谷胱甘肽欧洲药典5.1标准

GLUTATHIONEGlutathionumC10H17N3O6S Mr 307.3DEFINITIONL-?-Glutamyl-L-cysteinylglycine.Content : 98.0 per cent to 101.0 per cent (dried substance).谷胱甘肽C10H17N3O6S Mr 307.3定义描述Lr谷氨酰基L半胱氨酰基甘氨酸含量：按干燥品计算，98.0%-101.0%CHARACTERSAppearance: white or almost white, crystalline powder orcolourless crystals.Solubility : freely soluble in water, very slightly soluble inethanol (96 per cent) and in methylene chloride.性状外观性状：白色或几乎白色结晶性粉末或无色的结晶。溶解度：易溶于水，微溶于96%乙醇及二氯甲烷。IDENTIFICATIONA. It complies with the test for specific optical rotation (seeTests).B. Infrared absorption spectrophotometry (2.2.24).Comparison : glutathione CRS.鉴别A 比旋度符合特定的光学旋转测定（见测定项）。B 红外吸收光谱检测（2.2.24）对比：谷胱甘肽CRS.TESTSSolution S. Dissolve 5.0 g in distilled water R and dilute to 50 ml with the same solvent.Appearance of solution. Solution S is clear (2.2.1) and colourless (2.2.2, Method II).Specific optical rotation (2.2.7) : ?15.5 to ?17.5 (dried substance).Dissolve 1.0 g in water R and dilute to 25.0 ml with the same solvent.测定溶液S：取本品5.0g，蒸馏水R溶解并稀释至50ml。溶液澄清度 溶液S澄清(2.2.1)，无色(2.2.2, Method II)比旋度（2.2.7) 15.5。17.5（干品物质）取本品1.0g，蒸馏水R溶解并稀释至25.0ml。Related substances. Capillary electrophoresis (2.2.47).Prepare the solutions immediately before use.Internal standard solution (a). Dissolve 0.100 g of phenylalanine R in the electrolyte solution and dilute to 50.0 ml with the same solution.Internal standard solution (b). Dilute 10.0 ml of internal standard solution (a) to 100.0 ml with the electrolyte solution.Test solution (a). Dissolve 0.200 g of the substance to be examined in the electrolyte solution and dilute to 10.0 ml with the same solution.Test solution (b). Dissolve 0.200 g of the substance to be examined in internal standard solution (b) and dilute to 10.0 ml with the same solution.Reference solution (a). Dissolve 20 mg of the substance to be examined in internal standard solution (a) and dilute to 10.0 ml with the same solution.Reference solution (b). Dilute 5.0 ml of reference solution (a) to 50.0 ml with the electrolyte solution.Reference solution (c). Dissolve 0.200 g of the substance to be examined in 5 ml of the electrolyte solution. Add 1.0 ml of internal standard solution (a), 0.5 ml of a 2 mg/ml solution of L-cysteine R (impurity B) in the electrolyte solution, 0.5 ml of a 2 mg/ml solution of L-glutathione, oxidised R (impurity C) in the electrolyte solution and 0.5 ml of a 2 mg/ml solution of L-?-glutamyl-L-cysteine R (impurity D) in the electrolyte solution. Dilute to 10.0 ml with the electrolyte solution.有关物质 采用毛细管电泳法（2.2.47）溶液应临用前新鲜配制内标液（a） 取苯丙氨酸0.100g，加电解质溶液溶解并稀释至50.0ml内标溶液（b） 量取内标溶液（a）10.0ml，用电解质溶液稀释至100.0ml供试溶液（a）取待检物质0.200g，加电解质溶液溶解并稀释至10.0ml。