CN103483196B - Method for extracting oleocanthal from olive oil - Google Patents

Method for extracting oleocanthal from olive oil Download PDF

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Publication number
CN103483196B
CN103483196B CN201310461991.9A CN201310461991A CN103483196B CN 103483196 B CN103483196 B CN 103483196B CN 201310461991 A CN201310461991 A CN 201310461991A CN 103483196 B CN103483196 B CN 103483196B
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extraction
extracting
spraying dry
time
extraction agent
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CN103483196A (en
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文继承
蒋元勇
朱昂辉
易华
李丽金
雍小军
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SANYUAN JINRUI NATURAL INGREDIENTS Co.,Ltd.
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GUILIN MINGXING BIOTECHNOLOGY Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/48Separation; Purification; Stabilisation; Use of additives
    • C07C67/56Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/48Separation; Purification; Stabilisation; Use of additives

Abstract

The invention discloses a method for extracting oleocanthal from olive oil. The method comprises the steps as follows: water is added to the olive oil and modified starch for mixing, and then the mixture is subjected to spray drying; subcritical extraction is performed twice with a fluid formed by propane and dimethyl ether in a weight ratio of (40-60):(40-60) serving as an extracting agent; the subcritical extraction is performed again with absolute ethyl alcohol serving as an extracting agent; and spray drying is performed after an extraction liquid is concentrated,, so that a finished product is prepared. According to the method, the extraction process is simple, the usage amount of an organic solvent is small, the residual quantity is low, the final product yield is about 2%, the content can reach 30%-40%, and the oleocanthal with higher quality is effectively obtained from the olive oil which is difficult to extract.

