4 ml of water. After addition of 1 ml of ammonia test solution, the mixture was treated just as in the case of test solution to make standard solution. The absorptions at 205 nm of the test solution and standard solution were measured using 1.5% of ethanol as a blank, it made At and As, respectively. Weight of scopolamine (mg) was calculated from following formula. weight of scopolamine (mg)=10.00 (mg)×f×At/As As: absorbance at 205 nm of standard solution, At: absorbance at 205 nm of sample solution, f: purity of standard scopolamine The experimental results revealed that recovery from the prepared test material (2.0 g of BSB with 9.75 mg of scopolamine added) was 96.5± 1.63 (average± standard deviation) by our method, and these corresponds with the result of gas chromatography.
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臭化正ブチルスコポラミン中のスコポラミンの定量 : トロパンアルカロイドの分析研究(第7報)

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