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Method for separating emodin by means of co-crystallization

A technology of emodin and rhubarb, applied in the field of separation of emodin, can solve the problems of accelerated extraction rate, long synthesis route, large solvent consumption, etc., achieve rapid separation, facilitate industrial scale-up, and achieve low implementation costs

Inactive Publication Date: 2014-12-17
奉节县金云中药材种植专业合作社
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

supercritical fluid CO 2 The extraction method only reduces the impurities in the crude extraction, and cannot subdivide each anthraquinone component. If supercritical separation and purification is used, the process is cumbersome, and the equipment and instruments used make the cost higher
Patent 200510061919.2 provides the use of five extraction tanks for extraction in sequence to ensure that the medicinal materials and solvents in each extraction unit always maintain a large concentration difference and speed up the extraction rate, but it is only suitable for the countercurrent production of the tank group of Shujinfengshi wine
Patent 200910272508.6 describes the use of multiple ultrasonic extractions of crude emodin, and then using macroporous resin chromatography to separate and obtain more than 98% of high-purity emodin. Although problems such as loss and denaturation can be avoided, the process is still relatively cumbersome , only suitable for a small amount of separation in the laboratory
[0011] Chemical synthesis (for example CN200610067506.X; R.Eder, C.Widmer Helv.Chim., Acta., 1923,6,966-971; G.D.Graves, Roger Adams, J.Amer.Chem.Soc., 1923,45,2439 -2445; R.A.Jacobson, Roger Adams, J.Amer.Chem.Soc., 1924, 46, 1312-1317; N.R.Ayyangar, et al., J.Sci.Ind.Res., 1961, 20B, 493-499) Although it is possible to obtain emodin without relying on plant resources, this method has a long synthetic route and consumes a large amount of organic reagents, causing pollution to the environment, time-consuming and cost-intensive
[0012] Alumina chromatography or silicate chromatography, the procedures are cumbersome, time-consuming, solvent consumption is large, high cost, and the carrier will absorb part of the active ingredients; alkali concentration gradient method, the procedure is cumbersome, time-consuming, solvent consumption is large, and the cost is high ; Liquid-liquid extraction method, although the purity is high, but it takes a long time, the solvent consumption is large, and the procedure is cumbersome

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  • Method for separating emodin by means of co-crystallization
  • Method for separating emodin by means of co-crystallization

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Rhubarb total anthraquinone extract (purchased from Anhui Haozhou Kehui Pharmaceutical Co., Ltd., the first batch, containing 30% emodin, 25% other anthraquinones, determined by HPLC) 50.0g with 4.1g tert-butylamine, 6.7 1 g of isopropanol was mixed, and 98.0 ml of 75% ethanol in water was used as a solvent, heated to 80° C., and heated for 30 minutes to obtain a clear solution. Then within 4 hours, it was slowly cooled to 20° C. and stood for 6 hours to precipitate crystal I. Filter while recovering solvent and by-product mixture filtrate. Add 30.0ml of 85% ethanol to recrystallize the crystal I 13.3g, filter again, recover the ethanol solvent at the same time, then add 2.0mol / LH to the filter cake dropwise 2 SO 4Adjust the pH to 3 for decomposition, add 100mL of chloroform for extraction, take the organic layer to evaporate the solvent, recrystallize with 25.0ml of acetone, and finally dry to obtain 12.7g of emodin product with a purity of 98.4% and a yield of 84.7%...