Description

A kind of method extracting olive stimulation aldehyde from sweet oil
Technical field
The present invention relates to a kind of preparation method of extract, specifically a kind of method extracting olive stimulation aldehyde from sweet oil.
Background technology
Sweet oil is the one of vegetables oil, is squeezed into by Oleaceae Fructus oleae europaeae fruit, is conventional edible oil, also can in order to make makeup, medicine and oil lamp fuel etc.Sweet oil is rich in abundant monounsaturated fatty acids, i.e. oleic acid and linolic acid, linolenic acid, also has vitamin A, vitamins B, vitamins D, vitamin-E, vitamin K and polyphenoils etc., is considered to be best suited for one of edible grease of human body.
Olive stimulates aldehyde, or is called that sweet oil stimulates aldehyde, English Oleocanthal by name, and its structural formula is as follows:
Research finds, often edible sweet oil contributes to the risk that senile dementia (Alzheimer's disease, AD) is suffered from reduction.Nearest research shows especially, and the olive contained in sweet oil stimulates aldehyde, and can disturb the formation of characteristic neurological unit fiber knot and the amyloid-beta causing senile dementia, be the key that sweet oil reduces senile dementia morbidity.But olive stimulates the content of aldehyde in sweet oil lower, the olive how extracting higher yields and quality from sweet oil stimulates aldehyde, becomes preparation and the extensive key using olive to stimulate aldehyde.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method extracting olive stimulation aldehyde from sweet oil, adopts easy rational technique, and the olive obtaining higher yields and quality stimulates aldehyde extract.
In order to solve the problems of the technologies described above, the present invention by the following technical solutions:
A kind of method extracting olive stimulation aldehyde from sweet oil, first by spraying dry after sweet oil and modified starch water adding mixing, then the fluid formed by the weight ratio of 40 ~ 60:40 ~ 60 with propane and dme is extraction agent sub critical extraction twice, be extraction agent sub critical extraction again again with dehydrated alcohol, after after dehydrated alcohol extraction, gained extracting solution concentrates, spraying dry obtains finished product.
Wherein, the process of described mixing is: by sweet oil and modified starch by the weight ratio of 1:0.8 ~ 1.1, add water after being stirred to 12 ~ 15 Baumes and carry out spraying dry.
Wherein, with propane and dme for extraction agent carry out sub critical extraction time, extraction agent injection rate is 1 ~ 2 times of gained particle weight after first time spraying dry, and Extracting temperature is 48 ~ 52 DEG C, and extraction pressure is 2.4 ~ 2.8MPa, and extraction time is 30 ~ 50min; Preferably, the weight ratio of propane and dme is 50:50, and extraction agent injection rate is 1 ~ 2 times of gained particle weight after first time spraying dry, and Extracting temperature is 50 DEG C, and extraction pressure is 2.6MPa, and extraction time is 40min.
Wherein, take dehydrated alcohol as extraction agent when carrying out sub critical extraction, Extracting temperature is 58 ~ 62 DEG C, and extraction pressure is 3.3 ~ 3.7MPa, and extraction time is 20 ~ 40min; Preferably, Extracting temperature is 60 DEG C, and extraction pressure is 3.5MPa, and extraction time is 30min.
Wherein, described concentrating is, under the condition of 58 ~ 62 DEG C, extracting solution is concentrated into 12 ~ 15 Baumes.
Wherein, twice spray-dired processing condition is: charging flow velocity 35 ~ 45 ls/h, inlet temperature 180 ~ 200 DEG C, air outlet temperature 80 ~ 100 DEG C.
Wherein, described modified starch is used for inclusion sweet oil, the T809 modified starch that modified starch can select Qingdao Rui Jie food chemistry company limited to produce.
Beneficial effect of the present invention is:
Extracting method technique of the present invention is simple, organic solvent usage quantity is few, residual quantity is low, and the yield of the finished product is about 2%, and content can reach 30% ~ 40%, yield and content high, effectively obtain from the sweet oil not easily carrying out extracting higher quality olive stimulate aldehyde.
Embodiment
Be further described with embodiment below, but the present invention is not limited to these embodiments.
Embodiment 1
From sweet oil, extract olive stimulate aldehyde, step is as follows:
1) by sweet oil and modified starch (the T809 modified starch that the Qingdao Rui Jie food chemistry company limited produces) weight ratio by 1:1, add water after being stirred to 13 Baumes and carry out spraying dry, charging flow velocity during spraying dry is 40 ls/h, inlet temperature is 190 DEG C, and air outlet temperature is 90 DEG C;
2) fluid of the weight ratio composition of 50:50 is pressed with propane and dme for extraction agent, the particle obtained spraying dry carries out the identical sub critical extraction of twice processing condition, extraction agent injection rate is 1.5 times of particle weight, Extracting temperature is 50 DEG C, extraction pressure is 2.6MPa, and extraction time is 40min;
3) be that extraction agent carries out sub critical extraction again with dehydrated alcohol, Extracting temperature is 60 DEG C, extraction pressure is 3.5MPa, extraction time is 30min, extracting solution is concentrated into 13 Baumes under the condition of 60 DEG C, and then spraying dry obtains finished product, and charging flow velocity during spraying dry is 40 ls/h, inlet temperature is 190 DEG C, and air outlet temperature is 90 DEG C.
The product yield of obtained finished product is 2.2%, and olive stimulates the weight content of aldehyde to be 40%.
Embodiment 2
From sweet oil, extract olive stimulate aldehyde, step is as follows:
1) by sweet oil and modified starch (the T809 modified starch that the Qingdao Rui Jie food chemistry company limited produces) weight ratio by 1:0.8, add water after being stirred to 14 Baumes and carry out spraying dry, charging flow velocity during spraying dry is 45 ls/h, inlet temperature is 180 DEG C, and air outlet temperature is 90 DEG C;
2) fluid of the weight ratio composition of 60:40 is pressed with propane and dme for extraction agent, the particle obtained spraying dry carries out the identical sub critical extraction of twice processing condition, extraction agent injection rate is 1.5 times of particle weight, Extracting temperature is 52 DEG C, extraction pressure is 2.4MPa, and extraction time is 40min;
3) be that extraction agent carries out sub critical extraction again with dehydrated alcohol, Extracting temperature is 62 DEG C, extraction pressure is 3.3MPa, extraction time is 30min, extracting solution is concentrated into 12 Baumes under the condition of 62 DEG C, and then spraying dry obtains finished product, and charging flow velocity during spraying dry is 40 ls/h, inlet temperature is 200 DEG C, and air outlet temperature is 80 DEG C.
The product yield of obtained finished product is 2.1%, and olive stimulates the weight content of aldehyde to be 35.4%.
Embodiment 3
From sweet oil, extract olive stimulate aldehyde, step is as follows:
1) by sweet oil and modified starch (the T809 modified starch that the Qingdao Rui Jie food chemistry company limited produces) weight ratio by 1:1, add water after being stirred to 15 Baumes and carry out spraying dry, charging flow velocity during spraying dry is 35 ls/h, inlet temperature is 190 DEG C, and air outlet temperature is 9100 DEG C;
2) fluid of the weight ratio composition of 40:50 is pressed with propane and dme for extraction agent, the particle obtained spraying dry carries out the identical sub critical extraction of twice processing condition, extraction agent injection rate is 2 times of particle weight, Extracting temperature is 48 DEG C, extraction pressure is 2.6MPa, and extraction time is 50min;
3) be that extraction agent carries out sub critical extraction again with dehydrated alcohol, Extracting temperature is 58 DEG C, extraction pressure is 3.5MPa, extraction time is 40min, extracting solution is concentrated into 13 Baumes under the condition of 58 DEG C, and then spraying dry obtains finished product, and charging flow velocity during spraying dry is 45 ls/h, inlet temperature is 180 DEG C, and air outlet temperature is 90 DEG C.
The product yield of obtained finished product is 1.9%, and olive stimulates the weight content of aldehyde to be 30.8%.
Embodiment 4
From sweet oil, extract olive stimulate aldehyde, step is as follows:
1) by sweet oil and modified starch (the T809 modified starch that the Qingdao Rui Jie food chemistry company limited produces) weight ratio by 1:1.1, add water after being stirred to 12 Baumes and carry out spraying dry, charging flow velocity during spraying dry is 40 ls/h, inlet temperature is 200 DEG C, and air outlet temperature is 80 DEG C;
2) fluid of the weight ratio composition of 50:60 is pressed with propane and dme for extraction agent, the particle obtained spraying dry carries out the identical sub critical extraction of twice processing condition, extraction agent injection rate is 1 times of particle weight, Extracting temperature is 50 DEG C, extraction pressure is 2.8MPa, and extraction time is 30min;
3) be that extraction agent carries out sub critical extraction again with dehydrated alcohol, Extracting temperature is 60 DEG C, extraction pressure is 3.7MPa, extraction time is 20min, extracting solution is concentrated into 15 Baumes under the condition of 60 DEG C, and then spraying dry obtains finished product, and charging flow velocity during spraying dry is 35 ls/h, inlet temperature is 190 DEG C, and air outlet temperature is 100 DEG C.
The product yield of obtained finished product is 1.8%, and olive stimulates the weight content of aldehyde to be 36%.

