USP38附录(191)一般鉴别试验 联系客服

发布时间 : 星期六 文章USP38附录(191)一般鉴别试验更新完毕开始阅读7b380766d5bbfd0a785673a1

USP32 附录191一般鉴别试验:

主要的问题是里面的一些英文and是翻译成“和”还是“或”

Under this heading are placed tests that are frequently referred to in the Pharmacopeia for the identification of official articles. Before using any acid or base to modify the PH of the sample solution, make sure that the added substance will not interfere with the results of the test. [NOTE—The tests are not intended to be applicable to mixtures of substances unless so specified.]

此处列举的检查项目都是频繁应用于药典鉴别项下的内容。在用任何酸或基础物质调整样品溶液的PH前,要保证所加的物质不会影响到检测结果:(注:除另有规定外,不适用于混合物)

Acetate—Dissolve about 30mg of the substance to be examined in 3ml of the prescribed solution. Adjust the PH of the solution with sodium hydroxide to slightly alkaline. Add 0.25ml of lanthanum nitrate TS. If a white precipitate is formed, filter the solution. Add successively 0.1ml of iodine and potassium iodide TS 3 and 0.1ml of ammonia TS 2 to the solution. I f no blue color is observed, heat carefully to boiling. In the presence of acetates, a dark color develops or a blue precipitate is fprmed. With neureal solutions of acetates, ferric chloride TS produces a red color tha is destroyed by the addition of mineral acids. 醋酸盐:将30mg被检物溶于3ml的水中,或用3ml的规定溶液。用氢氧化钠调节PH至弱碱。加入0.25ml硝酸镧试液。如出现白色沉淀,过滤溶液。先后加入0.1ml的碘和碘化钾试液3和0.1ml的氨试液至溶液中。如没得到蓝色,小心加热至沸腾。如硝酸盐出现深色或蓝色沉淀物。取醋酸的中性溶液,加三氯化铁试液出现红色,加无机酸,红色破坏。Aluminum— With 6 N ammonium hydroxide, solutions of aluminum salts yield a

gelatinous, white precipitate that is insoluble in an excess of 6 N ammonium hydroxide. 1 N sodium hydroxide or sodium sulfide TS produces the same precipitate, which dissolves in an excess of either of these reagents.

铝:1、加入6N的氨水,应产生白色胶状沉淀,沉淀物在过量的6N的氨水中不溶。2、加入1N的氢氧化钠或硫化钠试液,应产生白色胶状沉淀,当上述试液过量时,沉淀应溶解。 Ammonium— Add 0.2g of magnesium oxide to the solution under test. Pass a current of air through the mixture, and direct the gas that escapes to just beneath the surface of an

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indicator solution, prepared by mixing 1ml of 0.1M hydrochloric acid and 0.05ml of methyl red TS2. In the presence of ammonium, the color of the indicator solution is changed to yellow. After directing the gas into the indicator solution for a sufficient period of time, add 1ml of freshly prepared sodium cobaltinitrite TS to the indicator solution. Upon the addition of the sodium cobaltinitrite TS, a yellow precipitate is formed when ammonium is present. 铵:溶液中加入0.2g氧化镁。混合物产生气体,把产生的气体通入指示剂的液面下,(指示剂配制:1ml0.1M盐酸和0.05ml的甲基红试液2.)指示液变黄色。气体通入指示液充分后,加入1ml新配的亚硝酸钴钠试液。由于亚硝酸钴钠试液的加入,铵会出现黄色沉淀物。 Antimony— With hydrogen sulfide, solutions of antimony (III) compounds, strongly acidified with hydrochloric acid, yield an orange precipitate of antimony sulfide that is insoluble in 6 N ammonium hydroxide, but is soluble in ammonium sulfide TS.

锑:三价锑溶液加盐酸酸化后,通硫化氢,应产生橘红色硫化锑沉淀,沉淀不溶于6N的氨水,可溶于硫化铵试液。

Barium— Solutions of barium salts yield a white precipitate with 2N sulfuric acid. This precipitate is insoluble in hydrochloric acid and in nitric acid. Barium salts impart a yellowish-green color to a nonluminous flame that appears blue when viewed through green glass.

钡:1、加2N硫酸,钡盐溶液产生白色沉淀。沉淀在盐酸和硝酸中不溶。2、钡盐于无色光焰中发出淡黄绿光,透过绿色玻璃观察应为蓝色。

Benzoate— In neutral solutions, benzoates yield a salmon-colored precipitate with ferric chloride TS. In moderately concentrated solutions, benzoates yield a precipitate of benzoic acid upon acidification with 2N sulfuric acid. This precipitate is readily soluble in ethyl ether.

苯甲酸盐:1、苯甲酸盐的中性溶液与三氯化铁试液反应产生赭色沉淀。2、苯甲酸盐的浓溶液被2N的硫酸酸化后应产生苯甲酸沉淀,沉淀在乙醚中易溶。 Bicarbonate— See Carbonate. 碳酸氢盐:参照碳酸盐

Bismuth— When dissolved in a slight excess of nitric acid or hydrochloric acid, bismuth salts yield a white precipitate upon dilution with water. This precipitate is colored brown by

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hydrogen sulfide, and the resulting compound dissolves in a warm mixture of equal parts of nitric acid and water.

