Fasudil_Hydrochloride_HNMR_19812_MedChemExpress
盐酸二甲双胍质量标准(英国药典)
Metformin HydrochlorideC4H11N5·HCl 165.62Imidodicarbonimidic diamide,N,N-dimethyl-,monohydrochloride.1,1-Dimethylbiguanide monohydrochloride [1115-70-4].»Metformin Hydrochloride contains not less than 98.5percent and not more than 101.0percent of C4H11N5·HCl,calculated on the dried basis.USP Reference standards 〈11〉—USP Metformin Hydrochloride P Metformin Related Compound A RS.Identification—A:Infrared Absorption 〈197K〉.B:It meets the requirements of the tests for Chloride 〈191〉.Loss on drying 〈731〉—Dry it at 105for 5hours:it loses not more than 0.5%of its weight. Residue on ignition 〈281〉:not more than 0.1%.Heavy metals,Method I〈231〉:0.001%.Related compounds—Mobile phase—Prepare a solution in water,containing 17g of monobasic ammonium phosphate per L,adjust with phosphoric acid to a pHof 3.0,and mix.Standard solution—Prepare a solution of USP Metformin Related Compound A RSin water having a known concentration of about 0.2mg per mL.Transfer 1.0mLof this solution to a 200-mLvolumetric flask,dilute with Mobile phase to volume,and mix.[NOTE—Metformin related compound Ais 1-cyanoguanidine.]Test solution—Transfer about 500mg of Metformin Hydrochloride,accurately weighed,to a 100-mLvolumetric flask,dissolve in and dilute with Mobile phase to volume,and mix.Diluted test solution—Transfer 1.0mLof the Test solution to a 10-mLvolumetric flask,dilute with Mobile phase to volume,and mix.Transfer 1.0mLof this solution to a 100-mLvolumetric flask,dilute with Mobile phase to volume,and mix.Resolution solution—Transfer about 10mg of melamine to a 100-mLvolumetric flask,and dissolve in about 90mLof water.Add 5.0mLof the Test solution,dilute with water to volume,and mix.Transfer 1.0mLof this solution to a 50-mLvolumetric flask,dilute with Mobile phase to volume,and mix.Chromatographic system (see Chromatography 〈621〉)—The liquid chromatograph is equippedwith a 218-nm detector and a 4.6-mm ×25-cm column containing packing L9.The flow rate is about 1.0to 1.7mLper minute.Chromatograph the Resolution solution,and record the peak responses as directed for Procedure:the resolution,R,between melamine and metformin is not less than 10.Procedure—Separately inject equal volumes (about 20µL)of the Test solution,the Standard solution,and the Diluted test solution into the chromatograph,record the chromatograms for not less than twice the retention time of metformin,and measure the peak areas.The area of a peak corresponding to metformin related compound Ain the chromatogram of the Test solution is not greater than the area of the corresponding peak in the chromatogram of the Standard solution:not more than 0.02%of metformin related compound Ais found.The area of any other secondary peak in the chromatogram of the Test solution is not greater than the area of the major peak in the chromatogram of the Diluted test solution;and the sum of the areas of all secondary peaks in the chromatogram of the Test solution is not greater than five times the area of the major peak in the chromatogram of the Diluted test solution:not more than 0.1%of any other impurity is found;and not more than 0.5%of total impurities is found.Assay—[NOTE—To avoid overheating of the reaction medium,mix thoroughly throughout the titration,and stop the titration immediately after the endpoint has been reached.]Dissolve about 60mg of Metformin Hydrochloride,accurately weighed,in 4mLof anhydrous formic acid.Add 50mLof acetic anhydride.Titrate with 0.1Nperchloric acid VS,determining the endpoint potentiometrically.Perform a blank determination,and make any necessary correction (see Titrimetry 〈541〉).Each mLof 0.1Nperchloric acid is equivalent to 8.28mg of C4H11N5·P28Auxiliary Information—Staff Liaison:Elena Gonikberg,Ph.D.,ScientistExpert Committee:(PA4)Pharmaceutical Analysis 4USP28–NF23Page 1231Pharmacopeial Forum:V olume No.29(6)Page 1925Phone Number:1-301-816-8251Metformin Hydrochloride(Ph Eur monograph 0931)C4H11N5,HCl 165.61115-70-4Ph EurDEFINITION1,1-Dimethylbiguanide hydrochloride.Content98.5 per cent to 101.0 per cent (dried substance).CHARACTERSAppearanceWhite crystals.SolubilityFreely soluble in water, slightly soluble in alcohol, practically insoluble in acetone and in methylene chloride.IDENTIFICATIONFirst identificationB, E.Second identificationA, C, D, E.A. Melting point (2.2.14): 222 C to 226 C.B. Infrared absorption spectrophotometry (2.2.24).Preparation. Discs of potassium chloride R.Comparison: Metformin hydrochloride CRS.C. Thin-layer chromatography (2.2.27).Test solution. Dissolve 20 mg of the substance to be examined in water R and dilute to 5 ml with the same solvent.Reference solution. Dissolve 20 mg of metformin hydrochloride CRS in water R and dilute to 5 ml with the same solvent.Plate. TLC silica gel G plate R.Mobile phase. Upper layer of a mixture of 10 volumes of glacial acetic acid R, 40 volumes of butanol R and 50 volumes of water R.Application. 