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蔗糖(欧洲药典方法)-整理稿

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2021-01-31 16:40
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2021年1月31日发(作者:马达加斯加岛)


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




其次鉴别


B



C




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

/



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:



0.5


%的麝香草酚溶 液(溶剂为


5ml


硫酸和


95ml


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)


.

< p>



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

< p>
)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



100ml




5ml



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,



磁性搅拌下测量该溶液的电导率为

C


1



,然后


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.









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

< p>
=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

< p>
3





糊精:


如果使用准备好的测试液测试糊精,



2ml


测试液中加入


8ml

水,


0.05ml


的稀盐酸和


0. 05ml



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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