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One-step method for separating pectin, chlorophyll and tigogenin in sisal pressed liquid

A technology of sisal saponin and squeeze liquid, which is applied in the direction of organic chemistry, steroids, etc., can solve the problem of single recycled products, and achieve the effects of increasing concentration, reducing cost, and improving purity

Inactive Publication Date: 2015-09-23
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above studies mainly focus on the production of pectin and saponin, and all of them use sisal paste as raw materials, and the recovered products are relatively single

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0032] 3) Preparation of sisal saponin: use the slag obtained in step 2) as raw material, add sulfuric acid according to the ratio of slag: 1.5mol / L sulfuric acid = 1:1, hydrolyze at 105-110°C for 6-8 hours, cool after hydrolysis to room temperature, add 2mol / L sodium hydroxide to neutralize while stirring, then filter to obtain the filter residue, wash the filter residue with water to remove Finally, dry at 80-100°C for 6-8 hours, grind the dried filter residue, use the finely ground filter residue as raw material, and use petroleum ether as the extraction agent for extraction. The extraction conditions are: 4-6 drops / s Reflux at a high speed for 6-8 hours, recover 70-80% of the extractant in the extract by vacuum concentration, cool the extract with ice-water mixture to 5-10°C and keep it for 2-3 hours, sisal saponin Crystals are formed, and then the crystals are filtered out, firstly washed with petroleum ether, and then dried at 80-100° C. for 1-2 hours to obtain sisal sa...

Embodiment 1

[0039] 1) Separation of pectin: obtain the sisal leaf squeeze liquid by mechanical pressing, add ethanol to the sisal leaf squeeze liquid while stirring until flocculent precipitation no longer occurs, then centrifuge at 3000r / min for 15min, To obtain the supernatant and flocculent precipitate, use the flocculent precipitate as raw material, add hydrochloric acid with a concentration of 0.06mol / L, wherein the amount of hydrochloric acid added is 10 times the mass of the flocculent precipitate, hydrolyze at 80°C for 1.5h, and the hydrolyzate After filtration and clarification, concentrate to a solid mass fraction of 3%. After concentration, add activated carbon for decolorization at 80°C for 10 minutes, then filter, add a 95% ethanol solution to the filtrate, and make the ethanol volume fraction reach 50% after adding the ethanol solution. %, the pectin is precipitated out, and then the pectin is obtained after pressure filtration, ethanol washing, vacuum drying and crushing;

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Embodiment 2

[0043] 1) Separation of pectin: obtain the sisal leaf squeeze liquid by mechanical pressing, add ethanol to the sisal leaf squeeze liquid while stirring until flocculent precipitation no longer occurs, and then centrifuge at 3000r / min for 12min, To obtain the supernatant and flocculent precipitate, use the flocculent precipitate as raw material, add hydrochloric acid with a concentration of 0.05mol / L, wherein the amount of hydrochloric acid added is 8 times the mass of the flocculent precipitate, hydrolyze at 85°C for 2 hours, and filter the hydrolyzed solution After clarification, concentrate to a solid mass fraction of 5%. After concentration, add activated carbon to decolorize at 85°C for 15 minutes, then filter, add a volume fraction of 75% ethanol solution to the filtrate, and make the volume fraction of ethanol reach 45% after adding the ethanol solution. , the pectin is precipitated out, and then the pectin is obtained after pressure filtration, ethanol washing, vacuum d...

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Abstract

The invention discloses a one-step method for separating pectin, chlorophyll and tigogenin in sisal pressed liquid. According to the invention, pectin in the sisal pressed liquid is separated with a flocculent precipitation method, and commercial pectin is obtained through a chemical treatment; a supernatant is concentrated, ethanol is recovered, and a paste is obtained; the dried and crushed paste is adopted as an extract material, and is subjected to Soxhlet extraction; a solvent is recovered, and chlorophyll is obtained; chlorophyll is adopted as a raw material, and water-soluble chlorophyll sodium copper salt is obtained; the extraction residue is adopted as a raw material, and steps such as hydrolysis, neutralization, filtration, washing, drying, extraction, cooling and drying are carried out, such that tigogenin is obtained. With the method provided by the invention, acid dose in tigogenin production can be reduced, environment pollution caused by tigogenin production can be controlled, pectin and chlorophyll resources in sisal are fully utilized, and tigogenin production cost is reduced.

Description

technical field [0001] The invention belongs to the field of pharmaceutical raw material production, and in particular relates to a method for separating pectin, chlorophyll and sisal saponin in sisal squeezed liquid by a one-step method. Background technique [0002] Sisal is a perennial, succulent, xerophyte of the Agave family. Native to Mexico's Longadan Peninsula, scientific name: Agave Sisalana Perrine. English name: Sisal. Alias: Sisar hemp. Sisal is a kind of leaf fiber crop. The sisal leaves are sword-shaped, hard and long and narrow. The leaves are generally 100cm-140cm long, 13cm-15cm wide, gray-green to blue-green. Sisal has the characteristics of temperature-loving and drought-tolerant, and is suitable for cultivation in tropical and subtropical regions. The main producing countries are Mexico, Brazil, Tanzania and other countries. In China, it mainly grows in Leizhou Peninsula and parts of Guangxi. [0003] Sisal leaves are pressed to obtain fibers and jui...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J71/00C07D487/22C08B37/06
CPCC07J71/0005C07D487/22C08B37/0045
Inventor 李祥王丽萍张彬师春兰豆静茹马倩鹤
Owner SHAANXI UNIV OF SCI & TECH
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