供试溶液（b）取待检物质0.200g，加溶液(b)溶解并稀释至10.0ml对照溶液（a）取待检物质20g，加标准溶液（a）溶解并稀释至10.0ml对照溶液（b）取对照溶液（a）5.0ml，加电解质溶液稀释至50.0ml对照溶液 (c) 取待检物质0.200g，加电解质溶液5ml溶解，加入1.0ml对照溶液（a），0.5ml2mg/ml L -半胱氨酸R的电解质溶液（杂质B），0.5ml2mg/ml氧化型谷胱甘肽R电解质溶液（杂质C）及0.5ml2mg/mlLr谷氨酰基L半胱氨酰基甘氨酸R的电解质溶液（杂质D），然后用电解质溶液稀释至10.0mlCapillary:- material: uncoated fused silica,- size: length to the detector cell = 0.5 m; totallength = 0.6 m; ? = 75 m.Temperature: 25 C.Electrolyte solution. Dissolve 1.50 g of anhydrous sodium dihy drogen phosphate R in 230.0 ml of water R and adjust to pH 1.80 with phosphoric acid R. Dilute to 250.0 ml with water R. Check the pH and, if necessary, adjust with phosphoric acid R or dilute sodium hydroxide solution R.Detection: spectrophotometer at 200 nm.Preconditioning of a new capillary: rinse the new capillary before the first injection with 0.1 M hydrochloric acid for 20 min at 138 kPa and with water R at 138 kPa for 10 min ; for complete equilibration, condition the capillary with the electrolyte solution for 40 min at 350 kPa, and subsequently for 60 min at a voltage of 20 kV;毛细管-材料：石英（未涂层）-尺寸：有效长度0.5m，总长：0.6m，内径75 m温度：25电解质溶液：取无水磷酸二氢钠R1.50g，加水R230.0ml，用磷酸R调节PH值为1.80。加水R稀释至150.0ml，检测PH值，如有必要，用磷酸R或氢氧化钠溶液R调节PH值。检测：采用分光光度计在200 nm处检测新毛细管的预处理： 在首次进样前在压力138Kpa下用0.1mol/L盐酸溶液前冲洗毛细管20min，138Kpa压力下用水R冲洗10分钟已达到全平衡状态，用电解质溶液在350kpa条件下冲洗40min，在电压20kv条件下保持60min。Preconditioning of the capillary: rinse the capillary at 138 kPa with the electrolyte solution for 40 min;Between-run rinsing : rinse the capillary with water R at 138 kPa for 1 min, with 0.1 M sodium hydroxide for 2 min, with water R at 138 kPa for 1 min, with 0.1 M hydrochloric acid for 3 min and with the electrolyte solution at 138 kPa for 10 min.Injection: under pressure (3.45 kPa) for 5 s ; inject the electrolyte solution (blank solution), reference solutions (b) and (c) and test solutions (a) and (b).Migration: apply a voltage of 20 kV.Run time: 45min.预处理的毛细管：138 kPa压力下，用电解质溶液冲洗毛细管40min；批间冲洗：138 kPa压力下，依次用水R冲洗毛细管1min，0.1mol/L氢氧化钠溶液冲洗2min；水R冲洗1min，0.1mol/L盐酸溶液冲洗3min，最后用电解质溶液冲洗10min；进样：3.45 kPa压力下维持5s；注入电解质溶液（空白溶液），对照溶液（b）、（c）和供试溶液a、b迁移：电压为20KV运行时间：45minRelative migration with reference to the internal standard (about 14 min) : impurity A = about 0.77;impurity B = about 1.04 ; impurity E = about 1.2 ;impurity C = about 1.26; impurity D = about 1.3.相对迁移率：相对于内标物质（约14min）杂质A=约0.77杂质B=约1.04；杂质E=约1.2杂质C=约1.26；杂质D=约1.3System suitability :- resolution: minimum 1.5 between the peaks due to the internal standard and impurity B in the chromatogram obtained with reference solution (c) ; if necessary increase the pH with dilute sodium hydroxide solution R;- peak-to-valley ratio : minimum 2.5, where Hp = height above the baseline of the peak due to impurity D and Hv = height above the baseline of the lowest point of the curve separating this peak from the peak due to glutathione in the chromatogram obtained with referencesolution (c) ; if necessary lower the pH with phosphoric acid R;- check that in the electropherogram obtained with test solution (a) there is no peak with the same migration time as the internal standard (in such case correct the area of the phenylalanine peak).