普羅雌烯USP與EP質(zhì)量標(biāo)準(zhǔn)

1、普羅雌烯USP質(zhì)量標(biāo)準(zhǔn)起草,物料名稱(chēng),USP檢驗(yàn)項(xiàng),USP限度,EP檢驗(yàn)項(xiàng),EP限度,現(xiàn)有SOP檢驗(yàn)項(xiàng),現(xiàn)有SOP限度,現(xiàn)有SOP參考標(biāo)準(zhǔn)雌二醇,/,/,性狀,性狀,鑒別,鑒別,鑒別,1.應(yīng)符合規(guī)定2.在280nm的波長(zhǎng)處有最大吸收3.應(yīng)與對(duì)照的圖譜（光譜集681圖）一致。,USP,溶解性,熔程,173179,熔程,173179,熔程,175180,比旋度,為+76至 +83,比旋度,為+76至 +83,比旋度,為+76至 +83,水分,0.035,水分,0.500g限度2.9%3.5%,水分,0.035,色譜純度（HPLC）,任何一個(gè)雜質(zhì)峰均不得超過(guò)0.5%，總雜質(zhì)峰不得超過(guò)1.0%。,有關(guān)

2、物質(zhì),雜質(zhì)D校正因子：0.4雜質(zhì)A、B、C、D0.3%未知雜質(zhì)：0.1%雜質(zhì)總和：0.5%忽略限：0.05%,色譜純度（HPLC）,任何一個(gè)雜質(zhì)峰均不得超過(guò)0.5%，總雜質(zhì)峰不得超過(guò)1.0%。,熾灼殘?jiān)?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?xì)埩?3000ppm,廠方企業(yè)標(biāo)準(zhǔn),乙醇?xì)埩?5000ppm,廠方企業(yè)標(biāo)準(zhǔn)無(wú)水乙醇,/,/,性狀,性狀,GB/T678-2002,不少于99.5%,比重,0.7890.791,GB/T678-2002,鑒別,鑒別,水分,0.50%,GB/T678-200

3、2,外觀,含量,99.50%,GB/T678-2002,比重,0.8120.816（15.56）,相對(duì)密度,0.790 t 0.793,酸堿度,酸堿度,紫外吸收,吸光度,揮發(fā)性雜質(zhì)（GC）,甲醇200ppm乙醛10ppm苯2ppm其他雜質(zhì)的總和300ppm,雜質(zhì)（GC）,甲醇200ppm乙醛10ppm苯2ppm其他雜質(zhì)的總和300ppm忽略限：9ppm,不揮發(fā)殘?jiān)南薅?2.5mg/100ml,不揮發(fā)殘?jiān)南薅?25ppmm/V.,硫酸二甲酯,外觀, HG/T 4001-2008,酸度,不高于1.0%,含量（滴定）,不低于98.0%,氫化鈉,外觀,內(nèi)控標(biāo)準(zhǔn),含量,5763%,金屬鈉,無(wú),性狀,

4、/,GB 22379-2008,含量（滴定）,不小于99.2%,GB 22379-2008乙酸乙酯,/,/,性狀,外觀, GB/T 3728-2007,鑒別,鑒別,比重,0.8940.898 g/cm3（25）,相對(duì)密度,0.898 to 0.902,比重,0.8970.902（20）,中國(guó)藥典2010版,折光率,1.370 to 1.373,外觀,酸度,酸度,與硫酸的反應(yīng),有關(guān)物質(zhì),0.20%,蒸發(fā)殘留,30ppm,水分,0.10%,易碳化物,不揮發(fā)物限度,0.0002,不揮發(fā)物限度,0.01%,GB/T 3728-2007,甲基物的限度,色譜純度（GC）,含量（滴定）,99.0%100.5

5、%,含量（滴定）,不低于99.0%,中國(guó)藥典2010版正溴丙烷,無(wú),外觀,企業(yè)內(nèi)控,相對(duì)密度,1.3431.355,pH,6.07.0,水分,0.1%,無(wú)水硫酸鈉,無(wú),性狀,性狀,GB/T 6009-2003,鑒別,鈣鎂總含量,不大于0.3%,外觀,水分,不得過(guò)0.50%,酸堿度,硫酸鈉含量的測(cè)定,含Na2SO4不低于98.0%,氯化物,450ppm,鈣,450ppm,鐵鹽,90ppm,鎂,200ppm,重金屬,45ppm.,干燥失重,0.50%,含量（電位滴定）,98.5101.0%,氫氧化鈉,/,/,性狀,EP,鑒別,鑒別,/,/,溶液外觀,/,/,氯化物,50ppm,/,/,硫酸鹽,50

6、ppm,/,/,鐵鹽,10ppm,重金屬,30ppm,重金屬,20ppm,含量（滴定）, 95.0%100.5%,含量（滴定）, 97.0%100.5%,不溶性物質(zhì)和有機(jī)物質(zhì),/,/,鉀,/,/,甲醇,性狀,GB338-2004,鑒別,密度,0.7910.793g/cm3,中國(guó)藥典2010版,酸堿度,酸度或堿度,酸度不大于0.0050%,GB338-2004,/,/,堿度不大于0.0015%,GB338-2004,/,/,水分,不得過(guò)0.15%,中國(guó)藥典2010版,/,/,/,/,/,/,/,/,水分,0.1%,易碳化物,不揮發(fā)性雜質(zhì),2mg/250ml,丙酮和醛,0.00%,易氧化物,含量（

7、GC）,不小于99.5%,氯化鈉,溶液外觀,/,外觀,性狀, GB/T 1266-2006,鑒別,/,鑒別,氯化物和鈉,pH值,5.08.0,酸堿度,酸堿度,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,磷酸鹽限度,0.0025%,0.0025%,碘化物,碘化物,藍(lán)色不出現(xiàn),鎂和堿土金屬,0.01%,鎂和堿土金屬,100ppm,砷鹽,1g/g,砷鹽,1ppm,鐵鹽,2 g/g,鐵鹽,2ppm,鋇鹽,鋇鹽,1,亞鐵氰化物,亞鐵氰化物,藍(lán)色不出現(xiàn),硫酸鹽,0.020%,硫酸鹽,0.020%,亞硝酸鹽,亞硝酸鹽,1,重金屬,5ppm,重金屬,

8、5ppm,鉀,500ppm,鋁鹽,0.2ppm,細(xì)菌內(nèi)毒素,less than 5IU/g,含量（滴定）,99.0%100.5%,99.0%100.5%,二甲亞砜,性狀,外觀,GB/T 21395-2008中國(guó)藥典2010版,鑒別,鑒別,酸度,水分,不得過(guò)0.3%,相對(duì)密度,凝點(diǎn),吸光度,270350nm,有關(guān)物質(zhì),雜志總和0.1%,水分,不超過(guò)0.2%,普羅雌烯成品,無(wú),性狀（熔點(diǎn)、比旋度）,中國(guó)藥典YBH00302005,鑒別,有關(guān)物質(zhì)（HPLC）,有機(jī)溶劑殘留量（甲醇、乙醇）,甲醇0.08%乙醇0.079%,干燥失重,1.0%,熾灼殘?jiān)?0.1%,重金屬,10ppm,乙酸乙酯殘留,待確定,含量（HPLC）,98.50%,普羅雌烯中間體雌二醇丙基醚,/,/,性狀,企業(yè)內(nèi)控,/,/,水分,0.5%,/,/,熔點(diǎn),99.5102.0,