主题：【求助】有没有用美国药典做甘油分析的?

有同样需求！！！！！

原文由 liang96(liang96) 发表:
参考USP30,测定甘油,都是英文的,不知道哪位有没有翻译成中文的,敬请上传一下,不胜感谢!

楼主，你有英文的么，能分享份给偶么，谢谢啦，拜托哇

原文由 taohuihui1128(taohuihui1128) 发表:

原文由 liang96(liang96) 发表:
参考USP30,测定甘油,都是英文的,不知道哪位有没有翻译成中文的,敬请上传一下,不胜感谢!

楼主，你有英文的么，能分享份给偶么，谢谢啦，拜托哇

以下USP32英文

Sodium periodate solution— Dissolve 60 g of sodium metaperiodate in sufficient water containing 120 mL of 0.1 N sulfuric acid to make 1000 mL. Do not heat to dissolve the periodate. If the solution is not clear, pass through a sintered-glass filter. Store the solution in a glass-stoppered, light-resistant container. Test the suitability of this solution as follows. Pipet 10 mL into a 250-mL volumetric flask, dilute with water to volume, and mix. To about 550 mg of Glycerin dissolved in 50 mL of water add 50 mL of the diluted periodate solution with a pipet. For a blank, pipet 50 mL of the solution into a flask containing 50 mL of water. Allow the solutions to stand for 30 minutes, then to each add 5 mL of hydrochloric acid and 10 mL of potassium iodide TS, and rotate to mix. Allow to stand for 5 minutes, add 100 mL of water, and titrate with 0.1 N sodium thiosulfate, shaking continuously and adding 3 mL of starch TS as the endpoint is approached. The ratio of the volume of 0.1 N sodium thiosulfate required for the glycerin–periodate mixture to that required for the blank should be between 0.750 and 0.765.

Procedure— Transfer about 400 mg of Glycerin, accurately weighed, to a 600-mL beaker, dilute with 50 mL of water, add bromothymol blue TS, and acidify with 0.2 N sulfuric acid to a definite green or greenish yellow color. Neutralize with 0.05 N sodium hydroxide to a definite blue endpoint, free from green color. Prepare a blank containing 50 mL of water, and neutralize in the same manner. Pipet 50 mL of the Sodium periodate solution into each beaker, mix by swirling gently, cover with a watch glass, and allow to stand for 30 minutes at room temperature (not exceeding 35[img=7,20]mk:@MSITStore:E:\专业及相关\甘油文献\甘油及衍生物标准\USP32-NF27.chm::/pub/data/images/chars/deg.gif[/img]) in the dark or in subdued light. Add 10 mL of a mixture of equal volumes of ethylene glycol and water, and allow to stand for 20 minutes. Dilute each solution with water to about 300 mL, and titrate with 0.1 N sodium hydroxide VS to a pH of 8.1 ± 0.1 for the specimen under assay and 6.5 ± 0.1 for the blank, using a pH meter. Each mL of 0.1 N sodium hydroxide, after correction for the blank, is equivalent to 9.210 mg of C3H8O3.

中文内容第一段
高碘酸钠溶液：将60克高碘酸钠（溶于含120mL 浓度为C（  H2SO4）=0.1mol/L 硫酸的蒸馏水中，稀释至总容积为1升，溶解时不要加热。如果溶液不透明，用多孔玻璃滤器过滤。贮存于一个深色带玻璃塞的瓶中， 质量品质试验：用移液管移取10mL高碘酸钠溶液至250mL的容量瓶中，稀释至刻度并混合均匀，取0.5～0.6g甘油于50mL蒸馏水中，用移液管移取 50.00mL稀释的高碘酸钠液加入，取50mL蒸馏水准备一个空白。静置30min，加5mL浓HCl，10mL 15%的KI溶液，摇匀，又静置5分钟，加入100mL蒸馏水，用0.1mol/L硫代硫酸钠溶液滴定，不断摇动，直至呈淡黄色。加入1-2mL淀粉指示剂，慢慢加入Na2S2O3溶液继续滴定，直到蓝色刚消失。当含有甘油的溶液消耗的Na2S2O3体积除以空白溶液消耗的Na2S2O3体积在0.750-0.765范围内时，高碘酸钠合格。

第二段
准确称取约0.4g甘油于600mL烧杯中，加水稀释到50mL，加溴百里酚蓝指示剂，并用浓度为0.2N的硫酸酸化至出现明显的绿色或黄绿色，用0.05 mol/L NaOH中和至终点，此时，溶液由绿色突变为蓝色。用移液管移取50.00mL高碘酸钠加入，轻轻转动，确保其均匀混合，用一块透明玻璃盖上，放置于黑暗处，室温下（不超过35℃）静置30分钟，然后加入10mL 1:1的乙二醇水溶液，轻轻转动，确保其均匀混合，并让其再静置20分钟，稀释至大约300mL，以50mL水代替样品按同样步骤处理进行空白试用。用0.1mol/L的NaOH滴定，用PH计判定终点。  空白PH=6.5±0.1，样品PH=8.1±0.1，结果扣除空白，每毫升0.1N氢氧化钠相当于9.21毫克甘油。