5 µl.Development. Over a path of 15 cm.Drying. At 100C105 C for 15 min.Detection. Spray with a mixture of equal volumes of a 100 g/l solution of sodium nitroprusside R, a 100 g/l solution of potassium ferricyanide R and a 100 g/l solution of sodium hydroxide R, prepared 20 min before use.Results. The principal spot in the chromatogram obtained with the test solution is similar inposition, colour and size to the principal spot in the chromatogram obtained with the reference solution.D. Dissolve about 5 mg in water R and dilute to 100 ml with the same solvent. To 2 ml of the solution add 0.25 ml of strong sodium hydroxide solution R and 0.10 ml of a-naphthol solution R. Mix and allow to stand in iced water for 15 min. Add 0.5 ml of sodium hypobromite solution R and mix. A pink colour develops.E. It gives reaction (a) of chlorides (2.3.1).TESTSSolution SDissolve 2.0 g in water R and dilute to 20 ml with the same solvent.Appearance of solutionSolution S is clear (2.2.1) and colourless (2.2.2, Method II).Related substancesLiquid chromatography (2.2.29).Test solutionDissolve 0.50 g of the substance to be examined in the mobile phase and dilute to 100.0 ml with the mobile phase.Reference solution (a)Dissolve 20.0 mg of cyanoguanidine R in water R and dilute to 100.0 ml with the same solvent. Dilute 1.0 ml to 200.0 ml with the mobile phase.Reference solution (b)Dilute 1.0 ml of the test solution to 50.0 ml with the mobile phase. Dilute 1.0 ml of this solution to 20.0 ml with the mobile phase.Reference solution (c)Dissolve 10.0 mg of melamine R in about 90 ml of water R. Add 5.0 ml of the test solution and dilute to 100.0 ml with water R. Dilute 1.0 ml of this solution to 50.0 ml with the mobile phase.Column:size: l = 0.25 m, Ø = 4.6 mm,stationary phase: irregular, porous silica gel to which benzenesulphonic acid groups have been chemically bonded (10 µm),orsize: l = 0.11 m, Ø = 4.7 mm,stationary phase: regular, porous silica gel to which benzenesulphonic acid groups have been chemically bonded (5 µm).Mobile phase17 g/l solution of ammonium dihydrogen phosphate R adjusted to pH 3.0 with phosphoric acid R.Flow rate1 ml/min.DetectionSpectrophotometer at 218 nm.Injection20 µl.Run timeTwice the retention time of metformin hydrochloride.System suitabilityReference solution (c):resolution: minimum of 10 between the peaks due to melamine and to metformin hydrochloride.Limits:impurity A: not more than the area of the corresponding peak in the chromatogram obtained with reference solution (a) (0.02 per cent),any other impurity: not more than the area of the principal peak in the chromatogram obtained with reference solution (b) (0.1 per cent).Heavy metals (2.4.8)Maximum 10 ppm.12 ml of solution S complies with limit test A. Prepare the standard 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 100C105 C for 5 h. Sulphated ash (2.4.14)Maximum 0.1 per cent, determined on 1.0 g.ASSAYDissolve 0.100 g in 4 ml of anhydrous formic acid R. Add 80 ml of acetonitrile R. Carry out the titration immediately. 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 16.56 mg of C4H12ClN5.IMPURITIESQualified impuritiesA.Other detectable impuritiesB, C, D, E, F.A. cyanoguanidine,B. R = NH-C(=NH)-NH2: (4,6-diamino-1,3,5-triazin-2-yl)guanidine,C. R = N(CH3)2: N,N-dimethyl-1,3,5-triazine-2,4,6-triamine,D. R = NH2: 1,3,5-triazine-2,4,6-triamine (melamine),E. 1-methylbiguanide,F. CH3-NH-CH3: N-methylmethanamine.Ph EurAction and useHypoglycaemic.PreparationMetformin Tablets。
麦吉丽Mageline水氧润护系列好用么
大家都说这是个看脸的时代，但是大家有好好对待过自己的脸嘛。
就像女人三十那部电影里面说的，其实这个世界上没有丑女人只有懒女人。
其实大家只要注意保养自己的皮肤应该是不会丑的。
有很多女生会很纠结到底该怎么去选择护肤品呢，或者是哪个牌子的护肤品好呢？其实护肤这个东西都是因人而异的，每个人肤质不一样适合的护肤品也是不同的。
下面小编给大家推荐几款麦吉丽的护肤品，大部分都是值得回购的空瓶分享哦。
花漾活肤卸妆水温和洁净彩妆、污垢和老化的多余角质产品说明深层卸除眼部及脸部彩妆、污垢和老化的多余角质，收细毛孔，打开肌肤吸收通道，促进后续护肤养分吸收，蕴含植物萃取保湿成分，在清洁的同时不带走肌肤水分，让洗净的肌肤任有润泽，无黏腻感，温和不刺激，缔造清爽澄净的肌肤。
产品成分水、丁二醇、马齿苋（PORTULACA OLERACEA）提取物、PEG-12 甘油月桂酸酯、甘油月桂酸酯、仙人掌（OPUNTIA DILLENII）提取物、PEG-40氢化蓖麻油、尿囊素用法用量喷雾直接喷于面部或取适量于掌心，在脸部以螺旋状涂抹开，待卸妆水与彩妆及污垢充分融合后，用清水或温水充分清洗。
卸妆后，请务必使用洁面品清洁。
水养润护柔肤水舒缓保湿调理肌肤水油平衡产品说明蕴含蜗牛提取精华、酵母、透明质酸等多种成分，温和补水，帮助打开肌肤水通道，促进肌肤水循环，帮助改善肌肤干燥、脱屑、脆弱泛红、肤色暗沉等现象，舒缓保湿，调理肌肤水油平衡，令肌肤水润光采有活力。
产品成分水、甘油、丁二醇、透明质酸钠、蜗牛分泌物滤液、酵母菌发酵溶胞产物滤液、β-葡聚糖、甘油聚甲基丙烯酸酯、PVM/MA 共聚物、黄原胶、月见草（OENOTHERA BIENNIS）提取物、库拉索芦荟（ALOE BARBADENSIS）提取物等。
用法用量洁面后，以化妆棉沾取适量，轻轻拍打全脸及颈部直至吸收。
水养润护精华液补水保湿舒缓修护肌肤温和不刺激产品说明甄选多种植物、酵母及蜗牛提取精华等护肤成分，深层补水保湿，帮助改善肌肤干燥、脱屑、脆弱泛红、肤色暗沉等现象，淡化干纹、细纹，均匀肤色，重建肌肤皮脂膜,滋养修护肌肤，日复一日，肌肤绽放健康水润光泽，晶莹通透。
盐酸法舒地尔说明书
分类：化学药品类别：3.1【药品名称】通用名：盐酸法舒地尔注射液曾用名：商品名：英文名：Fasudil Hydrochloride Injection汉语拼音：Yansuan Fashudier Zhusheye剂型：注射剂【成分】化学名称：六氢—1—(5—磺酰基异喹啉)—1(H)—1，4—二氮杂卓盐酸盐。
化学结构式：分子式：C14H17N3O2S?HCl分子量：327.83【性状】本品为白色、类白色或微黄色的结晶性粉末。
无臭，味微苦。
有引湿性。