Embodiment 2

[0034] Rhubarb total anthraquinone extract (purchased from Anhui Haozhou Kehui Pharmaceutical Co., Ltd., the second batch, containing 25% emodin, 23% other anthraquinones, determined by HPLC) 58.9g with 5.2g tert-butylamine, 6.5 Mix with 1 g of isopropanol, use 112.2ml of 85% ethanol as solvent, heat to 100°C, and heat for 40 minutes to obtain a clear solution. Then within 6 hours, it was slowly cooled to 10°C, and stood for 7 hours to precipitate crystal I. Filter while recovering solvent and by-product mixture filtrate. Crystal I13.1g was recrystallized by adding 25.2ml of 75% aqueous ethanol, and then filtered, while recovering the ethanol solvent, and then adding 2.0mol / L H 2 SO 4 Adjust the pH to 3.5 for decomposition, add 100mL of chloroform for extraction, take the organic layer to evaporate the solvent, recrystallize with 24.8ml of acetone, and finally dry to obtain 12.6g of emodin finished product with a purity of 97.8% and a yield of 85.6%. This embodiment uses HP...

Embodiment 3

[0038] Rhubarb total anthraquinone extract (purchased from Anhui Haozhou Kehui Pharmaceutical Co., Ltd., the third batch, containing 28% emodin, 26% other anthraquinones, determined by HPLC) 64.6g with 6.4g tert-butylamine, 7.3 1 g of isopropanol was mixed, and 125.4 ml of 95% aqueous ethanol was used as a solvent, heated to 70° C., and heated for 45 minutes to obtain a clear solution. Then within 8 hours, it was slowly cooled to -10°C, and stood for 8 hours to precipitate crystal I. Filter while recovering solvent and by-product mixture filtrate. Add 30.2ml methanol to recrystallize crystal I 15.7g, filter again, recover methanol solvent at the same time, then add 2.0mol / LH 2 SO 4 Adjust the pH to 2 for decomposition, add 100mL of chloroform for extraction, take the organic layer to evaporate the solvent, recrystallize with 28.6ml of ether, and finally dry to obtain 15.2g of emodin product with a purity of 99.2% and a yield of 84.0%. This embodiment uses HPLC to measure th...

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Abstract

The invention discloses a method for separating emodin by means of co-crystallization. According to the method, the rheum officinale total anthraquinone extract is an extract extracted by a reflux method by using rheum officinale rhizome as alcohol. The method comprises the following steps of: mixing the rheum officinale total anthraquinone extract with tert-butylamine and isopropanol, using 75%-95% hydrous ethanol as a solvent to have a full stirring reaction at 70-100 DEG C to obtain a settled solution; slowly cooling the obtained settled solution to minus 10-20 DEG C within 4-8 hours, silencing the solution until crystal is separated; filtering the solution to obtain a filter cake and a filtrate, re-crystallizing the filter cake by methanol or 75%-85% hydrous ethanol, adding an acid water solution to regulate the pH value of the obtained crude crystal product to 2-4 for decomposing, then adding chloroform for extraction, getting the organic layer, separating the solvent by evaporation to obtain a crude emodin product, and re-crystallizing the crude emodin product to obtain a pure emodin product. The method disclosed by the invention is simple in process and low in cost, and the obtained emodin has high yield and purity.

Description

(1) Technical field [0001] The invention relates to a method for separating emodin, in particular to the extraction of effective components from the traditional Chinese medicine rhubarb. (2) Background technology [0002] Rhubarb (Radix et Rhizoma Rhei Palmati) is the dried root and rhizome of Rheum palmatum L., Rheum tanguticum Maxim.ex Balf. or medicinal rhubarb (Rheum officinale Baill.) , named after its large shape and yellow color. The traditional Chinese medicine rhubarb is one of the famous specialty medicinal materials and clinical commonly used traditional Chinese medicine in my country. There are 39 varieties and 2 varieties in China. It has a long history of medicinal use and unique efficacy. It is cold in nature and bitter in taste. It can treat hot knot constipation, stagnant abdominal pain, damp-heat jaundice, and acute appendicitis, and can significantly repair chronic kidney function. It can be used externally to treat burns and scalds; it can also be used in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C46/10C07C50/34
Inventor 金志敏王聪李亚琴吕加恩周小波
Owner 奉节县金云中药材种植专业合作社