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Click to edit Master title style,Click to edit Master text styles,Second level,Third level,Fourth level,Fifth level,*,*,*,半期作业,1,取葡萄糖,4.0g,,加水,30ml,溶解后,加醋酸盐缓冲溶液(,pH3.5,),2.6ml,,依法检查重金属(中国药典),含重金属不得超过百万分之五,问应取标准铅溶液多少,ml,?(每,1ml,相当于,Pb10g/ml,),解:,标准铅溶液应取,2.0ml.,2,检查某药物中的砷盐,取标准砷溶液,2ml,(每,1ml,相当于,1g,的,As,)制备标准砷斑,砷盐的限量为,0.0001,,应取供试品的量为多少?,解:,供试品应取,2.0g,3.,肾上腺素中肾上腺酮的检查:称取肾上腺素,0.250g,,置于,25mL,量瓶中,加,0.05mol/L,盐酸液至刻度,量取,5mL,置另一,25mL,量瓶中,用,0.05mol/L,盐酸液稀释至刻度,用此液照分光光度法,在,310nm,处测定吸收度,不得大于,0.05,,问肾上腺素的限量是多少?(以百分表示,肾上腺素,Ecm1% =453,),解:,肾上腺酮的限量为,0.055%,4.,胃复康中检查二苯羟基乙酸的方法如下:取本品,0.5g,,酸性下用乙醚提取后蒸干,残渣用无水乙醇,10mL,溶解后,在,258nm,波长处测定吸收度,不得超过,0.02,求胃复康中二苯羟基乙酸的限量(以百分表示,二苯羟基乙酸在,258nm,波长处,Ecm,1%,的,19.7,),解:,胃复康中二苯羟基乙酸的限量为,0.02%,5.,取苯巴比妥,0.4045g,,加入新制的碳酸钠试液,16ml,使溶解,加丙酮,12ml,与水,90ml,,用硝酸银滴定液(,0.1025mol/L,)滴定至终点,消耗硝酸银滴定液,16.88 ml,,求苯巴比妥的百分含量(每,1ml0.1mol/L,硝酸银相当于,23.22mg,的,C,12,H,22,N,2,O,3,?,解:,苯巴比妥的含量为,99.3%.,6.,取标示量为,25mg,的盐酸氯丙嗪片,20,片,除去糖衣后称出总重为,2.412g,,研细,称出,0.2368g,,按药典方法测定含量,先配成,500ml,,滤过,稀释,20,倍后在,254nm,波长处测定吸收度为,0.435,。求该片剂按标示量表示的百分含量?(盐酸氯丙嗪的 以,915,计),解:,盐酸氯丙嗪片的标示量为,96.8,取标示量为,25mg,的盐酸氯丙嗪片,20,片,除去糖衣后称出总重,2.412g,,研细,精密称取适量,约相当于盐酸氯丙嗪,20mg,,问称取片粉的范围?,7.,取苯巴比妥对照品用适量溶剂配成,10g/ml,的对照液。另取,10,片苯巴比妥钠片,标示量为,75mg/,片,精密称定,重量为,1.5024g,,磨成片粉后,精密称取片粉,0.1021 g,(约相当于苯巴比妥钠,50mg,)。将供试品溶于水,加酸,用氯仿提取蒸干后,残渣用适当溶剂配成,100ml,供试品溶液。从中吸取,1.0ml,溶液用适当溶剂稀释至,50ml,,在,240nm,波长处测定吸收度,对照液为,0.431,,供试液为,0.392,,计算苯巴比妥钠片的标识量百分含量?(苯巴比妥钠与苯巴比妥的分子量之比为,1.095,),解:,苯巴比妥钠片的标示量为,97.70%.,8.,重酒石酸去甲肾上腺素注射液的含测:,对照品溶液制备:取重酒石酸去甲肾上腺素对照品约,70mg,,精密称定,置,25ml,量瓶中,加流动相溶解并稀释到刻度,摇匀,精密量取该溶液与内标溶液(,0.160mg/ml,)各,2ml,,置,10ml,量瓶中,用流动相稀释至刻度,摇匀即得。,供试品溶液的制备:精密量取标示量为,10mg/2ml,的重酒石酸去甲肾上腺素注射液,1ml,与内标溶液(,0.160mg/ml,),2ml,,至,10ml,的量瓶中,用流动相稀释至刻度,摇匀即得。,测定:取对照溶液和供试品溶液各,2ul,进样,测定对照品溶液中去甲肾上腺素和内标物的峰面积分别为,1635,和,1115,;供试品溶液中去甲肾上腺素的峰面积为,1454,,内标物的峰面积为,1123,。,试计算其含量占标示量的百分率,解:由于对照品溶液和供试品溶液稀释的倍数相同,所以可以直接按照对照品溶液和供试品溶液,10ml,中组分的量进行计算。先计算校正因子:,去甲肾上腺素标示量为,98.8%.,9.,阿莫西林克拉维酸钾片的,HPLC,法如下:,取本品,10,片,置,1000ml,量瓶中,加水适量,振摇使溶解,加水稀释至刻度,摇匀,精密量取,10ml,,置,50ml,量瓶中,加水稀释至刻度,摇匀,滤过,取续滤液,10,L,注入液相色谱仪,记录色谱图,,H,阿,.,样品,= 8.54,cm,H,克,.,样品,= 5.36 cm,。,另取阿莫西林对照品与克拉维酸对照品各适量,加水溶解,制成每,1 ml,中含阿莫西林,0.526mg,和克拉维酸,0.245mg,的混合液,同法测定,,H,阿,.,对照,= 8.25cm,H,克,.,对照,= 5.65cm,。,已知阿莫西林的标示量为,0.25g/,片,克拉维酸的标示量为,0.125g/,片,求阿莫西林的标示量,%,和克拉维酸的标示量,%,。,解:,(,1,)稀释倍数,D=1000,50/10=,5000,(,2,)阿莫西林:,C,样,= C,对,H,样,/H,对,= 8.54,0.526/8.25 = 0.544 mg/,mL,标示量,%= C,对,D/(10,片,标示量,),100% =0.544,5000/,(,10,0.25,1000,),100%= 108.8%,(,3,)克拉维酸:,C,样,= C,对,H,样,/H,对,= 5.36,0.245/5.65 = 0.232 mg/,mL,标示量,%= C,对,D/(10,片,标示量,),100% =0.232,5000/,(,10,0.125,1000,),100%= 92.8%,阿莫西林的含量为,108.8%,克拉维酸的含量为,92.8%,
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