本品在水中极易溶，在甲醇中溶解，在乙醇中略溶，在氯仿中极微溶，在乙醚中几乎不溶。
【药理毒理】盐酸法舒地尔是一种蛋白激酶抑制剂即细胞内钙离子拮抗剂。
血管平滑肌的收缩是由于平滑肌细胞内Ca2+浓度显著增高激活了关键酶的缘故。
当CA2+ 达到一定浓度时，与CA2+结合蛋白钙调素结合，激活肌球蛋白轻链磷酸化酶，将肌球蛋白轻链磷酸化，引起肌肉收缩。
蛛网膜下腔出血时，血管中释放出的各种血管收缩物质参与血管痉挛，最终通过肌球蛋白轻链磷酸化造成血管收缩。
盐酸法舒地尔通过阻断血管收缩过程的最终阶段，肌球蛋白轻链磷酸化，来扩张血管，抑制血管痉挛。
急性毒性：小鼠、大鼠口服给药的LD50分别为：小鼠雄性为273.9 mg／kg；雌性为277.3 mg／kg；大鼠雄性为335 mg／kg；雌性为348 mg／kg。
小鼠静脉给药的LD50 为69.5mg／kg。
亚急性毒性：以大鼠、猴静脉内给药1个月，无毒性剂量为：大鼠12.5mg／kg，猴3.125mg／kg。
慢性毒性：以大鼠、猴静脉内给药6个月，无毒性剂量为：大鼠9mg／kg，猴3.125mg／kg。
致突变性实验：细菌回复突变实验及啮齿类动物微核试验均为阴性。
哺乳类细胞染色体试验证明在体内无致突变性。
生殖毒性试验：妊娠前及妊娠初期的大鼠及大鼠胎仔器官形成期生殖和发育的毒性研究，剂量分别为1.56，6.25，25和1.6，8.0，40mg/kg。
法舒地尔杂质种类整理列表
中文名称英文名称CAS规格用途结构式
盐酸法舒地尔Fasudil HCl105628-07-710mg-25mg-50mg-100mg
项目报批
纯度高于99.89%
法舒地尔二聚体Fasudil Dimer1337967-93-710mg-25mg-50mg-100mg
项目报批
纯度高于99.89%
法舒地尔吡啶N-氧化物三氟乙酸盐Fasudil Pyridine N-
Oxide TFA Salt
186544-56-910mg-25mg-50mg-100mg
项目报批
纯度高于99.89%
法舒地尔杂质 3Fasudil Impurity 3166895-80-310mg-25mg-50mg-100mg
项目报批
纯度高于99.89%
法舒地尔N-羟基杂
质Fasudil N-Hydroxy
Impurity
1350827-92-710mg-25mg-50mg-100mg
项目报批
纯度高于99.89%
武汉斯坦德供应各种杂质对照品:泊沙康唑杂质、替卡格雷杂质、索拉非尼杂质、索拉菲尼相关杂质、去氧肾上腺素杂质、维生素BI杂质、马来酸氯苯那敏杂质、瑞格列奈杂质等；并提供COA、NMR、HPLC、MS等图谱。
专注各种杂质对照品 代理中检所/EP/BP/USP/LGC/TRC/DR/TLC/MC/SIGMA/BACHEM/STD等品牌
法舒地尔杂质种类整理列表。
爱丽德洗发露成分表
爱丽德洗发露成分表1. 产品简介爱丽德洗发露是一款广受欢迎的洗发产品，被广大消费者认可为有效清洁头发并保护秀发健康的选择。
本文将对爱丽德洗发露的成分进行详细分析，以帮助读者更好地了解该产品。
2. 成分列表以下是爱丽德洗发露中的主要成分：• 2.1 透明质酸• 2.2 瓜尔胶• 2.3 茶多酚• 2.4 椰油酰胺丙基甜菜碱• 2.5 氨基酸• 2.6 阿魏酸3. 成分详解3.1 透明质酸透明质酸是一种天然存在于皮肤中的多糖，具有保湿和润滑的作用。
它能够吸引并锁住水分，使头发保持水润，减少干燥和毛躁，同时也能增加头发的光泽。
3.2 瓜尔胶瓜尔胶是一种植物胶，具有丰富的营养成分，如维生素和矿物质。
它能够形成保护膜，保护头发免受外界环境的损伤，同时还能够修复受损的发丝，使头发更加柔顺顺滑。
3.3 茶多酚茶多酚是一种具有抗氧化和抗炎作用的成分，被广泛应用于美容和护肤产品中。
在洗发产品中，茶多酚能够清洁头皮，减少头屑的产生，同时还能够促进头发生长，提高头发的密度和质量。
3.4 椰油酰胺丙基甜菜碱椰油酰胺丙基甜菜碱是一种表面活性剂，具有良好的起泡和清洁能力。
它能够去除头皮和头发上的污垢和油脂，使头发清爽干净，同时还能够改善发丝的柔软度和顺滑度。
3.5 氨基酸氨基酸是构成蛋白质的基本成分，对头发的生长和修复起着重要作用。
洗发产品中添加氨基酸能够为头发提供养分，修复受损的发丝，增强发质，减少断裂和分叉。
3.6 阿魏酸阿魏酸是一种具有温和护理作用的成分，能够调节头皮的油脂分泌，减少头皮屑的产生。
同时它还具有镇静和舒缓头皮的功效，缓解头皮不适和瘙痒。
4. 使用效果爱丽德洗发露中的成分经过精心配制，能够为头发提供全面的护理和保护。
使用爱丽德洗发露后，您可以期待以下效果：•头发清洁彻底，油脂、污垢和头屑得到有效去除。
•头发保持水润和滋养，减少干燥和毛躁问题。
•头发变得柔顺顺滑，易于梳理和造型。
•头皮舒缓，减少头屑产生，改善头皮状况。
beely芦荟胶
Beely芦荟胶
芦荟胶又叫万用胶,万能胶！因为它可以全面的修补肌肤,最主要的功效就是杀菌消炎，因为芦荟有修复再生，美容养颜，抗辐射，抗衰老，所以芦荟胶有很多意想不到的作用，平常的补水保湿，美白祛斑，修护皮肤等功效都有，是居家旅行必备之品！
芦荟胶使用方法：
一般一天1-2次，在乳液后使用，在使用芦荟胶后建议再涂一次乳液！修复痘痕印疤，轻度一般28天(2支左右)一个疗程，中重度2-3个疗程可以达到明显的全面效果。
富含天然芦荟原汁，有效锁住肌肤水分，达到深度保湿作用。
并能在皮肤上形成特有的透气性保护膜，使皮肤免受外界的干扰，促进皮肤新陈代谢，使皮肤自然、健康、美白。
产品成分：水、库拉索芦荟（ALOEBARBADENSIS）叶提取物、甘油、B-葡聚糖、双甘油、透明质酸钠、卡波姆、三乙醇胺、聚山梨醇酯-20、咪唑烷基脲、香精、食品绿（CI42053）。
适用肌肤：任何肤质
使用方法：洁肤后，取适量涂于面部或身体其他所需部位，轻轻按摩，直至完全吸收。
注意事项：请谨防入眼，如不慎入眼请立即用清水洗净。
使用后，请盖紧瓶盖。
用户评价：用的挺好的，凉凉的很舒服，水水的，有淡淡的味道，透明状。
涂上吸收很快，很好。
文章来源于beely芦荟胶:。
磺达肝癸钠原料药USP38标准
Chromatographic systemAdd the following:(See Chromatography 〈621〉, System Suitability .)Mode: LCDetector: UV 254 nmvFondaparinux SodiumColumn: 4.6-mm × 25-cm; packing L1Flow rate: 1mL/min Injection size: 25µLSystem suitabilitySamples: System suitability solution and Standard solutionSuitability requirementsResolution: NLT 3.6 between folic acid related com-pound A (calcium formyltetrahydrofolate) and folic acid, System suitability solutionRelative standard deviation: NMT 2.0%, Standard solution C 31H 43N 3O 49S 8Na 101728.08Analysisα-D -Glucopyranoside, methyl O -2-deoxy-6-O -sulfo-Samples: Standard solution and Sample solution 2-(sulfoamino)-α-D -glucopyranosyl-(1→4)-O -β-D -Calculate the percentage of the labeled amount ofglucopyranuronosyl-(1→4)-O -2-deoxy-3,6-di-O -sulfo-folic acid (C 19H 19N 7O 6) in the portion of Tablets taken:2-(sulfoamino)-α-D -glucopyranosyl-(1→4)-O -2-O -sulfo-α-L -Result = (r U /r S ) × (C S /C U ) × 100idopyranuronosyl-(1→4)-2-deoxy-2-(sulfoamino)-, 6-(hy-drogen sulfate), decasodium salt;r U= peak area of folic acid from the SampleMethyl O -2-deoxy-6-O -sulfo-2-(sulfoamino)-α-D -glucopyra-solutionnosyl-(1→4)-O -β-D -glucopyranuronosyl-(1→4)-O -2-deoxy-r S = peak area of folic acid from the Standard3,6-di-O -sulfo-2-(sulfoamino)-α-D -glucopyranosyl-(1→4)-O -solution2-O -sulfo-α-L -idopyranuronosyl-(1→4)-2-deoxy-6-O -sulfo-C S = concentration of USP Folic Acid RS in the2-(sulfoamino)-α-D -glucopyranoside, decasodium salt Standard solution (mg/mL)[114870-03-0].C U = nominal concentration of folic acid in theDEFINITIONSample solution (mg/mL)Fondaparinux Sodium is the sodium salt of a syntheticAcceptance criteria: 90.0%–115.0%sulfated pentasaccharide anticoagulant based on the anti-PERFORMANCE TESTS thrombin binding moiety of heparin. It is synthesized •D ISSOLUTION 〈711〉from a natural source of chirally pure sugars (mono- and Medium: Water; 500mL di-saccharides). A range of coupling, (de)protection and Apparatus 2: 50 rpm functionalization reactions leads to crude fondaparinux so-Time: 45 mindium, which is further purified to yield the drug sub-Standard solution: Solution having a known concentra-stance. Fondaparinux Sodium contains NLT 95.0% and tion of USP Folic Acid RS, corrected for water content,NMT 103.0% of fondaparinux sodium, calculated on the in Mediumanhydrous and solvent-free basis. Fondaparinux Sodium is Sample solution: Filtered portion of the solution under a white to off-white powder.test, suitably diluted with the Medium if necessary IDENTIFICATIONAnalysis•A . 