综合性药学实验药物分析实验 阿司匹林片的质量分析 0
阿司匹林片的质量分析 综合性药学实验-药物分析实验
0 阿司匹林片的处方 处方：阿司匹林 20.0g 淀粉 6.4g 酒石酸 0.08g 4%HPMC乙醇液(50%) Qs 滑石粉 2% 200片量 规格100mg/片
阿司匹林片的处方 处方：阿司匹林 20.0ｇ 淀粉 6.4 g 酒石酸 0.08 g 4%HPMC乙醇液(50%) QS 滑石粉 2% 200片量 规格100mg/片
中华人民共和国药典(2020版)第二部，666页 阿司匹林片 Asipilin Pian Aspirin Tablets 本品含阿司匹林(C,H.O4)应为标示量的95.0%一 105.0%. 【性状】本品为白色片。 【鉴别】(1)取本品的细粉适量（约相当于阿司匹林 0.1g),加水10ml,煮沸，放冷，加三氯化铁试液1滴，即显 紫堇色。 (2)在含量测定项下记录的色谱图中，供试品溶液主峰的 保留时间应与对照品溶液主峰的保留时间一致
中华人民共和国药典（2020版）第二部，666页
【检查】游离水杨酸临用新制。取本品细粉适量（约 相当于阿司匹林0.5g),精密称定，置100ml量瓶中，用1%冰 醋酸的甲醇溶液振摇使阿司匹林溶解，并稀释至刻度，摇匀， 用滤膜滤过，取续滤液作为供试品溶液，取水杨酸对照品约 15mg,精密称定，置50ml量瓶中，加1%冰醋酸的甲醇溶液溶 解并稀释至刻度，摇匀，精密量取5ml,置100ml量瓶中，用 1%冰醋酸的甲醇溶液稀释至刻度，摇匀，作为对照品溶液。 照阿司匹林游离水杨酸项下的方法测定。供试品溶液色谱图 中如有与水杨酸峰保留时间一致的色谱峰，按外标法以峰面 积计算，不得过阿司匹林标示量的0.3%
不做 溶出度取本品，照溶出度与释放度测定法（通则0931 第一法)，以盐酸溶液（稀盐酸24ml加水至1000ml,即得） 500ml(50mg规格)或1000ml(0.1g、0.3g、0.5g规格)为溶出 介质，转速为每分钟100转，依法操作，经30分钟时，取溶液 10m1滤过，取续滤液作为供试品溶液，另取阿司匹林对照品， 精密称定，加1%冰醋酸的甲醇溶液溶解并稀释制成每1ml中 含0.08mg(50mg、0.1g规格)、0.24mg(0.3g规格)或0.4mg (0.5g规格)的溶液，作为阿司匹林对照品溶液；取水杨酸对 照品，精密称定，加1%冰醋酸的甲醇溶液溶解并稀释制成每 1ml中含0.01mg(50mg、0.1g规格)、0.03mg(0.3g规格)或 0.05mg(0.5g规格)的溶液，作为水杨酸对照品溶液。照含量 测定项下的色谱条件，精密量取供试品溶液、阿司匹林对照品 溶液与水杨酸对照品溶液各10l,分别注入液相色谱仪，记录 色谐图。按外标法以峰面积分别计算每片中阿司匹林与水杨 酸含量，将水杨酸含量乘以1.304后，与阿司匹林含量相加即 得每片溶出量。限度为标示量的80%，应符合规定
不做
【含量测定】照高效液相色谱法（通则0512）测定。 色谱条件与系统适用性试验用十八烷基硅烷键合硅胶 为填充剂，以乙腈-四氢呋喃-冰醋酸-水(20：5：5：70)为流 动相；检测波长为276nm。理论板数按阿司匹林峰计算不低 于3000，阿司匹林峰与水杨酸峰的分离度应符合要求。 测定法取本品20片，精密称定，充分研细，精密称取细 粉适量（约相当于阿司匹林10mg),置100ml量瓶中，用1%冰 醋酸的甲醇溶液强烈振摇使阿司匹林溶解，并用1%冰醋酸 的甲醇溶液稀释至刻度，摇匀，滤膜滤过，取续滤液作为供试 品溶液，精密量取10l注人液相色谱仪，记录色谱图；另取阿 司匹林对照品，精密称定，珈1%冰醋酸的甲醇溶液振摇使溶 解并定量稀释制成每1ml中约含0.1mg的溶液，同法测定。 按外标法以峰面积计算，即得
Aspirin Tablets General Notices 英国药典(2018) Acetylsalicylic Acid Tablets Action and use Salicylate;non-selective cyclo-oxygenase inhibitor;antipyretic;analgesic;anti-inflammatory DEFINITION Aspirin Tablets contain Aspirin. gomply with the requirements stated under Tablets and with the foliowina Content of aspirin,CaHaO4 95.0 to 105.0%of the stated amount. IDENTIFICATION Boil 0.5 g of the powdered tablets for 2 to 3 minutes with 10 mL of 5M sodiwm hydroxide,cool and add an excess of 1M su/furic acid;a crystalline precipitate is produced.To a solution of the precipitate in water add iron(//l)chloride solution R1:a deep violet colour is produced. TESTS Salicylic acid containing 0.20 a temperatu transfe ssler cylinder of freshly prepared ammonium 80,8ae”2 wow tand o5028C8882 allow to stand for 1 minute.Any violet colour produced is su/fate solution R1 to a mixture of 3 mL of a freshly prepared 0.10%w/v solution of salicylic acid,2 mL of ethano/(96%)and sufficient water to produce 50 mL contained in a second Nessler cylinder (3.0%). Dissolution Comply with the requirements for Monographs of the British Pharmacopoeia in the disso/ution test for tablets and capsules,Appendix XII B1. TEST CONDITIONS (a)Use Apparatus 1,rotating the basket at 50 revolutions per minute. the medium. PROCEDURE
英国药典（2018）
