[专题]吡咯烷酮羧酸钠生产标准

[专题]吡咯烷酮羧酸钠生产标准 Sodium dl-pyrrolidonecarboxylate solution Sodium dl-pyrrolidonecarboxylate solution is an aqueous solution of sodium dl-pyrrolidonecarboxyate. It contains not less than 48% and not more than 52% of sodium dl-pyrrolidonecar- -boxyate(CHNNaO). 563 Description: Sodium dl-Pyrrolidonecarboxylate Solution is a clear, colorless liquid. It is odorless. To 2 ml of Sodium dl-Pyrrolidonecarboxylate Solution add water to make 5 ml: this Solution shows no optical rotation. Identification (1) To l ml of sodium dl-pyrrolidonecarboxylate Solution add 5 ml of a solution of sodium hydroxide (9 in 100), stopper tightly, and heat at 180’ for 30minutes. After cooling,neutralize with diluted hydrochloric acid (1 in 5),add 1ml of ninhydrin TS,and heat for 3minutes:a red-purple color develops. 2)To 1ml of sodium dl-Pyrrolidonecarboxylate Solution add water to make 25ml,and this solution as the sample solution. Separately, dissolve 0.2g of Pyrrolidone carboxylic acid for thin-layer chromatogrphy in 10 ml of water ,and use this solution as the standard solution. Perform the test with these solution as directed under the thin-layer Chromatography. Spot 5ul each of the sample solution and the standard solution on a plate of silica gel for thin-layer chromatography .Develop the plate with a mixture of 1-butanol, water and acetic acid(100)(4:1:1)to a distance of about 10cm,and air-dry the plate. Then allow to stand in a container filled with chlorine for 10 minutes, and air-dry to exclude the chlorine. Spray evenly the plate with potassium iodido-starch TS : the principle spot from the sample solution and the spot from the standard solution show a purple color and the same Rf value. 3) Sodium dl-Pyrrolidonecarboxylate Solution responds to the Qualitative Tests for sodium salt. 20Specific gravity: d:1.260—1.300 20 Purity:1) Acidity and alkalinity—To 1ml of Sodium dl-Pyrrolidonecarboxylate Solution add water to make 10ml :the solution so obtained is neutral. 2)Chloride—To 0.25g of Sodium dl-Pyrrolidonecarboxylate Solution add 10ml of dilute nitric acid and water to make 50 ml , and perform the test using this solution as the test solution. Prepare the control solution as follows: to 0.5ml of 0.01mol/L hydrochloric acid VS add 10ml of dilute nitric acid and water to make 50ml (not more than 0.071%). 3)Sulfate –To 0.8g of Sodium dl-Pyrrolidonecarboxylate Solution add 6ml of dilute hydrochloric acid and water make 50 ml , and perform the test using this solution as the test solution. Prepare the control solution as follows: to 0.5ml of 0.005mol/L sulfuric acid VS add 6 ml of dilute hydrochloric acid and water to make 50ml (not more than 0.010%). 4) Heavy metal—Proceed with 1.0g of Sodium dl-Pyrrolidonecarboxylate Solution according to mothod 1, and perform the test. Prepare the control solution with 2.0ml of Standard Lead Solution (not more than 20ppm). Assay: Weigh accurately about 0.06g of Sodium dl-Pyrrolidonecarboxylate Solution, and perform the test as directed under Nitrogen Determination. Each ml of 0.005mol/l sulfuric acid VS =1.511mg of CHNNaO563. Containers and storage : Containers—Tighe containers.