求BP2016版的glycine质量标准？British Pharmacopoeia Volume I & II Monographs: Medicinal and Pharmaceutical Substances Glycine European Union chaplet of stars General Notices (Ph. Eur. monograph 0614) bp2013_v1_07_medicinal_and_pharmaceutical_substances_08 glycine_1_2012_70_cs.png C2H5NO2 75.1 56-40-6 Action and use Amino acid used for bladder irrigation during surgery. Preparation Glycine Irrigation Solution Ph Eur DEFINITION 2-Aminoacetic acid. Content 98.5 per cent to 101.0 per cent (dried substance). CHARACTERS Appearance White or almost white, crystalline powder. Solubility Freely soluble in water, very slightly soluble in ethanol (96 per cent). It shows polymorphism (5.9). IDENTIFICATION First identification A. Second identification B, C. A. Infrared absorption spectrophotometry (2.2.24). Comparison glycine CRS. If the spectra obtained in the solid state show differences, dissolve the substance to be examined and the reference substance separately in the minimum volume of ethanol (60 per cent V/V) R, evaporate to dryness and record the spectra again. B. Examine the chromatograms obtained in the test for ninhydrin-positive substances. Results The principal spot in the chromatogram obtained with test solution (b) is similar in position, colour and size to the principal spot in the chromatogram obtained with reference solution (a). C. Dissolve 50 mg in 5 mL of water R, add 1 mL of strong sodium hypochlorite solution R and boil for 2 min. Add 1 mL of hydrochloric acid R and boil for 4-5 min. Add 2 mL of hydrochloric acid R and 1 mL of a 20 g/L solution of resorcinol R, boil for 1 min and cool. Add 10 mL of water R and mix. To 5 mL of the solution add 6 mL of dilute sodium hydroxide solution R. The solution is violet with greenish-yellow fluorescence. After a few minutes, the colour becomes orange and then yellow and an intense fluorescence remains. TESTS Solution S Dissolve 5.0 g in carbon dioxide-free water R and dilute to 50 mL with the same solvent. Appearance of solution Solution S is clear (2.2.1) and not more intensely coloured than reference solution Y7 (2.2.2, Method II). pH (2.2.3) 5.9 to 6.4. Dilute 10 mL of solution S to 20 mL with carbon dioxide-free water R. Ninhydrin-positive substances Thin-layer chromatography (2.2.27). Test solution (a) Dissolve 0.10 g of the substance to be examined in water R and dilute to 10.0 mL with the same solvent. Test solution (b) Dilute 1.0 mL of test solution (a) to 10.0 mL with water R. Reference solution (a) Dissolve 10 mg of glycine CRS in water R and dilute to 10.0 mL with the same solvent. Reference solution (b) Dilute 1.0 mL of test solution (a) to 200 mL with water R. Reference solution (c) Dissolve 10 mg of glycine CRS and 10 mg of alanine CRS in water R and dilute to 25 mL with the same solvent. Plate cellulose for chromatography R as the coating substance. Mobile phase glacial acetic acid R, water R, butanol R (20:20:60 V/V/V). Application 5 μL. Development Over 2/3 of the plate. Drying At 80 °C for 30 min. Detection Spray with ninhydrin solution R and dry at 100-105 °C for 15 min. System suitability The chromatogram obtained with reference solution (c) shows 2 clearly separated spots. Limits In the chromatogram obtained with test solution (a): — any impurity: any spots, apart from the principal spot, are not more intense than the principal spot in the chromatogram obtained with reference solution (b) (0.5 per cent). Chlorides (2.4.4) Maximum 75 ppm. Dissolve 0.67 g in water R and dilute to 15 mL with the same solvent. Heavy metals (2.4.8) Maximum 10 ppm. 12 mL of solution S complies with test A. Prepare the reference solution using lead standard solution (1 ppm Pb) R. Loss on drying (2.2.32) Maximum 0.5 per cent, determined on 1.000 g by drying in an oven at 105 °C for 2 h. Sulfated ash (2.4.14) Maximum 0.1 per cent, determined on 1.0 g. ASSAY Dissolve 70.0 mg in 3 mL of anhydrous formic acid R and add 30 mL of anhydrous acetic acid R. Immediately after dissolution, titrate with 0.1 M perchloric acid, determining the end-point potentiometrically (2.2.20). 1 mL of 0.1 M perchloric acid is equivalent to 7.51 mg of C2H5NO2. Ph Eur查看更多
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