Fagopyrin in fagopyrum dibotrys and method for measuring content of fagopyrin

The technology of golden buckwheat and buckwheat alkali is applied in the field of extraction and purification of buckwheat alkali in golden buckwheat and the field of rapid determination of content, which can solve the problems such as the extraction and purification process and content determination of buckwheat alkali in golden buckwheat, and achieve high extraction rate. Effect

Active Publication Date: 2017-11-24
ZHONGXING PHARM CO LTD JIANGSU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no relevant research report on the extraction and puri...

Method used

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  • Fagopyrin in fagopyrum dibotrys and method for measuring content of fagopyrin
  • Fagopyrin in fagopyrum dibotrys and method for measuring content of fagopyrin
  • Fagopyrin in fagopyrum dibotrys and method for measuring content of fagopyrin

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preparation example Construction

[0042](2) Preparation of reference substance solution: accurately weigh 20 mg of buckwheat alkali reference substance, put in a 25ml volumetric flask, add methanol to dissolve and dilute to the scale, shake well to obtain, and make stock solution;

[0043] (3) Preparation of the test solution: Accurately weigh 1 g of the dried and pulverized golden buckwheat medicinal material, put it in a 100ml round bottom flask, add 20mL of petroleum ether for degreasing treatment, reflux in a water bath for 1h, filter, and then use a small amount of Wash the residue with petroleum ether, evaporate the solvent, add precisely 40mL of methanol-0.05M hydrochloric acid solution (1:1), vortex mix for 20-30s, sonicate for 2-3min, centrifuge for 15-20min at 12000-15000 rpm , repeat the operation once, combine the extracts, let cool, transfer to a 100ml measuring bottle, dilute to volume with methanol, and shake well.

[0044] Method specificity: the reference substance solution and the test soluti...

Embodiment 1

[0055] An extraction and purification process and rapid determination method of buckwheat alkali in golden buckwheat, comprising the following steps:

[0056] Weigh 50 g of dried and pulverized golden buckwheat medicinal material, and extract twice with purified water at a solid-to-liquid ratio of 1:10, each time for 1.5 hours; after the combined filtrate is filtered, it is concentrated under reduced pressure (temperature 60°) to Density 1.15, get medicinal extract; Add 95% ethanol alcohol to the medicinal extract to sink to alcohol content 50%, centrifuge (rotating speed 4000r / min, centrifugation time is 10min) get supernatant; Select lewatit-100 strongly acidic cation exchange resin (dosage 100g, the supernatant volume of sample loading is 200ml), acid-base pretreatment is carried out after wet packing, and the alcohol precipitation supernatant is carried out dynamic adsorption with the flow rate of 0.8ml / min; Adopt 0.5mol / L ammonia water to wash Elute the above strong acidi...

Embodiment 2

[0058] An extraction and purification process and rapid determination method of buckwheat alkali in golden buckwheat, comprising the following steps:

[0059] Weigh 50 g of the dried and pulverized golden buckwheat medicinal material, and extract with purified water for 3 times at a solid-to-liquid ratio of 1:12, each time for 1 hour; after the combined filtrate is filtered, it is concentrated under reduced pressure to a relative density of 1.20 to obtain the Add 95% ethanol to the extract to ethanol content 40%, centrifuge to get the supernatant; choose lewatit-100 strong acidic cation exchange resin, carry out acid-base pretreatment after wet packing, and use 1.5ml / min The flow rate is to dynamically adsorb the alcohol precipitation supernatant; use 0.5mol / L ammonia water eluent to elute the above-mentioned strong acidic cation exchange resin with 6 times the column volume, control the flow rate of the eluent to 1.5ml / min, collect and elute Liquid; the collected eluate was c...

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Abstract

The invention provides fagopyrin in fagopyrum dibotrys and a method for measuring content of the fagopyrin. A process of performing water extraction, then performing alcohol precipitation and purifying through cation-anion resin is adopted, so that a sample treatment method is simple and convenient, has a relatively high extraction rate, can obtain a fagopyrin product with relatively high purity, and is suitable for industrial production. The method for measuring the content of the fagopyrin provided by the invention can be used for quickly, simply and conveniently measuring the content of the fagopyrin in fagopyrum dibotrys medicinal materials and the extracted and purified product, does not need to perform derivatization treatment, is convenient and quick, is good in repeatability, and is relatively suitable for measuring the content of the fagopyrin in conventional production practice.

Description

technical field [0001] The invention relates to the relevant technical field of extracting and detecting buckwheat alkaloids from the traditional Chinese medicine plant buckwheat aureus, in particular to an extraction and purification process and a rapid content determination method for buckwheat alkaloids in aureus buckwheat. Background technique [0002] Golden buckwheat is the dried rhizome of Fagoptrum dibotrys (D.Don) Hara, a plant of the Polygonaceae family. It tastes sour, bitter, and cold in nature. It returns to the lung, stomach, and liver meridian. Indications for lung abscess, lung-heat cough and asthma, sore throat, dysentery, rheumatic arthralgia, bruises, carbuncle sores and snake bites. Golden buckwheat was first recorded in Tang Dynasty's "Xinxiu Materia Medica" under the name of "Chidili". "Records "Growing in the plains of Jiangdong, the flowers and leaves are like buckwheat, the roots are as tight and hard as a dog's spine, one name is Wuji, and the othe...

Claims

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Application Information

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IPC IPC(8): C07D211/46C07D211/30G01N30/02G01N30/06
CPCC07D211/30C07D211/46G01N30/02G01N30/06
Inventor 杨琴武俊明曹旭郦红岩
Owner ZHONGXING PHARM CO LTD JIANGSU
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