(1)After 45 minutes withdraw a sample of the medium and measure the absorbance of the filtered sample,suitably diluted with the dissolution medium if necessary,at the maximum at 265 nm,Appendix ll B using dissolution medium in the reference cell. (2)Measure the absorbance of a suitable solution of aspirin BPCRS using dissolution medium in the reference cell. DETERMINATION OF CONTENT Calculate the total content of aspirin,CoHaO4,in the medium from the absorbances obtained and using the declared content of CaHaO4 in aspirin BPCRS ASSAY Weigh and powder 20 tablets.To a quantity of the powder containing 0.5 g of Aspirin add 30 mL of 0.5M sodium hydroxide VS,boil gently for 10 minutes and titrate the excess of alkali with 0.5M hydrochloric acid VS using phenol red solution as indicator.Repeat the operation without the substance being examined.The difference between the titrations represents the amount of sodium hydroxide required.Each mL of 0.5M sodium hydroxide VS is equivalent to 45.04 mg of CaHaO4. LABELLING The label states that the tablets contain Aspirin,unless this word appears in the name of the tablets.This requirement does not apply in countries where exclusive proprietary rights in the name Aspirin are claimed
USP41-NF36 Aspirin Tablets >Aspirin Tablets contain not less than 90.0 per- cent and not more than 110.0 percent of the la- beled amount of aspirin (CoH8O4).Tablets of larger than 81-mg size contain no sweeteners or other flavors. NOTE-Tablets that are enteric-coated meet the requirements for Aspirin Delayed-Release Tablets. Packaging and storage-Preserve in tight containers.Pre- serve flavored or sweetened Tablets of 81-mg size or smaller in containers holding not more than 36 Tablets each. USP Reference standards (11) USP Aspirin RS USP Salicylic Acid RS Identification- A:Crush 1 Tablet,boil it with 50 mL of water for 5 min- utes,cool,and add 1 or 2 drops of ferric chloride TS:a violet-red color is produced. B:Infrared Absorption (197K)-Prepare the test specimen as follows.Shake a quantity of finely powdered Tablets, equivalent to about 500 mg of aspirin,with 10 mL of alco- hol for several minutes.Centrifuge the mixture.Pour off the clear supernatant,and evaporate it to dryness.Dry the resi- due in vacuum at 60 for 1 hour
USP41-NF36
Dissolution(711〉- Medium:0.05 M acetate buffer,prepared by mixing 2.99 g of sodium acetate trihydrate and 1.66 mL of glacial acetic acid with water to obtain 1000 mL of solution having a pH of4.50±0.05；500ml. Apparatus 1:50 rpm. Time:30 minutes. Procedure-Determine the amount of CoHaO4 dissolved from UV absorbances at the wavelength of the isosbestic point of aspirin and salicylic acid at 265+2 nm of filtered portions of the solution under test,suitably diluted with Me- dium,if necessary,in comparison with a Standard solution having a known concentration of USP Aspirin RS in the same Medium.[NOTE-Prepare the Standard solution at the time of use.An amount of alcohol not to exceed 1%of the total volume of the Standard solution may be used to bring the Reference Standard into solution prior to dilution with Medium.] Tolerances-Not less than 80%(Q)of the labeled amount of CoHaO4 is dissolved in 30 minutes