13C NMR S PECTRUMSamples: Standard solution and Sample solutionNMR reference: Dissolve in 1mL of deuterium oxide Proceed as directed in the Assay , making any necessary 20mg of (2,2,3,3-(d4)-3-(trimethylsilyl)propionic acid modifications.sodium salt (TSP), enriched to 98% deuterated or Calculate the percentage of the labeled amount of equivalent, as a chemical shift reference.folic acid (C 19H 19N 7O 6) dissolved:Standard solution: NLT 40mg/mL of USPResult = (r U /r S ) × (C S × D × V /L ) × 100Fondaparinux Sodium Identification RS in deuterium oxider U= peak area of folic acid from the SampleSample solution: NLT 40mg/mL of Fondaparinux So-solutiondium in deuterium oxide r S = peak area of folic acid from the StandardInstrumental conditionssolution(See Nuclear Magnetic Resonance 〈761〉.)C S = concentration of USP Folic Acid RS in theMode: NMR, pulsed (Fourier transform)Standard solution (mg/mL)Frequency: NLT 100MHz (for 13C)D = dilution factor for the Sample solution Temperature: 40°V = volume of Medium , 500mL System suitabilityL = label claim (mg/Tablet)Sample: Standard solutionTolerances: NLT 75% (Q ) of the labeled amount of folic Using a pulsed (Fourier transform) NMR spectrometer acid (C 19H 19N 7O 6) is dissolved.operating at NLT 100MHz for 13C, acquire a free in-•U NIFORMITY OF D OSAGE U NITS 〈905〉: Meet the duction decay (FID) using a 90° pulse and a 5-s delay.requirements Record the 13C NMR spectra of the NMR reference at 40°, and set the trimethylsilyl resonance to 0.0ppm.ADDITIONAL REQUIREMENTSCollect the 13C NMR spectrum with a spectral window •P ACKAGING AND S TORAGE : Preserve in well-closed of at least 235 to −10ppm with spinning at 20 Hz,containers.using line broadening of NLT 1. The number of tran-•USP R EFERENCE S TANDARDS 〈11〉sients should be adjusted until the signal-to-noise ratio USP Folic Acid RSof the signal for the C-1 in the β-D -glucopyra-USP Folic Acid Related Compound A RS nosyluronic acid ring of fondaparinux sodium in the Calcium formyltetrahydrofolate.Standard solution meets the suitability requirements.The Standard solution shall be run at least daily when the Sample solution is being run. The chemical shift forthe C-1 resonance of the β-D-glucopyranosyluronic Standard solution: 5.0mg/mL of USP Fondaparinux acid ring of fondaparinux sodium in the Standard solu-Sodium for Assay RS in water. Prepare in duplicate.tion should be observed at 103.9 ± 0.1ppm. Record Sensitivity check solution: 0.01mg/mL of USPthe 13C NMR spectrum of the Sample solution at 40°Fondaparinux Sodium for Assay RS in water from the using the same conditions.Standard solutionSuitability requirements Sample solution: 5.0mg/mL of fondaparinux sodium Number of transients: The signal-to-noise of the β-D-in water. Prepare in at least duplicate.glucopyranosyluronic acid ring of fondaparinux so-Blank: Waterdium in the Standard solution is at least 20/1 in the Chromatographic systemregion near 103.9ppm.(See Chromatography 〈621〉, System Suitability.)Chemical shift: The trimethylsilyl resonance for the Mode: LCNMR reference should be set to 0.0ppm, which acts Detector: UV 210 nmas an external calibration for all samples.Column: 4-mm × 25-cm; packing L46Chemical shifts for system suitability: The O-methyl Column temperature: 25°and two carbonyl carbons of fondaparinux sodium Flow rate: 1.0mL/minshould be observed at 58.2, 176.7, and 178.0ppm,Injection volume: 100µLall ± 0.3ppm, respectively, in the Standard solution.System suitabilityAnalysis Samples:System suitability solution, Standard solution, Sample:Sample solution Sensitivity check solution, and BlankAcceptance criteria: Resonances for fondaparinux so-Inject the Blank in duplicate, the Sensitivity check solu-dium should be observed at 58.2, 59.5, 60.5, 60.8,tion, and the System suitability solution. Inject the Stan-68.9, 69.2, 69.6, 98.9, 100.4, 101.1, 102.4, 103.9,dard solution at least six times consecutively.176.7, and 178.0ppm. The chemical shifts of these sig-Suitability requirementsnals do not differ by more than ±0.3ppm. Other sig-Specificity and baseline driftnals of variable heights and chemical shifts, attributable The chromatogram of the second Blank injection to fondaparinux sodium, may be seen between shows a baseline drift between 0.00 and 0.02 AU58.0–80.5ppm and 98.7–104.5ppm.over 30 min. If necessary, adjust the DMSO content •B. C HROMATOGRAPHIC I DENTITY of the Mobile phase until an acceptable baseline is Analysis: Proceed as directed in the