美国药典阿司匹林中英文对照

2024年10月25日发(作者：)

美国药典阿司匹林中英文对照

Aspirin

Acetylsalicyiic Add,ph Eur monograph 0309) C9H8O4180.2

[5O-78-2]

Action and use

Salicylate; non-selective cyclo-oxygenase inhibitor;

antipyretic; analgesic;

anti-inflammatory.

Preparations

Aspirin Tablets

Dispersible Aspirin Tablets

Effervescent Soluble Aspirin Tablets Gastro-resistant Aspirin

Tablets

Aspirin and Caffeine Tablets

Co-codaprin Tablets

Dispersible Co-codaprin Tablets

DEFINITION

2-(Acetyloxy)benzoic acid.

CONTENT

99.5 per cent to 101.0 per cent (dried substance).

CHARACTERS

Appearance

White or almost white, crystalline powder or colourless

crystals.

Solubility

Slightly soluble in water, freely soluble in ethanol (96 per

cent),

MP

About 143 °C (instantaneous method). IDENTIFICATION

First identification A, B.

Second identification B, C, D.

A. Infrared absorption spectrophotometry {2.2.24).

Comparison acetylsalicyiic acid CRS.

B. To 0.2 g add 4 ml of dilute sodium hydroxide solution R

and boil for 3 min. Cool and add 5 ml of dilute sulphuric add R

A crystalline precipitate is formed. Filter, wash the precipitate

and dry at 100-105 °C. The melting point (2.2.14) is 156 °C to

161 °C.

C. In a test tube mix 0.1 g with 0.5 g of

阿司司匹林

Acetylsalicyiic添加、ph值0309欧元专著) C9H8O4 180.2 [5O-

78-2]

作用和用途

水杨酸盐;选择性的环氧化酶抑制剂;解热、镇痛、抗炎。

准备

阿司匹林药片

阿司匹林分散片

阿司匹林泡腾片

阿司匹林抗胃片

阿司匹林和咖啡因药片

复方可待因阿司匹林片

复方可待因阿司匹林分散片

定义

2 -(乙酰氧基)苯甲酸。

内容

99.5%到101.0%(干物质)。

特性

外观

白色或几乎白色,结晶粉末或无色晶体。

溶解度

微溶于水,易溶于乙醇(96%)。

熔点

大约143°C(瞬时方法)。

鉴别

首先识别A,B。

第二个识别B,C,D。

a .红外吸收法{ 2.2.24)。

乙酰水杨酸 CRS 比较

b到0.2 g添加4 ml的氢氧化钠溶液的稀释R并且煮沸3分钟。

冷却后加5毫升的稀硫酸添加R

形成晶状沉淀。过滤,洗沉淀和干在100 - 105°C。熔点(2.2.14)是

156°C--160°C。

c .在试管中混合0.1g 和0.5 g的

calcium hydroxide R. Heat the mixture and expose to the

fumes produced a piece

of filter paper impregnated with 0.05 ml of

nitmbenzaldehyde solution R. A

greenish-blue or greenish-yellow colour develops on the

paper. Moisten the paper with dilute hydrochloric acid R. The

colour becomes blue.

ve with heating about 20 mg of the precipitate

obtained in identification test B in 10 ml of water R and cool. The

solution gives reaction (a) of salicylates {2.3.1).

TESTS

Appearance of solution

The solution is clear (2.2.1) and colourless (2.2.2, Method II)

.

Dissolve 1.0 g in 9 ml of ethanol (96 per cent) R.

Related substances

Liquid chromatography (2.2.29). Prepare the solutions

immediately before use.

Test solution Dissolve 0.10 g of the substance to be examined

in acetonitrile for chromatography R and dilute to 10.0 ml with

the same solvent.

Reference solution (a) Dissolve 50.0 mg of salicylic acid R in

the mobile phase and dilute to 50.0 ml with the mobile phase.

Dilute 1.0 ml of this solution to 100.0 ml with the mobile phase.

