-
Aspirin
Acetylsalicyiic Add,ph
Eur monograph 0309)
C
9
H
8
O
4
< br>
180.2
[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
Acetylsal
icyiic
添加、
ph
值
0309
欧元专著
)
C
9
H
8
O
4
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
<
/p>
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
C
9
H
8
O<
/p>
4
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
< br>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
0.2
ml
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<
/p>
氢氧化钠相当于
45.04
毫克
C
9
H
8
O
4
Aspirin Tablets
? Aspirin Tablets contain not less than
90.0
percent and not more than 110.0
percent of
the labeled amount of
aspirin (C
9
H
8
O
4
).
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
C
9
H
8
O
< br>4
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
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<
/p>
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。
< br>
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
——<
/p>
A:
粉碎<
/p>
1
片药片，
50ML
水煮沸
5
分钟
,
< br>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<
/p>
: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
< br>4.50
±
0.05
的溶液<
/p>
;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
C
9
H
8
O
< br>4
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