蔗糖(欧洲药典方法)-整理稿

更新时间:2023-06-24 02:48:55 阅读: 评论:0

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 ethanolfauchon
IDENTIFICATION
First identification : A.
Second identification : B, C.
A. Infrared absorption spectrophotometry (2.2.24).
Comparison : sucro 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 beafraidmethanol R and dilute to 20 ml with the same mixture of solvents.
Reference solution (a). Dissolve 10 mg of sucro 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 fructo CRS, gluco CRS, lacto CRS and
sucro 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 pha: cold saturated boric acid solution R, 60 per cent jeremy sumpterV / v solution of glacial acetic acid R, ethanol R, acetone R, ethyl acetate R (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BC
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20ml.
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R1015206060(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.
长脸适合什么发型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 "C for 10 min.
System suitability: the chromatogram obtained with reference solution (b) shows 4 clearly parated 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 (e Tests) to 100 ml with water R. To 5 ml of the solution a
dd 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. 好听的英文名字女孩An orange precipitate is formed immediately.
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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. 环球雅思北京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
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).
结果:pardon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:用水稀释1ml的溶液S100ml,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50.0g样品,并用水定容至100ml
溶液S外观:溶液澄清
电导率:<35 pS-cm-'
用新制备的无二氧化碳水溶解31.3g样品,在磁性搅拌下测量该溶液的电导率为C1 ,然后用新制备的无二氧化碳水测量电导率为C2 ,读数必需稳定,30s之内的变动不能
Measure the conductivity of the solution (C1), while gently stirring with a magnetic stirrer, and that of the water ud for preparing the solution (C2). 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:
C1 - 0.35 C2
Specific optical rotation (2.2.7): + 66.3 to + 67.0.时代周刊年度人物
Dissolve 26.0 g in water R and dilute to 100.0 ml with the same solvent.
Colour value : going homemaximum 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; u 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 u 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.

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