Assay.achieved.Acceptance criteria: The retention time of the major The chromatogram of the second Blank injection does peak of the Sample solution corresponds to ±5% of that not contain peaks between 3.00 and 30.00 min.of the Standard solution.Signal-to-noise ratio: NLT 10 for the fondaparinux •C. S ODIUM D ETERMINATION peak in the chromatogram of the Sensitivity check Analysis: Proceed as directed in Sodium Determination.solutionAcceptance criteria: It meets the requirements.Chromatogram similarity: The chromatogram of theSystem suitability solution corresponds to that of the ASSAY chromatogram provided with USP Fondaparinux So-•P ROCEDURE dium System Suitability Mixture A RS.5 mM phosphate solution: Dissolve 0.210g of mono-Relative standard deviation: For six consecutive in-basic sodium phosphate dihydrate and 0.650g of diba-jections of the Standard solution, the calculated % sic sodium phosphate dihydrate in water, and dilute RSD of the area of the fondaparinux peak is NMT with water to 1000mL. pH of solution is approximately 2.0%. The retention time of the fondaparinux peak7.3.should be ±5% of the mean value. The calculated %Solution A: 15±10 ppm dimethylsulfoxide (DMSO) in RSD of the response factors for all replicate injections5 mM phosphate solution (1 in 67000, v/v). Filter before of the Standard solution is NMT 2.0%. The calculateduse.% RSD of the pooled response factors for all injec-Solution B: 2.0 M sodium chloride solution with 5 mM tions of the Standard solution is NMT 2.0%. The % phosphate solution RSD of the mean response factors for each duplicate Mobile phase: See Table 1.Standard solution is NMT 2.0%.[N OTE—Make adjustments to Solution A as necessary,Analysisand degas the Mobile phase and the sample before Samples:Standard solution and Sample solutionuse. Dissolved gas in the injected solution may lead to Inject the Standard solution at least six times consecu-baseline interference. Degassing of the Mobile phase is tively and the Sample solution in duplicate. Record the critical to obtain a suitable signal-to-noise ratio and chromatograms and measure the retention times and higher sensitivity. An eluant generator1 installed be-areas for the major peaks (excluding peaks before 3.00 tween the injector and the column may reduce the and after 30.00 min).baseline interference.]For each injection of the Standard solution, calculate aresponse factor (F R):Table 1F R = (C S/r S)Time Solution A Solution B(min)(%)(%)C S= concentration of fondaparinux sodium in the05050Standard solution (mg/mL)r S= peak response of fondaparinux sodium from 55050the Standard solution25595Calculate the mean response factor (F M) for each 30595duplicate injection, and determine the % RSD for the 355050peak areas of fondaparinux sodium (rS) for six 505050consecutive injections of the Standard solution.Using the mean response factor, calculate the System suitability solution: 5.0mg/mL of USP percentage of fondaparinux in the portion of sample Fondaparinux Sodium System Suitability Mixture A RS taken:1One suitable eluant generator is Dionex DEGAS EG40/50 (12×17 cm, thick-ness 2.2cm).Result (% w/w) = (F M× r U×D× 100)/WF M= mean response factor for each duplicateChromatographic systeminjection(See Chromatography 〈621〉, System Suitability .) r U = peak response of fondaparinux sodium in theMode: LCSample solutionDetector: Conductivity (range 200 µS, suppressor cur-D = dilution factor for the sample (mL)rent 300mA)W = weight of fondaparinux sodium taken toColumn: 4.6-mm × 5-cm; packing L23, coupled with a prepare the Sample solution (mg)neutralization micromembrane suppressor 2Acceptance criteria: 95.0%–103.0% on an anhydrous Regenerating solvent for the suppressor: Ultrapuri-and solvent-free basisfied water in a counter current direction Column temperature: Ambient OTHER COMPONENTS Flow rate: 1.0mL/min •S ODIUM D ETERMINATIONInjection volume: 50µL (See Spectrophotometry and Light-Scattering 〈851〉.)Run time: 24 min 2% Nitric acid solution: 21mL nitric acid diluted with System suitabilitywater to 1000mLSamples: Calibration standard solutions and Resolution Sodium solution: 1000ppm sodium in 2% Nitric acid solutionsolutionSuitability requirementsStandard solutions: Prepare Standard solutions contain-Resolution: NLT 2 between the chloride and nitrite ing 20, 30, 40, 50, and 60ppm of sodium ion from the ion peaks, Resolution solutionSodium solution , diluting with 2% Nitric acid solution .Response stability: ±5% between injections of 5ppm Sample solution: 0.3mg/mL of Fondaparinux Sodium of each of the Calibration standard solutions before in 2% Nitric acid solutionand after the Sample solutionAnalysis: Concomitantly determine the absorbances of Relative standard deviation: NMT 3% for NLT 5 in-the Sample solution and Standard solutions at 330.2 nm jections