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Organic-solvent-free combined extraction method of thyme essential oil and thyme total flavonoids

An organic solvent and combined extraction technology, which is applied in the direction of essential oils/fragrances, anti-toxic agents, drug combinations, etc., can solve the problems of easy oxidation of thyme essential oil, lower volatility, lower yield, etc., achieve short preparation time and reduce the total amount , the effect of low production cost

Pending Publication Date: 2021-08-27
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at problems such as the easy oxidation of thyme essential oil that exists in the existing steam distillation technology, resulting in yield reduction and quality decline, the purpose of the present invention is to provide a method for mechanochemical extraction of thyme essential oil without organic solvents, which can improve the yield of thyme essential oil in aqueous solution. It has medium solubility and reduces its volatility, so that the essential oil components in thyme can be converted into water-soluble substances. The use of organic solvents is avoided in the preparation and no heating is required, which meets the requirements of low-temperature extraction and environmental protection.

Method used

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  • Organic-solvent-free combined extraction method of thyme essential oil and thyme total flavonoids
  • Organic-solvent-free combined extraction method of thyme essential oil and thyme total flavonoids
  • Organic-solvent-free combined extraction method of thyme essential oil and thyme total flavonoids

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add thyme powder (50.0g) and sodium hydroxide (5g) in the 200mL stainless steel ball mill jar, then add stainless steel ball mill beads as the grinding medium, the diameter of the ball mill beads is 10mm, and the control filling rate is 58% ((ball volume × ball number) / the total volume of the ball milling tank), after mixing evenly, put the ball milling tank into the planetary ball mill, set the rotating speed to 400rpm, and the time is 1.5 hours. After the ball milling, take out the powder, put the powder in a beaker, add 200mL petroleum ether and stir at room temperature After extracting for 5 minutes and filtering, concentrate the filtrate under reduced pressure at 35°C to constant weight, which is thyme essential oil, and accurately record the quality of the oily liquid; Wash the filter cake with 50 mL of deionized water. Combine the filtrates and concentrate to 50mL, slowly add 8.20g of citric acid to completely neutralize and filter, the obtained solid is the tot...

Embodiment 2

[0030]Add thyme powder (50.0g) and sodium carbonate (5g) in the 200mL stainless steel ball mill jar, then add stainless steel ball mill beads as the grinding medium, the diameter of the ball mill beads is 10mm, and the control filling rate is 58% ((ball volume × ball number) / The total volume of the ball milling tank), after mixing evenly, put the ball milling tank into the planetary ball mill, set the rotation speed to 400rpm, and the time is 1.5 hours. After the ball milling, take out the powder, put the powder in a beaker, add 200mL petroleum ether and stir at room temperature to extract After 5 minutes of filtration, concentrate the filtrate under reduced pressure at 40°C to constant weight, which is the thyme essential oil. Accurately record the quality of the oily liquid; after the filter residue is evaporated, add 500mL of deionized water and stir for 5 minutes at room temperature, and filter to obtain a clear filtrate and use Wash the filter cake with 50 mL of deionized...

Embodiment 3

[0032] Add thyme powder (50.0g) and sodium bicarbonate (5g) in the 200mL stainless steel ball mill jar, then add stainless steel ball mill beads as the grinding medium, the diameter of the ball mill beads is 10mm, and the control filling rate is 58% ((ball volume × ball number) / the total volume of the ball milling tank), after mixing evenly, put the ball milling tank into the planetary ball mill, set the rotating speed to 400rpm, and the time is 1.5 hours. After the ball milling, take out the powder, put the powder in a beaker, add 200mL petroleum ether and stir at room temperature After extraction for 5 minutes and filtration, concentrate the filtrate under reduced pressure at 40°C to constant weight, which is the thyme essential oil. Accurately record the quality of the oily liquid; after the filter residue is evaporated, add 500mL deionized water and stir for extraction at room temperature for 5 minutes, and filter to obtain a clear filtrate And wash the filter cake with 50...

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Abstract

The invention discloses an organic-solvent-free combined extraction method of thyme essential oil and thyme total flavonoids. The method comprises the following steps: by taking an overground part of a thyme plant as a raw material, in the presence of an alkaline auxiliary agent, enabling flavone in thyme to react with the alkaline auxiliary agent to form a water-soluble salt through a mechanochemical effect, so as to prevent polysaccharide substances dissolved out of essential oil and a cell wall structure from being damaged at the same time; and respectively obtaining the thyme oil and the thyme total flavonoids with high yield by adopting different polar solvents for extraction. Through the mechanical force effect and the mechanochemical auxiliary effect, cell walls are destroyed to promote dissolution and release of the essential oil, the extraction rate of the essential oil is improved, heating is not needed in the extraction process, so that the loss of the essential oil is greatly reduced, and the preparation method is simple, easy to implement, low in cost, non-toxic, harmless, and obvious in effect. The obtained thyme essential oil can be used as high-quality essential oil and an oral and external antibacterial agent for animals, and thyme flavone is a health-care product with an anti-oxidation effect and has a wide market prospect.

Description

technical field [0001] The invention belongs to the technical field of extraction of plant effective components, and in particular relates to an economical and green method for combined extraction of thyme essential oil and total flavonoids of thyme without organic solvents. Background technique [0002] Thyme essential oil is a volatile liquid extracted from the aerial parts of thyme plants such as Thymus vulgaris L., T.zygis L. and Thymus mongolicus Ronn. Its main components are Thymol (30% to 70%) and carvacrol (2% to 15%), with a total phenolic content ≥ 40%. Thyme essential oil, as a natural source of antibiotic substitute, has good antibacterial properties, is not easy to produce drug resistance and is harmless to human body. The inhibition rate of bacteria was significantly better than that of the antibiotic colistin sulfate. The development of thyme essential oil as a plant-derived antibiotic is beneficial to the greening of the swine industry. However, the active...

Claims

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Application Information

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IPC IPC(8): C11B9/02A61K36/53
CPCC11B9/025A61K36/53A61P31/04A61P39/06A61K2236/15A61K2236/35A61K2236/53
Inventor 贺彦桥唐静施宣任许文灏
Owner ZHEJIANG UNIV OF TECH
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