ORDINARY IMPURITIES翻译.docx

ORDINARY IMPURITIESTest Solution Prepare, in the solvent specified in the monograph, a solution of the substance under test having an accurately known final concentration of about 10 mg per mL. noteHeat or sonication may be used to dissolve the drug substance where use of such does not adversely affect the compound. 供试液的制备：按品种项下规定的溶剂，取适量的供试品，精密称定，用该溶剂溶解并制成最终浓度为大约10mg/ml（备注：可利用加热或者超声的方法使之完全溶解，但该方法不得给样品带来不利影响）Standard Solutions Prepare, in the solvent specified in the monograph, solutions of the USP Reference Standard or designated substance having accurately known concentrations of 0.01 mg per mL, 0.05 mg per mL, 0.1 mg per mL, and 0.2 mg per mL. noteHeat or sonication may be used to dissolve the drug substance where use of such does not adversely affect the compound. 対照液的制备：按品种项下规定的溶剂，取适量的USP标准品或指定的物质，精密称定，用该溶剂溶解并制成浓度为0.01mg/ml 0.05mg/ml 0.1mg/ml 和0.2mg/ml（备注：可利用加热或者超声的方法使之完全溶解，但该方法不得给样品带来不利影响）Procedure Use a thin-layer chromatographic plate coated with a 0.25-mm layer of chromatographic silica gel mixture, and the Eluant specified in the monograph. Apply equal volumes (20 L) of the Test Solution and Standard Solutions to the plate, using a stream of nitrogen to dry the spots. 操作过程：使用涂有一层0.25毫米厚的色谱硅胶混合物的薄层色谱板和品种项下规定的洗脱液，分别用20L的测试溶液和标准溶液点板，用氮气流吹干斑点。Allow the chromatogram to develop in a pre-equilibrated chamber until the solvent front has moved about three-fourths of the length of the plate. Remove the plate from the chamber, and air-dry. View the plate using the visualization technique(s) specified. Locate any spots other than the principal spot in the chromatogram of the Test Solution, and determine their relative intensities by comparison with the chromatograms of the appropriate Standard Solutions. See discussion above with regard to reporting and specifying total ordinary impurities.将点好样的薄层板放入加有品种项下规定的展开液（洗脱液）的展开缸中，待溶剂展开至薄层板的约四分之三处，拿出薄层板，在空气中晾干。然后用规定的可视化技术，将供试液除主斑点外的其它任意斑点与対照液的比较，看相对强度。来讨论报告和指定的总普通杂质key for visualization techniques 关键的可视化技术(1) Use UV light at 254 nm and at about 366 nm.254nm和366nm的紫外灯(2) Use Iodoplatinate TS.碘铂酸盐试液(3) Solution AMix 850 mg of bismuth subnitrate with 40 mL of water and 10 mL of glacial acetic acid.溶液A-混合850毫克碱式硝酸铋、40毫升水和冰醋酸10毫升。Solution BDissolve 8 g of potassium iodide in 20 mL of water. Mix A and B together to obtain a Stock Solution which can be stored for several months in a dark bottle. Mix 10 mL of the Stock Solution with 20 mL of glacial acetic acid, and dilute with water to make 100 mL, to prepare the spray reagent.溶液B-溶解8克碘化钾在20毫升的水中。混合A和B得到一可以在避光的瓶子中储存几个月的储备液。取10毫升的储备液于20毫升的冰醋酸中，用水稀释使成100ml，以备喷雾剂用。(4) Ninhydrin SprayDissolve 200 mg of ninhydrin in 100 mL of alcohol. Heat the plate after spraying.茚三酮喷雾-溶解茚三酮200毫克在100毫升的酒精中。喷淋后加热薄层板。