Reference solution (b) Dissolve 10.0 mg of salicylic acid R in

the mobile phase and dilute to 10.0 ml with the mobile phase. To

1.0 ml of this solution add 0.2 ml of the test solution and dilute

to 100.0 ml with the mobile phase.

Mobile phase phosphoric acid R, acetonitrile for

chromatography R, water R (2:400:600 VIVIV).

氢氧化钙 R 加热混合物，将薄层板用0.05 毫升的硝基苯甲醛溶液

溶解R.

蓝绿色或黄绿色的颜色在薄层板上生长。

把纸用稀盐酸弄湿，颜色就变成蓝色。

D.加热溶解大约20毫克在鉴定测试B的沉淀中的10毫升R水并

冷却。这个方案给予反应(一个)的水杨酸酯{ 2.3.1)。

测试

溶液的外观

溶液澄清，无色

溶解1.0 g在9毫升的乙醇(96%)R。

有关物质

液相色谱法(2.2.29)。准备使用前的溶液。

试验溶液溶解0.10 g的物质乙腈色谱审查R并用相同的溶剂稀释

到10.0毫升

参比溶液(a) 在流动相中溶解50.0 mg的水杨酸R 并稀释到50.0

毫升。用流动相稀释1.0毫升的这种溶液到100.0毫升。

参比溶液(b) 溶解10.0毫克的水杨酸R在流动相中并用流动相稀

释到10.0毫升。将1.0毫升的这种溶液和0.2毫升的测试溶液用流动

相稀释到

100.0ml 。

流动相磷酸R:乙腈R、水R(2:400:600 V/V/V)。

Flow rate 1 ml/min.

Detection Spectrophotometer at 237 nm, Injection 10 ul.

Reference solution (b):

-- resolution: minimum 6.0 between the 2 principal peaks

Limits:

-- any impurity: for each impurity, not more than the area of

the principal peak in the chromatogram obtained with reference

solution (a) (0.1 per cent);

--total: not more than 2.5 times the area of the principal peak

in the chromatogram obtained with reference solution (a) (0.25

per cent);

-disregard limit. 0.25 times the area of the principal peak in

the chromatogram obtained with reference solution (a) (0.025

per cent). Heavy metals (2.4.8)

Maximum 20 ppm.

Dissolve 1.0 g in 12 ml of acetone R and dilute to 20 ml with

water R. 12 ml of this solution complies with test B. Prepare the

reference solution using lead standard solution (1 ppm Pb)

obtained by diluting lead standard solution (100 ppm Pb) R with

a mixture of 6 volumes of water R and 9 volumes of acetone R.

Loss on drying (2.2.32)

Maximum 0.5 per cent, determined on 1.000 g by drying in

vacuo. , *

Sulphated ash (2.4.14)

Maximum 0.1 per cent, determined on 1.0 g. ASSAY

In a flask with a ground-glass stopper, dissolve 1.000 g in 10

ml of ethanol (96 per cent) R. Add 50.0 ml of 0.5 M sodium

hydroxide. Close the flask and allow to stand for 1 h.

Using 0.2 ml of phenolphthalein solution R as indicator,

titrate with 0.5 M hydrochloric acid. Carry out a blank titration.

1 ml of 0.5 M sodium hydroxide is equivalent to 45.04 mg of

C9H8O4流速 1毫升/分钟。

分光光度计检测在237 nm

注入10 ul。

系统适应性参考解决方案(b):

——解析度:最低的6.0到2个主要的山峰

限制:

——无杂质:对于每个杂质,不超过参比溶液(a)所得色谱图的主峰

面积(a)(0.1%);

——总:不大于由参比溶液(a)所得色谱图的主峰面积的0.25倍

(a)(0.25%);

--忽略不计：不大于由参比溶液(a)所得色谱图的主峰面积的0.25

倍(0.025%)。

重金属(2.4.8)

最大20 ppm。

溶解1.0 g在12毫升的丙酮R并用水R稀释到20毫升.12毫升

的这种溶液符合测试b .准备参考解决方案使用含铅标准溶液(1 ppm

Pb)得到稀释标准溶液铅(100 ppm Pb)R的混合物,6卷的水R和9卷

的丙酮R。

干燥失重(2.2.32)

1g样品在真空中干燥，失重不超过0.5%。

灰分(2.4.14)

1g样品中，不超过0.1%。

鉴别

用带磨砂玻璃瓶塞的烧瓶，溶解1.000 g在10毫升的乙醇(96%)r .

