-
SUCROSE
Saccharurn
DEFINITION
β
-D-Fructofuranosyl
α
-D-glucopyranoside.
It contains no additives.
CHARACTERS
Appearance:
white or almost white, crystalline
powder, or shiny, colourless or white
or almost
white crystals
Solubility:
very soluble in
water, slightly soluble
in alcohol,
practically insoluble in ethanol
IDENTIFICATION
First identification
:
A.
Second identification
:
B, C.
A.
Infrared absorption spectrophotometry
(2.2.24).
Comparison
:
sucrose CRS.
B. Thin-layer
chromatography (2.2.27).
Test
solution.
Dissolve 10 mg of
the substance to be
examined in a
mixture of 2 volumes of
water R
and 3 volumes of
methanol R
and dilute to 20 ml
with the
same mixture of solvents.
Reference solution (a).
Dissolve 10 mg of
sucrose
CRS
in a mixture of
2
volumes of
water
R
and
3
volumes of
methanol R
and dilute to 20
ml with the
same mixture of solvents
。
Reference solution (b).
Dissolve 10 mg each of
fructose CRS, glucose CRS, lactose CRS
and
sucrose CRS
in a mixture of 2 volumes of
water
R
and 3
volumes of
methanol R
and
dilute to 20
ml with the same mixture
of solvents
Plate: TLC
silica gel G plate R.
Mobile phase: cold saturated boric acid
solution
R,
60
per
cent
V
/
v
solution
of
glacial
acetic
acid
R,
ethanol
R,
acetone
R,
ethyl
acetate
R <
/p>
(10:15:20:60:60
~/v/v/v/v).
Application:
2uL
蔗糖
定义
β
-D
-
呋喃果糖基
α
-D-
吡喃葡萄糖苷
性质
外观:
白色或接近白色晶体粉末,
或者是有光
泽的无色或白色或接近白
色的晶体。
溶解性:
在水中易溶,在乙醇中几乎不溶,微
溶于酒精。
鉴别
首先鉴别
A
项
其次鉴别
B
、
C
项
A
:红外光谱吸收
对照品:标准蔗糖
薄层色谱测试:
用甲醇水溶液
(
2:3=
水:
甲醇
)
溶解
10mg
的样品并定容至
20ml
。
参照溶
液
(a
)
:
用
甲醇水溶液(
2:3=
水:甲醇)
溶解
10mg
的蔗糖标准品并定容至
20m
l.
参照溶液(
b
)
:用甲醇水溶液(
2:3=
水:甲
醇
)溶解
10mg
的果糖标准品、葡萄糖标准品、
乳糖标准品、蔗糖标准品并定容至
20ml
。
色谱板:为硅胶板
展开剂:饱和醋酸
/60
%冰醋酸
/
乙醇
/
丙酮
/
乙
酸乙酯
R
=
10
:
15
:
20
:
60
:
60
(体积比)。
取样量:
2uL
Development:
in an
unsaturated tank over a path
of 15 cm.
Drying:
in a
current of warm air.
Detection
:
spray
with a solution of 0.5 g of
thymol R
in a mixture of 5 ml of
sulphuric acid
R
and 95 ml of
alcohol
R. Heat the plate at 130
System suitability:
the
chromatogram obtained
with reference
solution (b) shows 4 clearly
separated
spots
Results:
the principal
spot in the chromatogram
obtained with
the test solution is similar in
position, colour and size to the
principal spot in
the chromatogram
obtained with reference
solution (a).
C. Dilute 1 ml
of solution S (see Tests) to 100
ml
with
water R.
。
To 5 ml of the solution add
0.15 ml of freshly prepared
copper sulphate
solution R
and 2 ml of freshly prepared
dilute
sodium hydroxide
solution R.
。
The
solution is
blue and clear and remains
so after boiling. To
the hot solution
add 4 ml of
dilute hydrochloric
acid R
and boil for 1 min.
Add 4 ml of
dilute
sodium
hydroxide solution R.
An orange
precipitate is formed immediately.
TESTS
Solution S.
Dissolve 50.0 g
in
carbon
dioxide-free water
R
prepared from
distilled
water R
and dilute to 100 ml with
the same
solvent.
Appearance of solution.
Solution S is clear
(2.2.1).
Conductivity
(2.2.38)
:
maximum 35 pS-cm-'.
