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Overview
Rutin is widely found in the plant community and has been found to contain at least 70 species of plants, such as tobacco leaves, eucalyptus flowers, buckwheat and dandelion. In particular, eucalyptus rice (an unoolved bud for the plant Sophorajaponica) and buckwheat are the highest content and can be used as raw materials for the large extraction of reeds. Reedin is a dehydrated glycoside of hydroxy and rutinose on three bits of Quercetin, a double sugar made up of glucose and Rhamnose.
reeds are light yellow powder or very fine needle-like crystallization, containing three molecules of crystalline water, melting point of 174 to 178 degrees C, no water 188 to 190 degrees C. Solubility: 1:10000 in cold water; 1:200 in hot water; 1:650 in cold ethanol; 1:60 in hot ethanol; and 1:12 in cold water. Micro-soluble in acetone, ethyl acetate, insoluble in benzene, ether, chloroform, petroleum ether, soluble in alkali and yellow.
reeds have a vitamin P-like effect. Helps to maintain and restore the normal elasticity of capillaries, mainly used as an auxiliary treatment for the prevention and treatment of hypertension, but also for the prevention and treatment of other hemorrhage caused by the lack of reeds.the purpose and requirements of the experiment
1. Objective:
(1) to master the principle and operation of the extraction of flavonoids by alkali-acid method through the extraction and refining of reeds.
(2) through the detection of reed structure, to understand the general procedures and methods of glycosine structure research.
(3) to understand the application of UV and NMR in the structural identification of flavonoids.
2. Requires
(1) to obtain the following three compounds: reedin, quercetin, reedin full acetyl compounds.
(2) can be based on chemical tests and UV, NMR data to initially infer the structure of reeds. There is also a general understanding of the structural determination of flavonoids.test method
1. Extraction and separation of reeds
2. The identification of reeds
1) the qualitative reaction of reeds
take reeds 3 to 4 mg, add ethanol 5 to 6 ml to dissolve it, divided into three parts for the following tests:
A. Take the above solution 1 to 2 ml, plus 2 drops of thick hydrochloric acid, in the discretionary addition of a little magnesium powder, pay attention to observe color changes.
B. Take 1 to 2 ml of the above solution, then add 2% citric acid methanol solution, pay attention to observe color changes, continue to
trol tube
to add 2% ZrOCl2 methanol solution, and record color changes in detail.
C. Take 1 to 2 ml of the above solution, and then add 10% α- volume of phenol ethanol solution, shake well, along the pipe wall drops with thick sulfuric acid, pay attention to observe the color changes produced by the two liquid surfaces.
2) Ultraviolet
spectral
analysis of reeds
reedin dissolved in
chromatography
pure methanol, add the prescribed
reagement
, determine its UV spectrum, test the spectrum and initially determine its structure.
3) Reed's NMR spectrum resolution
. A. Analysis of the NMR spectrum of trimethyl silicon ether NMR spectrum of reedin
B. NMR spectral analysis
4) identification of sugar and glycosides after reedin hydrolysing
A. Hydrolytic method: precision name reed 1g (±0.01g), plus 1% sulphuric acid 100ml,
heat
40min, set aside calmly,
filter
. The resulting precipitation is washed with a little water to remove the acid,
dry
weighing, calculating the weight ratio of the glycoside to the sugar. It is then recrystryed with ethanol (95% about 10 ml), i.e. the nucleotide.
identification of B. nucleotides: paper chromatography and
control
control.the main points and considerations of this experiment
(1) reed extraction method, focusing on the principle of alkali-acid method and precautions.
(2) the purpose, significance and considerations of qualitative experiments.
(3) UV and NMR spectra in reed structure detection.
.