添加50.0毫升的0.5 M氢氧化钠。关闭烧瓶里然后允许放置1个小

时。

用0.2ml的酚酞溶液R为指示剂，滴定0.5M硫酸，完成空白滴

定。

1毫升的0.5 M氢氧化钠相当于45.04毫克C9H8O4

Aspirin Tablets

Aspirin Tablets contain not less than 90.0 percent and not

more than 110.0 percent of the labeled amount of aspirin

(C9H8O4). 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. Preserve

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 minutes,

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 alcohol for several

minutes. Centrifuge the mixture. Pour off the clear supernatant,

and evaporate it to dryness. Dry the residue in vacuum at 60° for

1 hour.

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 of 4.50±0.05;

500 mL.

Apparatus 1: 50 rpm.

Time: 30 minutes.

Procedure-Determine the amount of C9H8O4dissolved 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 Medium if necessary, in

comparison with a Standard solution having 阿司匹林片

阿司匹林药片含有90.O%--110.0%标示量的阿司

匹林。药片超过81毫克大小不含有甜味剂或其他添加剂。

注意——包有肠溶衣的药片需要符合阿司匹林的

要求。

包装和保藏—保存在密封容器中。保存81毫克大小或是更小的带

有香味或是甜味的药片每个容器不

超过36片。

USP参考标准< 11)-

USP阿司匹林RS USP水杨酸RS鉴别——

A:粉碎1片药片，50ML水煮沸5分钟,冷却,加1或2滴氯化铁 TS:

紫红色的产生。

B:红外吸收(197 K)-准备测试样如下。用10ml的酒精将些变成粉

末的药片（相当于500毫克阿司匹林）混合,振摇数分钟。用离心机分

离混合物，倒出上层清液,并蒸发到干燥。在60°C真空中干燥残留物

在1小时。

溶解(711)——

方法:0.05M醋酸缓冲区,准备通过混合2.99 g的醋酸钠和1.66毫

升的冰醋酸获得1000毫升pH值4.50 ±0.05的溶液;500毫升。

仪器1:50 rpm。

时间:30分钟。

步骤——在阿司匹林等吸收点的波长的紫外吸光度和和水杨酸

265±2nm过滤的试验溶液确定

C9H8O4的用量，与标准溶液相比，如果必要，适当用已知浓度

的USP阿司匹林RS相同物质稀释

a known concentration of USP Aspirin RS in the same

Medium.

Limit of free salicylic acid-

Mobile phase and Diluting solution^-Prepare as directed in

the Assay.

Standard solution-Dissolve an accurately weighed quantity

USP Salicylic Acid RS in the Standard preparation prepared as

directed in the Assay, to obtain a solution having a known

concentration of about 0.015 mg of salicylic acid per mL.

Test solution-Use the Stock solution prepared as directed for

Assy Preparation in the Assay.

Chromatographic system-Use the chromatographic system

described in the tograph the Standard,

solution,and record the peak responses as directed for Procedure:

the relative retention times are about 0.7 for salicylic acid and 1.0

for aspirin; the resolution, R, between salicylic acid and aspirin is

not less than 2.0; and the relative standard, deviation of the

salicylic acid peak responses is not more than 4.0%.