of 5-ppm Calibration standard solutions by using a sodium hollow-cathode lamp and anAnalysisair–acetylene flame. Using the absorbances of the Stan-Sample: Sample solutiondard solutions , determine the sodium content in the [N OTE —Regenerate the anion-exchange column for 15Sample solution after appropriate blank correction.min with 0.1 M sodium hydroxide after each injection Acceptance criteria: 11.5%–15.0% on the anhydrous of fondaparinux sample, followed by equilibration with and solvent-free basis Mobile phase for 21 min.]Inject 50µL of each of the Calibration standard solutions IMPURITIESand 50µL of the Sample solution in triplicate. The peak •F REE S ULFATE AND R ESIDUAL C HLORIDE D ETERMINATIONarea responses for the chloride and sulfate ion peaks in Mobile phase: 3 mM carbonate solution containing the chromatograms obtained with the Calibration stan-0.106g of sodium carbonate and 0.168g of sodium dard solutions show two peaks corresponding respec-hydrogen carbonate in 1000mL of watertively to chloride ions at a retention time of approxi-Standard solution 1: Dissolve 164.9mg of sodium mately 3.6 min and to sulfate ions at a retention time chloride in 80mL of water, and dilute with water to of approximately 14.1 min. The Calibration standard 100.0mL.solutions and the corresponding standard concentra-Standard solution 2: Dissolve 147.9mg of anhydrous tions are used to construct five-point calibration curves sodium sulfate in 80mL of water, and dilute with water for both chloride and sulfate ions. The concentrations to 100.0mL.of sulfate and chloride ions in the Sample solutions are Standard solution 3: Dilute 1.0mL of Standard solution calculated using the standard curves.1 with water to 100.0mL.Calculations: Calculate the free sulfate and residual Standard solution 4: Dilute 1.0mL of Standard solution chloride ion contents in % w/w of fondaparinux so-2 with water to 100.0mL.dium in the solution to be examined:Calibration standard solutions: Using appropriate volumes of the Standard solutions , prepare calibration Result = C S × F × (1/C U ) × 100standards as shown in Table 2.C S= concentration of the ion calculated from thequadratic calibration equation (µg/mL)Table 2F = conversion factor (µg/mL to mg/mL)Volume of Volume of C U = concentration of Fondaparinux Sodium in theSulfate Chloride Sample solution (mg/mL)Concentra-Solution Solution Final VolumeReport the average of the triplicate determinations.tion (mL)(mL)(mL)Acceptance criteria: NMT 0.30% free sulfate; NMT 5.0, Standard 10.0, Standard 0.5 ppm SO 4−21.0% chloride /1 ppm Cl −solution 4solution 3100.0•O RGANIC I MPURITIES0.50, Standard 0.50, Standard Analysis: Proceed as directed in the Assay .2.5 ppm SO 4−2/2.5 ppm Cl −solution 2solution 1200.0Samples: System suitability solution , Standard solution ,Sensitivity check solution , Sample solution , and Blank 0.50, Standard 0.50, Standard 5.0 ppm SO 4−2Calculate the percentage of each individual impurity in /5.0 ppm Cl −solution 2solution 1100.0the portion of Fondaparinux Sodium taken:20.0 ppm 2.0, Standard 2.0, Standard SO 4−2/20 ppmResult (% area/area) = [r U /(r S + r T )] × 100Cl −solution 2solution 1100.050.0 ppm r U= peak response of each impurity from the5.0, Standard 5.0, Standard SO 4−2/50 ppmSample solutionCl −solution 2solution 1100.0r S = peak response of fondaparinux sodium fromthe Sample solutionResolution solution: Dissolve 150mg of sodium nitrite r T= sum of all peak responses for impurities fromin 100.0mL of water. Combine 2.0mL of this solution the Sample solutionand 2.0mL of Standard solution 1 in 80mL of water,and dilute with water to 100.0mL.2One suitable suppressor is Dionex ASRS 300 4mm.Sample solution: 3mg/mL of Fondaparinux Sodium in waterThe total impurities content (% area/area) is the sum of Table 4all mean unrounded contents of an individual impurityHold Time that are NLT 0.200%.Initial at Final Acceptance criteria: See Table 3.Tempera-Temperature Final Tempera-ture Ramp Temperature tureTable 3(°)(°/min)(°) (min)40—4020Relative Acceptance40102400Retention Criteria,Name Time NMT (%)240—2405 Impurity peak A a0.930.8 (a/a)Carrier gas: Helium with a linear velocity ofImpurity peak B a 1.2b0.6 (a/a)20–30cm/sAny unspecified im-Injection type: Split ratio, 1:7—purity0.3Head space autosamplerTotal impurities—NMT 2.0%Sample equilibration temperature: 80°a Impurity peak A contains two structures: Methyl (2-deoxy-2-sodium Sample equilibration time: 60 minsulfoamino-6-O-sodium sulfonato-α-D-glucopyranosyl)-(1→4)-(sodium β-D-Transfer line temperature: 110°glucopyranosyluronate)-(1→4)-(2-deoxy-2-sodium sulfoamino-3,6-di-O-so-System suitabilitydium sulfonato-α-D-glucopyranosyl)-(1→4)-(sodium 2,3-di-O-sodiumsulfonato-α-L-idopyranosyluronate)-2-deoxy-2-sodium sulfoamino-6-O-sodi-Samples:Standard solution 2 (A and B) and Blankum sulfonato-α-D-glucopyranoside; and Methyl (2-deoxy-2-formylamino-6-Assay a water Blank followed by six consecutive samples O-sodium sulfonato-α-D-glucopyranosyl)-(1→4)-(sodium-β-D-glucopyra-of Standard solution 2(A), followed by a single injection nosyluronate)-(1→4)-(2-deoxy-2-sodium sulfoamino-3,6-di-O-sodiumof Standard solution 2(B).sulfonato-α-D-glucopyranosyl)-(1→4)-(sodium 2-O-sodium sulfonato-α-L-idopyranosyluronate)-2-deoxy-2-sodium sulfoamino-6-O-sodium sulfonato-Suitability requirementsα-D-glucopyranoside.Blank: The chromatogram of the water Blank should b Impurity peak B can appear as a complex set of peaks and not fully not present a peak corresponding to ethanol or resolved. In such a case, the integration should be performed such that all pyridine.such peaks are combined.Signal-to-noise ratio: NLT 40 of the pyridine peak in •P YRIDINE AND E THANOL D ETERMINATION the chromatogram of Standard solution 2(A) (See Residual Solvents 〈467〉.)Relative standard deviation: NMT 5% for the aver-Pyridine standard solution: In a 100-mL volumetric age areas of the chromatographic peaks for ethanol flask containing about 20mL of water, transfer 101.8µL and pyridine in six consecutive assaysof pyridine accurately. Dilute with water to 100mL.AnalysisInternal standard solution: 500-µg/mL solution of Samples:Internal standard solution, Standard solution 1-butanol in water2(A), and Sample solutionStandard solution 1: In a 100-mL volumetric flask con-Calculations: Calculate the ethanol and pyridine con-taining about 20mL of water, transfer accurately tent in ppm (µg/g) in the portion of Fondaparinux So-1.27mL of ethanol and 1.0mL of Pyridine standard so-dium taken:lution. Dilute with water to 100.0mL.Standard solution 2:Standard solution 1 and water Result = C S× (R U/R S) × (V/M) ×D(1:100). Prepare in duplicate (A and B).C S= concentration of Standard solution 2 (µg/mL)Sample stock solution: 10mg/mL of Fondaparinux So-R U= peak response ratio of solvent “s” in the dium in water in triplicateSample solution to solvent “s” in the Internal Sample solution: 2mg/mL of Fondaparinux Sodium instandard solutionwater from the Sample stock solutionR S= peak response ratio of solvent “s” in Standard Blank: Watersolution 2 to solvent “s” in the Internal Sample preparation: For the Blank, transfer 5.0mL ofstandard solutionwater and 5g of potassium carbonate to an appropriateV= volume of solution used to prepare the Sample headspace vial, apply stopper, cap, and mix. For sam-solution (mL)ples and standards, add 5.0mL of the Sample solutionM= mass of sample dissolved to prepare the or Standard solution 2 with 5g of potassium carbonateSample solution (g)and 0.1mL of the Internal standard solution to an ap-D= dilution factor of the Sample solution propriate headspace vial, apply stopper, cap, and mix.The average of three independent assays constitutes Chromatographic systemthe results.(See Chromatography 〈621〉, System Suitability.)Acceptance criteria: NMT 5×104 ppm for ethanol and Mode: GC with headspace sampler50ppm for pyridineDetector: Flame ionizationColumn: 0.32-mm × 30-m fused silica, 1.8-µm filmSPECIFIC TESTSthickness; support G43•B ACTERIAL E NDOTOXINS T EST〈85〉: It contains NMT 25 TemperaturesUSP Endotoxin Units/mg.[N OTE—At initial temperature NLT 3 min between•P H 〈791〉: 6.0–8.0, in a solution, at 20°–25° (2.5% w/v) injections.]•M ICROBIAL E NUMERATION T ESTS〈61〉: NMT 350 cfu/g Injector: 140°•W ATER D ETERMINATION, Method Ic〈921〉: It contains NMT Detector: 250°20.0% (w/w).Column: See Table 4.ADDITIONAL REQUIREMENTS•P ACKAGING AND S TORAGE: Preserve in tight containers,and store at or below 25° in a dry environment.•L ABELING: Label to indicate mass of active drug substanceper container.•USP R EFERENCE S TANDARDS〈11〉Blank: WaterUSP Endotoxin RS Chromatographic systemUSP Fondaparinux Sodium for Assay RS(See Chromatography 〈621〉, System Suitability.)USP Fondaparinux Sodium Identification RS Mode: LCUSP Fondaparinux Sodium System Suitability Mixture A Detector: UV 210 nmRS v USP38Column: 4-mm × 25-cm; packing L46Column temperature: 25°Flow rate: 1.0mL/minInjection volume: 100µLSystem suitabilitySamples:System suitability solution, Standard solution, Add the following:Sensitivity check solution, and BlankInject the Blank in duplicate, the Sensitivity check solu-tion, and the System suitability solution. Inject thev Fondaparinux Sodium Injection Standard solution at least six times consecutively.Suitability requirementsDEFINITION Specificity and baseline drift: The chromatogram of Fondaparinux Sodium Injection is a sterile solution of a second Blank injection shows a baseline drift be-Fondaparinux Sodium in Water for Injection with sodium tween 0.00 and 0.02 AU over 30 min. If necessary, chloride added for isotonicity. It is a clear, colorless to adjust the DMSO content of the Mobile phase until an slightly yellow solution.acceptable baseline is achieved. The chromatogramof a second Blank injection does not contain peaks IDENTIFICATION between 3.00 and 30.00 min.