普罗雌烯USP与EP质量标准

1、普罗雌烯USP质量标准起草,物料名称,USP检验项,USP限度,EP检验项,EP限度,现有SOP检验项,现有SOP限度,现有SOP参考标准雌二醇,/,/,性状,性状,鉴别,鉴别,鉴别,1.应符合规定2.在280nm的波长处有最大吸收3.应与对照的图谱（光谱集681图）一致。,USP,溶解性,熔程,173179,熔程,173179,熔程,175180,比旋度,为+76至 +83,比旋度,为+76至 +83,比旋度,为+76至 +83,水分,0.035,水分,0.500g限度2.9%3.5%,水分,0.035,色谱纯度（HPLC）,任何一个杂质峰均不得超过0.5%，总杂质峰不得超过1.0%。,有关

2、物质,杂质D校正因子：0.4杂质A、B、C、D0.3%未知杂质：0.1%杂质总和：0.5%忽略限：0.05%,色谱纯度（HPLC）,任何一个杂质峰均不得超过0.5%，总杂质峰不得超过1.0%。,炽灼残渣,0.10%,含量（HPLC）,97.0%103.0%,含量（HPLC）,97.0%103.0%,含量（HPLC）,97.0%103.0%,甲醇残留,3000ppm,厂方企业标准,乙醇残留,5000ppm,厂方企业标准无水乙醇,/,/,性状,性状,GB/T678-2002,不少于99.5%,比重,0.7890.791,GB/T678-2002,鉴别,鉴别,水分,0.50%,GB/T678-200

3、2,外观,含量,99.50%,GB/T678-2002,比重,0.8120.816（15.56）,相对密度,0.790 t 0.793,酸碱度,酸碱度,紫外吸收,吸光度,挥发性杂质（GC）,甲醇200ppm乙醛10ppm苯2ppm其他杂质的总和300ppm,杂质（GC）,甲醇200ppm乙醛10ppm苯2ppm其他杂质的总和300ppm忽略限：9ppm,不挥发残渣的限度,2.5mg/100ml,不挥发残渣的限度,25ppmm/V.,硫酸二甲酯,外观, HG/T 4001-2008,酸度,不高于1.0%,含量（滴定）,不低于98.0%,氢化钠,外观,内控标准,含量,5763%,金属钠,无,性状,

4、/,GB 22379-2008,含量（滴定）,不小于99.2%,GB 22379-2008乙酸乙酯,/,/,性状,外观, GB/T 3728-2007,鉴别,鉴别,比重,0.8940.898 g/cm3（25）,相对密度,0.898 to 0.902,比重,0.8970.902（20）,中国药典2010版,折光率,1.370 to 1.373,外观,酸度,酸度,与硫酸的反应,有关物质,0.20%,蒸发残留,30ppm,水分,0.10%,易碳化物,不挥发物限度,0.0002,不挥发物限度,0.01%,GB/T 3728-2007,甲基物的限度,色谱纯度（GC）,含量（滴定）,99.0%100.5

5、%,含量（滴定）,不低于99.0%,中国药典2010版正溴丙烷,无,外观,企业内控,相对密度,1.3431.355,pH,6.07.0,水分,0.1%,无水硫酸钠,无,性状,性状,GB/T 6009-2003,鉴别,钙镁总含量,不大于0.3%,外观,水分,不得过0.50%,酸碱度,硫酸钠含量的测定,含Na2SO4不低于98.0%,氯化物,450ppm,钙,450ppm,铁盐,90ppm,镁,200ppm,重金属,45ppm.,干燥失重,0.50%,含量（电位滴定）,98.5101.0%,氢氧化钠,/,/,性状,EP,鉴别,鉴别,/,/,溶液外观,/,/,氯化物,50ppm,/,/,硫酸盐,50

6、ppm,/,/,铁盐,10ppm,重金属,30ppm,重金属,20ppm,含量（滴定）, 95.0%100.5%,含量（滴定）, 97.0%100.5%,不溶性物质和有机物质,/,/,钾,/,/,甲醇,性状,GB338-2004,鉴别,密度,0.7910.793g/cm3,中国药典2010版,酸碱度,酸度或碱度,酸度不大于0.0050%,GB338-2004,/,/,碱度不大于0.0015%,GB338-2004,/,/,水分,不得过0.15%,中国药典2010版,/,/,/,/,/,/,/,/,水分,0.1%,易碳化物,不挥发性杂质,2mg/250ml,丙酮和醛,0.00%,易氧化物,含量（

7、GC）,不小于99.5%,氯化钠,溶液外观,/,外观,性状, GB/T 1266-2006,鉴别,/,鉴别,氯化物和钠,pH值,5.08.0,酸碱度,酸碱度,含量,不得低于99.5%,干燥失重,0.5%,0.5%,溴化物限度,0.010%,溴化物,100ppm,磷酸盐限度,0.0025%,0.0025%,碘化物,碘化物,蓝色不出现,镁和碱土金属,0.01%,镁和碱土金属,100ppm,砷盐,1g/g,砷盐,1ppm,铁盐,2 g/g,铁盐,2ppm,钡盐,钡盐,1,亚铁氰化物,亚铁氰化物,蓝色不出现,硫酸盐,0.020%,硫酸盐,0.020%,亚硝酸盐,亚硝酸盐,1,重金属,5ppm,重金属,

8、5ppm,钾,500ppm,铝盐,0.2ppm,细菌内毒素,less than 5IU/g,含量（滴定）,99.0%100.5%,99.0%100.5%,二甲亚砜,性状,外观,GB/T 21395-2008中国药典2010版,鉴别,鉴别,酸度,水分,不得过0.3%,相对密度,凝点,吸光度,270350nm,有关物质,杂志总和0.1%,水分,不超过0.2%,普罗雌烯成品,无,性状（熔点、比旋度）,中国药典YBH00302005,鉴别,有关物质（HPLC）,有机溶剂残留量（甲醇、乙醇）,甲醇0.08%乙醇0.079%,干燥失重,1.0%,炽灼残渣,0.1%,重金属,10ppm,乙酸乙酯残留,待确定,含量（HPLC）,98.50%,普罗雌烯中间体雌二醇丙基醚,/,/,性状,企业内控,/,/,水分,0.5%,/,/,熔点,99.5102.0,