Procedure- Calculate the percentage of salicylic acid

(C7H6O3) in the portion of Tablets taken by the formula:

2000(C/QA)(rvJ rs). r

> Assay-

Mobile phase-Dissolve 2 g of sodium 1

-heptanesulfonate in a mixture of 850 mL of water and 150

mL of acetonitrile, and adjust with glacial acetic acid to a pH of

3.4. Diluting solution-Prepare a mixture of acetonitrile and formic

add (99:1). Standard preparation-Dissolve an accurately weighed

quantity of USP Aspirin RS in Diluting solution to obtain a

solution tsavlng a known concentration of about 0.5 mg per mL.

Assay preparation-Weigh and finely powder not fewer than

J Tablets. Transfer an accurately weighed quantity of the powder,

游离水杨酸限度

流动相和稀释溶液^ -在试验中按照指示做好准备。

标准溶液——在标准溶液制剂准备中溶解精密称

定的一个准确地重数量USP水杨酸RS,以得到一个

每毫升含水杨酸约0.015毫克的溶液。

试验溶液——使用原液按照指示准备试验中。

色谱系统-使用色谱法色谱标准分析标准溶液，记录最大峰值: 水

杨酸相对保留时间约为0.7和阿司匹林相对保留时间约为1.0;,R之间、

水杨酸和阿司匹林是不低于2.0,相对标准偏差的水杨酸峰值不

超过4.0%。

步骤——通过公式计算水杨酸(C7H6O3)在药片中的含量。

2000(C / QA)(rvJ rs)。 r

流动相-溶解 2 g的钠混合在850ml水和150ml乙腈中，并且用

冰醋酸调节PH至3.4.

稀释液——准备混合物的乙腈和甲酸（99:1）

标准液的制备——精密称取美国药典阿司匹林标准品并溶解在稀

释液中，去配制一个已知浓度约为每毫克0.5毫克的溶液。

样品的制备——称量和细粉不少于20片，准确称取细粉相当于

100毫克阿司匹林

equivalent to about 100 mg of aspirin, to a suitable gainer.

Add 20.0 mL of Diluting solution and about 10 beads,Shake

vigorously for about 10 minutes, and centrifuge (Stock solution)

Quantitatively dilute an accurately measured volume of the Stock

solution with 9 volumes of Diluting solution (Assay Ptyaroation).

Retain the remaining portion of Stock solution for the test for

Limit of free salicylic acid. Chromatographic system (see

Chromatography (621})-The liquid chromatograph is equipped

with a 280-nm detector and a 4.0-mm x 30-cm column

containing packing L1. The flow rate is about 2 ml. per minute.

Chromatograph the Standard preparation, and record the

peak responses as directed for Procedure: the tailing factor is not

greater than 2.0; and the relative standard deviation is not more

than 2.0%.

Procedure-Separately inject equal volumes (about 10 uL) of

the Standard preparation and the Assay preparation into the

chromatograph, record the chromatograms, and measure the

responses for the major peaks. Calculate the quantity, in mg, of

aspirin (C9H8O4) in the portion of Tablets taken by the formula:

200C(r u/r s) .

in which C is the concentration, in mg per mL, of USP Aspirin

RS in the Standard preparation; and r u and r s are the peak re-

sponses of the aspirin peaks obtained from the Assay preparation

and the Standard preparation, respectively. 置于合适的容器;加入

20ml稀释液和10滴溶液。用力振摇约10min 离心（原液）。定量稀

释精确测量体积的溶液成9倍稀释液（含量测定）保留一份作为无水

水杨酸的空白对照。

色谱系统（见色谱<621>）

液相色谱在280nm下测定，用4.0mmx30cm 的圆柱所包含L1,

这个流动速率大约为2毫升每分钟。

色谱的标准和记录峰值的频率较之前作为对照。拖尾因子不大于

2.0%。

步骤——分别进样等体积（约10ul）的标准品和样品进入色谱仪，

记录色谱图，并测量反应的主要峰。计算峰值，单位是mg。每份阿司

匹林C9H8O4 片的计算公式：

200C(r u/r s) .

其中C是浓度，单位是毫克每毫升。美国药典阿司匹林参比标准

品的标准制备r u和r s 的阿司匹林的峰值包含测定准备和标准制备。