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Preparation method of high-content alliin

A technology with high content of alliin, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of immature production technology, achieve the effect of reducing the concentration time of rotary steaming and ensuring stability

Active Publication Date: 2016-05-04
青岛博恩高科生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, although there have been many studies on garlic extract, the production process for the efficient separation and extraction of one of the sulfur-containing compounds-alliin is not yet mature enough

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The preparation method of the high-content alliin described in the present embodiment comprises the following steps:

[0033] 1. Weigh 100g of peeled and clean garlic cloves, and heat them in high-heat microwave for 1min;

[0034] 2. Beat with 200ml of ethyl acetate, and then pass through a 20-mesh sieve;

[0035] 3. Discard the ethyl acetate layer, collect the filter residue, then add 100ml of 20% ethanol aqueous solution, mix well, extract by ultrasonic for 15min, centrifuge at 4000rpm for 10min, repeat the extraction twice, add 100ml extractant each time, shake and mix well , ultrasound, centrifugation;

[0036] 4. Collect the filtrate after 3 extractions, and concentrate to about 35ml by rotary evaporation at 60°C;

[0037] 5. Then use 2M hydrochloric acid to adjust the pH value of the concentrated solution to less than 4.5;

[0038] 6. Use strong acid cation exchange resin type 732 for further separation, and then use 0.5M ammonia water for elution, one collecti...

Embodiment 2

[0051] The preparation method of the high-content alliin described in the present embodiment comprises the following steps:

[0052] 1. Weigh 100g of peeled and clean garlic cloves, and heat them in high-heat microwave for 5 minutes;

[0053] 2. Beat with 300ml of ethyl acetate, and then pass through a 20-mesh sieve;

[0054] 3. Discard the ethyl acetate layer and collect the filter residue. Then add 300ml of 50% ethanol aqueous solution once, after mixing, ultrasonic extraction, time 10min, 4000rpm centrifugal 10min,

[0055] 4. Collect the filtrate and concentrate it to about 35ml by rotary evaporation at 60°C;

[0056] 5. Then use 2M hydrochloric acid to adjust the pH value of the concentrated solution to less than 4.5;

[0057] 6. Use strong acid cation exchange resin type 732 for further separation, and then use 0.5M ammonia water for elution, one collection bottle for each 50ml. TLC identified all the components where alliin was located, and after summarizing, concen...

Embodiment 3

[0061] The preparation method of the high-content alliin described in the present embodiment comprises the following steps:

[0062] 1. Weigh 100g of peeled and clean garlic cloves, and heat them in high-heat microwave for 8 minutes;

[0063] 2. Beat with 200ml of ethyl acetate, and then pass through a 20-mesh sieve;

[0064] 3. Discard the ethyl acetate layer, collect the filter residue, add 300ml of 50% ethanol aqueous solution, mix well, extract by ultrasonic for 15min, and centrifuge at 4000rpm for 10min;

[0065] 4. Collect the filtrate after 3 extractions, and concentrate to about 35ml by rotary evaporation at 60°C;

[0066] 5. Then use 2M hydrochloric acid to adjust the pH value of the concentrated solution to less than 4.5;

[0067] 6. Use strong acid cation exchange resin type 732 for further separation, and then use 0.5M ammonia water for elution, one collection bottle for each 50ml. TLC identified all the components where alliin was located, and after summarizing, ...

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Abstract

The invention discloses a preparation method of high-content alliin. The preparation method comprises the steps of firstly performing enzyme deactivation treatment on garlic by a microwave heating mode; then adding an appropriate ratio of ethyl acetate into garlic cloves after enzyme deactivation for beating, sieving, and collecting filter residues; then adding ethanol water, performing supersonic extraction, then performing centrifugation, finally collecting filter liquor after the supersonic extraction and centrifugation, performing vacuum concentration, and adjusting the pH value of a concentrated solution by using hydrochloric acid; performing further separation by using strong acid type cation exchange resin, eluting with ammonium hydroxide, collecting eluant, performing TLC (Thin-Layer Chromatography) identification, and determining a component containing the alliin; performing vacuum concentration again after aggregation, drying, so as to obtain a crude product of the alliin, then adding an appropriate ratio of the ethanol water again, performing cold storage and standing, and crystallizing, thus a refined product of the alliin is obtained.

Description

technical field [0001] The invention relates to a production process of garlic extract, in particular to a preparation method of high-content alliin. Background technique [0002] Garlic is the underground bulb of the Allium plant in the Liliaceae family. Modern medical research has confirmed that garlic has more than 100 kinds of medicine and health care, including 43 kinds of sulfur-containing volatiles, 13 kinds of sulfinic acid (such as allicin) esters, 9 kinds of amino acids, 8 kinds of peptides, and glycosides. 12 kinds, 11 kinds of enzymes. Its extensive health benefits are attributed to sulfur-containing compounds, such as alliin, allicin, diallyl disulfide (DADS), S-allyl. L-cysteine ​​(SAC) and several reserve diamines are involved in the protective mechanism of garlic against cardiovascular disease and cancer, which can effectively reduce the risk of cardiovascular and cancer. Among them, alliin is a unique component of garlic. It mainly exists in the cells of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/48C07C315/06
CPCC07C315/06C07C317/48
Inventor 任鹏飞
Owner 青岛博恩高科生物技术有限公司
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