•A. The retention time of the major peak of the Sample Chromatogram similarity: The chromatogram of the solution corresponds to that of the Standard solution, as System suitability solution corresponds to that of the obtained in the Assay.reference chromatogram provided with USP•B. I DENTIFICATION T ESTS—G ENERAL, Chloride 〈191〉: Pro-Fondaparinux Sodium System Suitability Mixture B ceed as directed in the chapter. Meets the requirements RS.of the Chloride and Sulfate 〈221〉 test.Signal-to-noise ratio: NLT 10 for the fondaparinuxpeak in the chromatogram of the Sensitivity check ASSAY solution•P ROCEDURE Resolution: NLT 1.2 between fondaparinux related5 mM phosphate solution: 0.210g of monobasic so-compound C and fondaparinux related compound D,dium phosphate dihydrate and 0.650g of dibasic so-System suitability solution; NLT 1.1 betweendium phosphate dihydrate. Dissolve in and dilute with fondaparinux related compound F and fondaparinux water to 1000mL. pH is approximately 7.3.related compound G (see Table 2), System suitability Solution A: 15±10 ppm of dimethylsulfoxide (DMSO)solutionin 5 mM phosphate solution (1 in 67000, v/v)Standard agreement: The difference in the mean re-Solution B: 2.0 M sodium chloride solution in 5 mM sponse factors for each Standard solution is NMT phosphate solution 2.0%.Mobile phase: See Table 1. [N OTE—Make adjustments Relative standard deviation: For six consecutive in-to Solution A as necessary, and degas the Mobile phase jections of the Standard solution the calculated % RSD before use. Dissolved gas in the injected solution may of the area of the fondaparinux peak is NMT 2.0%.lead to baseline interference. Degassing of the Mobile The retention time of the fondaparinux peak should phase is critical to obtain a suitable signal-to-noise ratio be ±5% of the mean value. The calculated % RSD of and higher sensitivity. An eluant generator1 installed be-the response factors for six consecutive injections of tween the injector and the column may reduce the the Standard solution is NMT 2.0%. The calculated % baseline interference.]RSD of the pooled response factors for all injectionsof the Standard solution is NMT 2.0%. The % RSD of Table 1the mean response factors for the duplicate prepara-tions of the duplicate Standard solutions is NMT Time Solution A Solution B2.0%.(min)(%)(%)Analysis05050Samples:Standard solution and Sample solution55050Inject the Standard solution at least six times consecu-25595tively. Inject duplicate preparations of the Sample solu-tion. Record the chromatograms, and measure the re-30595tention times and areas for the major peaks (excluding 355050peaks before 3.00 and after 30.00 min).505050Calculations: For each injection of the Standard solu-tion calculate a response factor (F R): System suitability solution: 5.0mg/mL of USPFondaparinux Sodium System Suitability Mixture B RSF R = (C S/r S)Standard solution: 5.0mg/mL of USP FondaparinuxSodium for Assay RS in water. Prepare in duplicate.C S= concentration of fondaparinux sodium in theSensitivity check solution: 0.01mg/mL of USPStandard solution (mg/mL) Fondaparinux Sodium for Assay RS in water from ther S= peak response of fondaparinux sodium from Standard solutionthe Standard solution Sample solution: Transfer the contents of prefilled sy-Relative retention times (RRT) are calculated by ringes to a suitable container, and mix well. Dilute withdividing the retention time of the peak by the water, if needed, to obtain a 5.0-mg/mL solution ofretention time of fondaparinux established by the fondaparinux sodium.Standard solution. Using the mean response factor1One suitable eluant generator is Dionex DEGAS EG40/50 (12×17 cm, thick-(F M), calculate the concentration (mg/mL) ofness 2.2cm).。
编码产品名称硫氢化钠
五、消防措施 适当的灭火剂：可用雾状水、干粉、泡沫等灭火。 化学品产生的具体危险：在高温高热下燃烧分解，释放出有毒气体。 消防人员的特殊防护行动：消防人员必须配戴空气呼吸器、消防衣及防护手套，根据着火原 因选择适当灭火剂，在安全距离以外的上风向灭火。
六、意外释放措施 人身防范、保护设备和应急程序：建议应急处理人员戴正压式呼吸器，穿防毒工作服。不 要直接接触泄漏物。 环境防范措施：隔离泄漏污染区，限制出入。 抑制和清洁的方法和材料：小量泄漏：避免扬尘，用洁净的铲子收集于干燥、洁净、有盖的 容器中，转移至安全场所。切勿使产品进入下水道等限制性区域。大量泄漏：用塑料布、帆 布覆盖。使用无火花工具收集回收或运至废物处理场所处置。
十四、运输信息 联合国编号：2949。 联合国正式运输名称：氢硫化钠，含结晶水不低于 25%。 运输危险分类：8。 包装类别（如果适用）：II。 环境危险：/ 用户的特殊防范措施：/
十五、管理信息 国内化学品安全管理法规：本化学品安全数据单遵照了以下相关国家标准：GB 16483-2008、 GB 13690-2009、GB 6944-2012、GB/T 15098-2008、GB 18218-2009、GB 15258-2009、GB 190-2009、GB 191-2009、GB 12268-2008、GA 57-1993、GBZ 2-2007 以及相关法规：《铁路 危险货物运输管理规则》、《危险化学品安全管理条例》。
九物理及化学性质外观物理状态颜色等气味气味阈值ph熔点凝固点初始沸点和沸腾范围闪点蒸发速率易燃性固体气体上下易燃极限或爆炸极限蒸气压力蒸气密度相对密度可溶性分配系数
编 码： 产品名称：硫氢化钠
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可能腐蚀金属。吞咽会中毒。皮肤接触致命。造成严重皮肤灼伤和眼损伤。对水生生物有毒。