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

A technology of sisal saponin and squeezing liquid, applied in the directions of steroids, organic chemistry, etc., can solve the problems of low utilization rate, high cost, large amount of acid and organic extractant, etc., to reduce production cost, control pollution, The effect of improving purity

Active Publication Date: 2015-04-29
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The object of the present invention is to provide a method for separating pectin, chlorophyll and sisal saponin in sisal squeezed liquid by one-step method, which overcomes the low utilization rate of existing sisal juice, high cost, and sisal saponin Problems of low purity, large amount of acid and organic extractant used in production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0037] 3) Preparation of sisal saponin

[0038] Use the filter residue obtained by the above process as raw material, add sulfuric acid according to the ratio of filter residue: 1.5mol / L sulfuric acid = 1:1, hydrolyze at 108°C for 6-8h, cool to room temperature, add 2mol / L sodium hydroxide solution while stirring Neutralize, filter, and wash the filter residue with water until the filtrate does not contain SO4 -- , collect the filter residue, dry the filter residue at 80-100°C for 4-6 hours, grind the filter residue finely, use the finely ground (crushed) filter residue as the raw material, use petroleum ether as the extraction agent, and extract for 6-8 hours by Soxhlet extraction method. The extract is concentrated in vacuum to recover part of the petroleum ether, cooled and crystallized, and filtered to obtain sisal saponin with a purity of 92-98%.

Embodiment 1

[0040] The method for separating pectin, chlorophyll and sisal saponin in sisal squeezed liquid by one-step method comprises the following steps:

[0041] 1) Pectin separation

[0042] Take 1000mL of sisal pressing liquid, add 800mL of industrial ethanol while stirring, stop stirring after flocculent precipitates are formed, centrifuge at 3000r / min for 15min, collect the supernatant and flocculent precipitates, and use the flocculent precipitates as Raw material Preparation of pectin with a degree of esterification of 20%.

[0043] 2) Chlorophyll separation

[0044] Using the above supernatant as a raw material, recover ethanol at a vacuum of 0.085 MPa and a temperature of 45°C to obtain a paste, put the paste in an oven at 85°C to dry for 6 hours, grind or pulverize, and grind (finely grind) ) dry paste as raw material, take ether (acetone) as extractant, reflux for 6h at a reflux rate of 4 drops / s, cool to room temperature and separate to obtain extract and slag (paste tha...

Embodiment 2

[0048] The method for separating pectin, chlorophyll and sisal saponin in sisal squeezed liquid by one-step method comprises the following steps:

[0049] 1) Pectin separation

[0050] Take 1000mL of sisal pressing liquid, add 1000mL of industrial ethanol while stirring, stop stirring after flocculent precipitates are formed, centrifuge at 3000r / min for 12min, collect supernatant and flocculent precipitates, and use flocculent precipitates as Raw material Preparation of pectin with a degree of esterification of 18%.

[0051] 2) Chlorophyll separation

[0052] Using the above supernatant as raw material, recover ethanol at a vacuum of 0.009MPa and a temperature of 40°C to obtain a paste, put the paste in an oven at 80°C to dry for 6 hours, grind or pulverize, and use the pulverized dry paste As raw material, take diethyl ether (acetone) as extractant, reflux for 6h at a reflux rate of 6 drops / s, cool to room temperature and separate to obtain extract and slag (paste from whic...

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Abstract

The invention discloses a one-step method for separating pectin, chlorophyll and tigogenin in sisal hemp pressed liquor and belongs to the field of medicinal raw material production. The method comprises the following steps: 1) adding ethanol to the sisal hemp pressed liquor and stirring until no flocks are generated, and centrifuging to obtain a liquid supernatant and flocks for producing the pectin; 2) recovering the ethanol in the liquid supernatant to obtain a paste, drying, crushing, performing soxhlet extraction and separating to obtain an extract and a paste removed from the chlorophyll; recovering the solvent to obtain a chlorophyll extract, and performing a saponification or iron or copper substitution reaction to form a salt, thereby obtaining water-soluble sodium ferrous chlorophyllin or sodium copper chlorophyllin; 3) adding sulfuric acid to the paste removed from the chlorophyll, cooling after reflux hydrolysis, regulating the reaction system to be neutral by use of a base, and filtering to collect the filter residue; and 4) washing the filter residue and then drying, performing soxhlet extraction, and then recovering the solvent, filtering and washing to obtain the tigogenin. The method has the advantages of high sisal hemp liquor utilization rate, low cost and high tigogenin purity.

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 squeezed to obtain fibers and si...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/22C07J71/00C08B37/06
CPCC07D487/22C07J71/0005C08B37/0003
Inventor 李祥豆静茹马倩鹤王丽萍张彬师春兰
Owner SHAANXI UNIV OF SCI & TECH