铋:铋盐的水稀释液加入稍过量的硝酸或者盐酸,应产生白色沉淀。沉淀加入硫化氢后变为棕色,产物溶于温热的硝酸溶液(硝酸:水=1:1)。 Bisulfite— See Sulfite. 亚硫酸氢盐:参照硫酸盐。

Borate— To 1 mL of a borate solution, acidified with hydrochloric acid to litmus, add 3 or 4 drops of iodine TS and 3 or 4 drops of polyvinyl alcohol solution (1 in 50): an intense blue color is produced. When a borate is treated with sulfuric acid, methanol is added, and the mixture is ignited, it burns with a green-bordered flame.

硼酸盐:1、1ml硼酸盐溶液用盐酸酸化至对石蕊试纸显酸性,加入3-4滴碘试液和3-4滴聚乙烯醇溶液(1:50),溶液应显深蓝色。2、硼酸盐溶于硫酸,加入甲醇后点燃,火焰边缘应为绿色。

Bromide— Solutions of bromides, upon the addition of chlorine TS, dropwise, liberate bromine, which is dissolved by shaking with chloroform, coloring the chloroform red to reddish brown. Silver nitrate TS produces in solutions of bromides a yellowish–white precipitate that is insoluble in nitric acid and is slightly soluble in 6N ammonium hydroxide. 溴化物:1、溴化物溶液逐滴加入氯试液,游离出溴,用氯仿萃取,氯仿层应为红棕色。2、溴化物溶液中加入硝酸银试液,应产生浅黄色絮乳状沉淀,沉淀不溶于硝酸,微溶于6N的氨水。

Calcium— Solutions of calcium salts form insoluble oxalates when treated as follows. To a solution of the calcium salt (1 in 20) add 2 drops of methyl red TS, and neutralize with 6N ammonium hydroxide. Add 3N hydrochloric acid, dropwise, until the solution is acid to the indicator. Upon the addition of ammonium oxalate TS, a white precipitate is formed. This precipitate is insoluble in 6N acetic acid but dissolves in hydrochloric acid. Calcium salts moistened with hydrochloric acid impart a transient yellowish-red color to a nonluminous flame.

钙:按以下方式钙盐溶液形成不溶的草酸盐。钙盐溶液(1→20)中加入2滴甲基红试液,用6N的氨水中和,缓缓滴加3N的盐酸使其恰成酸性。加入草酸铵试液,应生成白色沉淀。沉淀不溶于6N乙酸,溶于盐酸。用盐酸润湿的钙盐在无色光焰中应呈砖红色。

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Carbonate— Carbonates and bicarbonates effervesce with acids, evolving a colorless gas that, when passed into calcium hydroxide TS, produces a white precipitate immediately. A cold solution (1 in 20) of a soluble carbonate is colored red by phenolphthalein TS, while a similar solution of a bicarbonate remains unchanged or is only slightly colored.

碳酸盐:1、碳酸盐与碳酸氢盐遇酸,剧烈反应,产生无色气体,通入氢氧化钙溶液中,立即产生白色沉淀。2、可溶性冷的碳酸盐溶液(1→20)加入酚酞试液显红色,同浓度的碳酸氢盐也呈现红色或略浅的红色。

Chlorate— Solutions of chlorates yield no precipitate with silver nitrate TS. The addition of sulfurous acid to this mixture produces a white precipitate that is insoluble in nitric acid, but is soluble in 6N ammonium hydroxide. Upon ignition, chlorates yield chlorides, recognizable by appropriate tests. When sulfuric acid is added to a dry chlorate, decrepitation occurs, and a greenish yellow-gas is evolved. [Caution—Use only a small amount of chlorate for this test, and exercise extreme caution in performing it. ]

氯酸盐:1、氯酸盐溶液加入硝酸银试液不会出现沉淀,当加入亚硫酸后,混合物产生白色沉淀,沉淀不溶于硝酸,可溶于6N的氨水。2、用适当的方法表明氯酸盐经点燃应产生氯化物。3、在干燥的氯酸盐上滴加硫酸,剧烈反应,并产生黄绿色气体。(警告:进行此试验应使用极小量氯酸盐,且操作时要谨慎小心。)

Chloride— With silver nitrate TS, solutions of chlorides yield a white, curdy precipitate that is insoluble in nitric acid but is soluble in a slight excess of 6N ammonium hydroxide. When testing amine (including alkaloidal) hydrochlorides that do not respond to the above test, add one drop of diluted nitric acid and 0.5 mL of silver nitrate TS to a solution of the substance being examined containing, unless otherwise directed in the monograph, about 2mg of chloride ion in 2mL: a white, curdy precipitate is formed. Centrifuge the mixture without delay, and decant the supernatant layer. Wash the precipitate with three 1-mL portions of nitric acid solution (1 in 100), and discard the washings. Add ammonia TS dropwise to this precipitate. It dissolves readily. When a monograph specifies that an article responds to the test for dry chlorides, mix the solid to be tested with an equal weight of manganese dioxide, moisten with sulfuric acid, and gently heat the mixture: chlorine, which is recognizable by the production of a blue color with moistened starch iodide paper, is evolved.

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