系统适用性分辨率：内标物质产生的峰与对照溶液C中那个杂质B产生的峰之间最低为1.5，如有必要，使用稀氢氧化钠溶液上调PH值峰-谷比：最低位2.5.其中：HP=杂质D产生的基线峰以上的高度HV=对照溶液中谷胱甘肽产生的峰的分离曲线的最低点以上的高度如有必要采用磷酸下调PH。电泳法测定以上项目，供试溶液a在与内标物质在相同的迁移时间里没有出现峰（可用苯丙氨酸峰进行校正）Limits: test solution (b):- corrected areas: divide all the peak areas by the corresponding migration times ;- correction factors: for the calculation of contents, multiply the ratio of time corrected peak areas of impurity and the internal standard by the corresponding correctionfactor : impurity B = 3.0; impurity D = 1.4;限度 供试溶液B校正面积：相对迁移时间除以所有峰面积之和校正因子：- impurities A, B, E: for each impurity, not more than 0.5 times the ratio of the area of the peak due to glutathione to the area of the peak due to the internal standard in the electropherogram obtained with reference solution (b) (0.5 per cent) ;- impurities C, D: for each impurity, not more than 0.7 times the ratio of the area of the peak due to glutathione to the area of the peak due to the internal standard in the electropherogram obtained with reference solution (b) (0.7 per cent) ;- any other impurity: for each impurity, not more than 0.1 times the ratio of the area of the peak due to glutathione to the area of the peak due to the internal standard in the electropherogram obtained with reference solution (b) (0.1 per cent) ;- total : not more than twice the ratio of the area of the peak due to glutathione to the area of the peak due to the internal standard in the electropherogram obtained with reference solution (b) (2.0 per cent) ;- disregard limit : 0.05 times the ratio of the area of the peak due to glutathione to the area of the peak due to the internal standard in the electropherogram obtained with reference solution (b) (0.05 per cent) ; disregard any peak due to the blank.杂质A、B、E：Chlorides (2.4.4) : maximum 200 ppm.Dilute 2.5 ml of solution S to 15 ml with water R.氯化物 不得大于200ppm取溶液S2.5ml，加水R稀释至15ml。Sulphates (2.4.13) : maximum 300 ppm.Dilute 5 ml of solution S to 15 ml with distilled water R.硫酸盐 不得大于300ppm取溶液S2.5ml，加蒸馏水R稀释至15mlAmmonium (2.4.1) : maximum 200 ppm.50 mg complies with limit test B. Prepare the reference solution using 0.1 ml of ammonium standard solution (100 ppm NH4) R.铵盐 不得超过200ppmIron (2.4.9) : maximum 10 ppm.In a separating funnel, dissolve 1.0 g in 10 ml of dilute hydrochloric acid R. Shake with 3 quantities, each of 10 ml, of methyl isobutyl ketone R1, shaking for 3 min each time.To the combined organic layers, add 10 ml of water R and shake for 3 min. The aqueous layer complies with the test.General Notices (1) apply to all monographs and other texts 2937铁 不得超过10ppm取本品1.0g置分液漏斗中，加10ml稀盐酸溶解。分三次加入甲基异丁基酮并振摇，每次用量为10ml，每次振摇3min。合并有机层，加入10ml水R，振摇3min。Heavy metals (2.4.8) : maximum 10 ppm.12 ml of solution S complies with limit test A. Prepare the reference solution using lead standard solution (1 ppm Pb) R.重金属 ：不得超过10ppm。取溶液S12ml，按照限度测定方法A，应符合规定。以铅标准溶液为对照。Loss on drying (2.2.32) : maximum 0.5 per cent, determined on 1.000 g by d