Claims (8)

1. one kind is extracted the method that olive stimulates aldehyde from sweet oil, it is characterized in that: first by spraying dry after sweet oil and modified starch water adding mixing, then the fluid formed by the weight ratio of 40 ~ 60:40 ~ 60 with propane and dme is extraction agent sub critical extraction twice, be extraction agent sub critical extraction again again with dehydrated alcohol, after after dehydrated alcohol extraction, gained extracting solution concentrates, spraying dry obtains finished product.
2. method according to claim 1, is characterized in that, described mixing process is: by sweet oil and modified starch by the weight ratio of 1:0.8 ~ 1.1, add water after being stirred to 12 ~ 15 Baumes and carry out spraying dry.
3. method according to claim 1, it is characterized in that: with propane and dme for extraction agent carry out sub critical extraction time, extraction agent injection rate is 1 ~ 2 times of gained particle weight after first time spraying dry, Extracting temperature is 48 ~ 52 DEG C, extraction pressure is 2.4 ~ 2.8MPa, and extraction time is 30 ~ 50min.
4. method according to claim 1, is characterized in that: take dehydrated alcohol as extraction agent when carrying out sub critical extraction, Extracting temperature is 58 ~ 62 DEG C, and extraction pressure is 3.3 ~ 3.7MPa, and extraction time is 20 ~ 40min.
5. method according to claim 1, is characterized in that: described concentrating is, under the condition of 58 ~ 62 DEG C, extracting solution is concentrated into 12 ~ 15 Baumes.
6. method according to claim 1, is characterized in that, twice spray-dired condition is: charging flow velocity 35 ~ 45 ls/h, inlet temperature 180 ~ 200 DEG C, air outlet temperature 80 ~ 100 DEG C.
7. method according to claim 1, it is characterized in that: with propane and dme for extraction agent carry out sub critical extraction time, the weight ratio of described propane and dme is 50:50, extraction agent injection rate is 1 ~ 2 times of gained particle weight after first time spraying dry, Extracting temperature is 50 DEG C, extraction pressure is 2.6MPa, and extraction time is 40min.
8. method according to claim 1, is characterized in that: take dehydrated alcohol as extraction agent when carrying out sub critical extraction, Extracting temperature is 60 DEG C, and extraction pressure is 3.5MPa, and extraction time is 30min.
CN201310461991.9A 2013-09-30 2013-09-30 Method for extracting oleocanthal from olive oil Active CN103483196B (en)

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Publication number Priority date Publication date Assignee Title
CN111440064A (en) * 2020-05-13 2020-07-24 中国林业科学研究院林产化学工业研究所 Enrichment, purification and preparation method of oleocanthal in extra virgin olive oil
WO2024023550A1 (en) * 2022-07-27 2024-02-01 Gorgio International Holding Llc Malt supplement containing oleocanthal

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FR2904312B1 (en) * 2006-07-31 2010-10-22 Girex PROCESS FOR EXTRACTING OLEOCANTHAL FROM OLIVE OIL
CN101905091B (en) * 2010-07-12 2012-05-30 新疆大学 Equipment and method for extracting biologically active ingredients from subcritical fluid

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Address after: 713800 Qinghe Industrial Park, Sanyuan County, Xianyang City, Shaanxi Province

Patentee after: SANYUAN JINRUI NATURAL INGREDIENTS Co.,Ltd.

Address before: 541300 Yingbin Road, Xingan County, Guilin, the Guangxi Zhuang Autonomous Region (Guilin Canal chemical plant warehouse)

Patentee before: GUILIN APLANAT BOTANICAL RESOURCES CO.,LTD.