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Method for extracting and purifying natural flavor valencene and nootkatone from juglans regia

A technology of natural spice and citronella ketone, which is applied in extraction and purification/separation, distillation purification/separation, separation/purification of carbonyl compounds, etc., can solve the problem of low oil yield and poor effect of citronella ketone content in educational fruit. and other problems to achieve high permeability and improve extraction efficiency.

Active Publication Date: 2008-09-03
APPLE FLAVOR & FRAGRANCE GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Citron is a solid crystal with a melting point of 36°C, which means that its vapor pressure is very low under normal pressure, so the effect of steam distillation extraction is not good, and the oil yield and content of Citrus are low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Pulverize 50kg of nutmeg, pass 100% through a 20-mesh sieve, put into a supercritical extraction tank, and carry out supercritical extraction. The conditions for controlling the extraction are: extraction pressure 10MPa, extraction temperature 32°C, flow rate 12L / min, extraction time 3 hours. The separation pressure is 4MPa, and the separation temperature is 30°C. Obtain about 1042g brown-yellow nootropic oil, have strong fragrance, and oil yield is about 2%. The oil contains about 14% valenciene and about 13% narone as determined by gas chromatography. Continuously extracting 10 batches, a total of 10.36kg brown-yellow nootropic oil was obtained.

[0023] Put 10.36kg of above-mentioned puzzle oil into the emulsification kettle, add 41.5Kg of 70% ethanol aqueous solution, at room temperature, stir with homogeneous mixer, rotating speed 3800~4000 rev / min, time 2 hours, then static layering 4 Hour. The upper oil layer contains 22% valenciene by chromatography, and the...

Embodiment 2

[0027] Pulverize 50kg of nutmeg, pass 100% through a 20-mesh sieve, put into a supercritical extraction tank, and carry out supercritical extraction. The conditions for controlling the extraction are: extraction pressure 18MPa, extraction temperature 45°C, flow rate 15L / min, extraction time 3 hours. The separation pressure is 4MPa, and the separation temperature is 30°C. Obtain about 1350g of brown nootropic oil, which has a strong aroma and an oil yield of about 2.7%. The oil contains about 10% of valenciene and about 8.5% of naringone as determined by gas chromatography. Continuous extraction of 10 batches yielded a total of 13.50kg of brown nootropic oil.

[0028] The above-mentioned puzzle oil 13.50kg was added in 5.4 kilograms of 70% methanol aqueous solution, at room temperature, mixed and emulsified with emulsification pump, pressure 4MPa, time 2 hours, then static layering 4 hours. The upper oil layer contains 19% valenciene as determined by chromatography, and the ...

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PUM

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Abstract

A method for extracting and purifying natural perfume that is valencene and nootkatone in the walnut extracts and purifies valencene and nootkatone by the processes of supercritical fluid extraction, dissolvant liquid-liquid extraction, high precision fractionation, preparing chromatography, and recrystallization in turns, comprising: extracting the walnut by fluid under a supercritical state, performing a liquid-liquid extraction using lower alcohol solution through an emulsification pump and a homogenizer, mixing the walnut oil and alcohol solution, emulsifying the solution to achieve a full liquid-liquid contact and extraction, the high precision fractionation using vacuum fractionation, fractionating hydrocarbons component of the walnut oil after liquid-liquid extraction to obtain valencene, using polyporous material as a chromatography fillers, chromatographically separating and recrystallizing a crude product of nootkatone obtained form alcohol solution after liquid-liquid extraction to obtain the purified nootkatone.

Description

technical field [0001] The present invention relates to a production method of natural spices, in particular to a production method of extracting and purifying valenciene and narone from the fruit of natural plant Alpinia oxyphylla Miq. Background technique [0002] Citrus flavor is a kind of flavor widely used in food, beverage and pharmaceutical products, two of which are very important flavoring ingredients are valenciene (chemical name: naphthylcyclene, 1, 2, 3, 5 , 6,7,8,8a-octahydro-1,8a-dimethyl-7-(1-methylvinyl)-[1R-(1α,7β,8aα], CAS No.4630-07-3 ) and narone (chemical name: 2(3H)naphthylcycloenone, 4,4a,5,6,7,8-hexahydro-4,4a,-dimethyl-6-(1-methylethylene Base)-[4R-(4α, 4aα, 6β], CAS No.4674-50-4). Citron gives people a sweet, ripe orange fragrance, which is pleasant; Valenciaene has a Flavoring effect, they are very important spices. But in nature, their content in natural state is extremely low. Some citrus oils contain these two components, the content is 0.02-0...

Claims

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Application Information

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IPC IPC(8): C07C7/04C07C7/10C07C15/58C07C45/78C07C49/796
CPCY02P20/54
Inventor 胡勇成华立明单逢三
Owner APPLE FLAVOR & FRAGRANCE GRP
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