(5) Acid SprayIn an ice bath, add slowly and cautiously, with stirring, 10 mL of sulfuric acid to 90 mL of alcohol. Spray the plate, and heat until charred.酸性喷雾-在冰浴里，边小心缓缓的搅拌边将10ml硫酸加入到90ml酒精中，将此喷淋到板上，加热直到焦化。(6) AcidDichromate SprayAdd sufficient potassium dichromate to 100 mL of sulfuric acid to make a saturated solution. Spray the plate, and heat until charred.重铬酸喷雾-加足量的重铬酸钾至100ml硫酸中使成饱和溶液，喷淋板，然后加热至焦化(7) VanillinDissolve 1 g of vanillin in 100 mL of sulfuric acid.香兰素-溶解1g香兰素至100ml硫酸中(8) Chloramine TTrichloroacetic AcidMix 10 mL of a 3% aqueous solution of chloramine T with 40 mL of a 25% alcoholic solution of trichloroacetic acid. Prepare immediately before use.氯胺T三氯乙酸-将10ml3%的氯胺T水溶液与40ml25%的三氯乙酸的酒精溶液混合，临用前制备。(9) Folin-CAdd 10 g of sodium tungstate and 2.5 g of sodium molybdate to 70 mL of water, add 5 mL of 85% phosphoric acid and 10 mL of 36% hydrochloric acid, and reflux this solution for 10 hours.Folin-C（是一种显色剂）- 加10 g的钨酸钠和2.5克钼酸钠至70毫升的水中,加入5毫升的85%磷酸和10毫升36%的盐酸，回流10个小时。(10) KMnO4Dissolve 100 mg of Potassium Permanganate in 100 mL of water.高锰酸钾-溶解100mg的高锰酸钾到100ml水中(11) DABMix 1 g of p-dimethylaminobenzaldehyde in 100 mL of 0.6 N hydrochloric acid.DAB-将1g 对二甲氨基苯甲醛加到100ml0.6N的盐酸中，混合。(12) DACMix 100 mg of p-dimethylaminocinnamaldehyde in 100 mL of 1 N hydrochloric acid.DAC-将100Mg的对二甲氨基肉桂醛加到100ml 1N 的盐酸中，混合。(13) FerricyanideMix equal volumes of a 1% ferric chloride solution and a 1% potassium ferricyanide solution. Use immediately.铁氰化物-混合等体积的1%的氯化铁溶液和1%铁氰化钾溶液，立即使用。(14) Fast Blue BReagent ADissolve 500 mg of Fast Blue B Salt in 100 mL of water.Reagent B0.1 N sodium hydroxide.Spray first with A, then with B.坚固兰：试剂A-溶解500mg坚固兰盐到100ml水中。 试剂B-0.1N氢氧化钠先喷A，然后喷B(14) Alkaline Ferric CyanideDilute 1.5 mL of a 1% potassium ferricyanide solution with water to 20 mL, and add 10 mL of 15% sodium hydroxide solution.碱性铁氰化物-将1.5ml的1%铁氰化钾溶液用水稀释到20ml，然后加入15%的氢氧化钠溶液15ml。(15) Iodine SprayPrepare a 0.5% solution of iodine in chloroform. 碘喷雾-用氯仿制备0.5%的碘溶液(16) Expose the plate for 10 minutes to iodine vapors in a pre-equilibrated closed chamber, on the bottom of which there are iodine crystals.将板暴露在底部有碘晶体的碘蒸气预平衡室中。 (18) Solution ADissolve 0.5 g of potassium iodide in 50 mL of water.Solution BPrepare a solution of 0.5 g of soluble starch in 50 mL of hot water.Just prior to use, mix equal volumes of Solution A and Solution B.溶液A-溶解0.5g的碘化钾于50ml水中。溶液B-将0.5g的可溶性淀粉溶于50ml热水中使用前，取相同体积的A和B混合(19) PTSSDissolve 20 g of p-toluenesulfonic acid in 100 mL of alcohol, spray the plate, dry for 15 minutes at 110, and view under UV light at 366 nm.PTSS-溶解20g 对甲苯磺酸于100ml酒精中，喷淋板，110度干燥15min,然后再366nm紫外灯下检视。(20) o-Tolidine SprayDissolve 160 mg of o-tolidine in 30 mL of glacial acetic acid, dilute with water to make 500 mL, add 1 g of potassium iodide, and mix until the potassium iodide has dissolved.邻联甲苯胺喷雾-溶解 160mg的邻联甲苯胺于30ml的冰醋酸中,用水稀释至500毫升,加1g碘化钾,混合，直到碘化钾溶解(21) Mix 3 mL of chloroplatinic acid