Dissolve
31.3
g
in
carbon
dioxide-free
water R
prepared from
distilled
water R
and dilute to 100
ml
with the same solvent.
展开:在不饱和展开缸中展开长度为
15cm
干燥:加热烘干
< br>测定:
用
0.5
%的麝香草酚溶
液(溶剂为
5ml
硫酸和
95ml
p>
酒精混合的溶液)浸湿后,在
130
℃下放
置
10min
)
系统适用性:
用参照溶液(
b
)获得的色谱图
呈
现
4
个明显分离的斑点)
.
结果:
测试液的色谱
图上最大的斑点的位置、
颜色、大小与参照溶液(
a
)的色谱图上的最
大的斑点相似)
C:<
/p>
用水稀释
1ml
的溶液
< br>S
到
100ml
,
在
5ml
该
溶液中加入新配
制的
0.15ml
硫酸铜溶液和新
配制
2ml
稀氢氧化钠溶液。
在溶液沸腾后
仍呈
现蓝色、
澄清,
在热溶液中加入<
/p>
4ml
盐酸沸腾
1min
后加入
4ml
的稀氢氧化钠溶液立刻产生
橙色沉淀。
测试:
溶液
S:
用新制备的无二氧化碳水溶解
50.0
g样
品,并用水定容至
100ml
。
<
/p>
溶液
S
外观:溶液澄清
< br>
电导率:<
35 pS-cm-'
<
/p>
用新制备的无二氧化碳水溶解
31.3
g
样品,
在
磁性搅拌下测量该溶液的电导率为
C
1
,然后
用
新制备的无二氧化碳水测量电导率为
C
< br>2
,
读数必需稳定,
30
s之内的变动不能
Measure
the
conductivity
of
the
solution
(C
1
),
while gently stirring with a magnetic
stirrer, and
that of the water used for
preparing the solution
(C
2
).
The
readings
must
be
stable
within
1
per
cent
over
a
period
of
30
s.
Calculate
the
conductivity
of
the
solution
of
the
substance
to
be examined from the following
expression:
C
1
-
0.35
C
2
通过下列公式计算出样品溶液的电导率。
C
1
-
0.35
C
2
Specific optical rotation
(2.2.7):
+
66.3
to
+
67.0.
比旋度:
+
66.3 to
+
67.0
Dissolve 26.0 g in
water R
and dilute to 100.0
ml with
the same solvent.
Colour value
:
maximum 45.
Dissolve 50.0 g
in 50.0 ml of
water R.
Mix,
filter
(diameter of pores 0.45 um) and
degas. Measure
the absorbance (2.2.25)
at 420 nm, using a cell
of at least 4
cm (a cell length of 10 cm or more is
preferred).
Calculate the colour value using the
following
expression:
A
×
1000
b
×
c
A
=
absorbance
measured a t 420 nm,
b
=
path length in centimetres,
c
=
concentration
of the solution, in grams per
millilitre, calculated from the
refractive index
(2.2.6) of the
solution; use Table 0204.-1 and
interpolate the values if necessary.
System
suitability:
-
repeatability:
the absolute
difference
between 2 results is maximum
3.
Dextrins.
If
intended for use in the preparation
of
large-volume infusions, it complies with the
test for dextrins.
To 2 ml
of solution S add
8
ml of
water R,
0.05 ml of
dilute hydrochloric
acid R
and 0.05 ml of
0.05 M
iodine.
The
solution remains
yellow.
p>
用水溶解
26.0
g样品并定容至
100.0ml
。
色值:不超过
45
< br>用水溶解
50.0
g样品,用
0
.45
um的膜过滤
后,用
4
cm的比色杯在
420
nm处测定吸光
值或是
10
cm或者更大的比色杯
通过下列公式计算色值
A
×
1000
b
×
c
A
=溶液在
420nm
处的吸收值
B
=吸收路径的长度,单位为
cm
)
C=
通过溶液折射率计算出溶液中的每毫升
的浓度
系统适用性
重现性:
两次测量结果的吸光值之间绝对误
差小于
3
)
糊精:
如果使用准备好的测试液测试糊精,
在
2ml
测试液中加入
8ml
水,
0.05ml
的稀盐酸和
0.
05ml
的
0,05M
的碘溶液,溶液
保持黄色)
Reducing sugars.
To 5 ml of
solution S in a
-
-
-
-
-
-
-
-
-
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