CN1488289A - Process for separating zanthookylum bungeanum ingredient using supercritical fluid technology - Google Patents

Process for separating zanthookylum bungeanum ingredient using supercritical fluid technology Download PDF

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Publication number
CN1488289A
CN1488289A CNA031323413A CN03132341A CN1488289A CN 1488289 A CN1488289 A CN 1488289A CN A031323413 A CNA031323413 A CN A031323413A CN 03132341 A CN03132341 A CN 03132341A CN 1488289 A CN1488289 A CN 1488289A
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China
Prior art keywords
extraction
spicy component
prickly ash
chinese prickly
separate
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Granted
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CNA031323413A
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Chinese (zh)
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CN1220450C (en
Inventor
孙晓明
金敬宏
张卫明
吴素玲
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Zhongjing Food Co ltd
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NANJING INSTITUTE FOR COMPREHENSIVE UTILIZATION OF WILD PLANT CHINA CO-OP
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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  • Extraction Or Liquid Replacement (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses a technique to use supercritical fluid technology to separate Zantho- xylum bungeanum's tingling-taste component. It crushes Zantho- xylum bungeanum's peel into powder, places in supercritical extraction pot and adds carrier, alcohol, to extract the component; and adjusts the separation pot to control parameters, to separate the component. It adopts CO2 as extraction solvent, has not pollution and can be used as raw material of food and drug.

Description

Utilize supercritical fluid technique to separate the technology of Chinese prickly ash spicy component
Technical field
The present invention relates to a kind of technology of separating the Chinese prickly ash spicy component, particularly relate to a kind of technology of utilizing supercritical fluid technique to separate the Chinese prickly ash spicy component.
Background technology
Chinese prickly ash is the distinctive a kind of spice kind of China, in China long use history is arranged, and is one of spice kind of often using in people's daily life, is a kind of traditional flavoring kind.Chinese prickly ash is a spicy flavor kind unique in the common flavoring, and the alcohol fiber crops are good to eat, are a kind of splendid flavorings.But except China and minority Asian countries are accustomed to this flavoring, external most countries is not approved this spicy flavor, and this has just hindered Chinese prickly ash and has added the international market.Meanwhile, the spicy composition of Chinese prickly ash also is a kind of pharmaceutical raw material, have anesthesia, excitement, antibacterial, dispel rheumatism, effect such as desinsection and analgesia, be a kind of traditional Chinese medicine.Secondly the spicy component of Chinese prickly ash is separated, at first be can be used as medicine material, can be used for composite other fiber crops flavor compound seasoner, can also remove the fiber crops flavor of Chinese prickly ash, promote that Chinese prickly ash moves towards the international market.
The spicy component of Chinese prickly ash mainly is some amide-type compositions such as sanshool, sanshool etc. and skimmianine, green pepper alkali etc., all is some water-soluble chemical materials, is rich in the pericarp of Chinese prickly ash.The Chinese prickly ash spicy component does not also have corresponding industrialized producing technology at present.Some research adopts chemical solvent to carry out extract and separate, and there is dissolvent residual in complex process, is unfavorable for Chinese prickly ash is fully utilized.
Summary of the invention
The purpose of this invention is to provide a kind of technology of utilizing supercritical fluid technique to separate the Chinese prickly ash spicy component.
Purpose of the present invention can realize by following measures:
A kind of technology of utilizing supercritical fluid technique to separate the Chinese prickly ash spicy component comprises the following step:
A. pulverize: get the Chinese prickly ash pericarp and pulverize, sieve, choose 60~80 purpose Pricklyash peels;
B. the extract and separate of oleoresin: Pricklyash peel is added in the supercritical extract jar, adjust extractant flow velocity to extracting pressure and be under the condition of 40~60 ℃ of 30~35Mpa, extraction temperature and extract, the time is 1~3 hour; The pressure of adjusting knockout drum is that 5~8Mpa, temperature are 30~45 ℃, and the separated and collected extract gets xanthoxylum oleoresin, and xanthoxylum oleoresin is done him in addition and used;
C. add entrainer: after xanthoxylum oleoresin separates fully, add entrainer ethanol in the extractor, concentration is 70~95%, and addition is 1~4% of a Pricklyash peel weight;
D. the extraction of spicy component: balance is 0.5~2 hour under the condition of 40~60 ℃ of extracting pressure 28~35Mpa, extraction temperature, carries out the extraction of spicy component;
E. the separation of spicy component: after spicy component extraction balance is finished, adjust the extractant flow velocity, control knockout drum pressure is that 5~7Mpa, temperature are 30~40 ℃, proceeds extraction separation process 1~3 hour, then the spicy component that obtains in the knockout drum is separated.
Purpose of the present invention can also realize by following measures:
Utilize supercritical fluid technique to separate the CO that extractant in the technology of Chinese prickly ash spicy component is 99.5~99.9% food grade for concentration 2
Utilize supercritical fluid technique to separate extractant CO in the technology of Chinese prickly ash spicy component 2Flow velocity be 100~300kg/h.
Advantage of the present invention:
The present invention adopts the carbon dioxide supercritical extraction isolation technics that the spicy component in the Chinese prickly ash pericarp is separated, by in CO 2 fluid, adding an amount of entrainer, change the polarity of supercritical fluid, thereby spicy component is dissolved in the fluid, it is separated.The carbon dioxide that this process using is nontoxic, cheap, be easy to get is as extractant, easy and simple to handle, product is pure, the yield height, the extraction that can carry out xanthoxylum oleoresin simultaneously separates, and product does not have dissolvent residual, final product is not polluted, carbon dioxide can recycle, and equipment operating cost is lower, is suitable for carrying out suitability for industrialized production.Adopt the product quality height of the present invention's preparation, can be used as the raw material of food, medicine.
The specific embodiment
The invention will be further described by the following examples.
Embodiment 1:
Get the Chinese prickly ash pericarp and pulverize, sieve, choose 60 purpose Pricklyash peels; Pricklyash peel is added in the supercritical extract jar (the overcritical equipment in Huaan, Jiangsu Co., Ltd, HA-9548 type) CO of food grade with 99.9% 2Make extractant, control CO 2Flow velocity is 300kg/h to extracting pressure is that 35Mpa, extraction temperature are to extract under 40 ℃ the condition, and the time is 3 hours; The pressure of knockout drum is that 5Mpa, temperature are 45 ℃, and the separated and collected extract gets xanthoxylum oleoresin, CO 2After the high-pressure pump pressurization, recycle; After xanthoxylum oleoresin separates fully, add entrainer ethanol, concentration is 80%, addition is 4% of a Pricklyash peel weight; Balance is 1 hour under the condition of 50 ℃ of extracting pressure 30Mpa, extraction temperature, carries out the extraction of spicy component; After spicy component extraction balance is finished, adjust CO 2The control parameter is that 5Mpa, temperature are 30 ℃ for knockout drum pressure, proceeds extraction separation process 2 hours, then the spicy component that obtains in the knockout drum is separated CO 2After the high-pressure pump pressurization, recycle.
Embodiment 2:
Get the Chinese prickly ash pericarp and pulverize, sieve, choose 80 purpose Pricklyash peels; Pricklyash peel is added in the supercritical extract jar (the overcritical equipment in Huaan, Jiangsu Co., Ltd, HA-9548 type) CO of food grade with 99.5% 2Make extractant, control CO 2Flow velocity is 100kg/h to extracting pressure is that 30Mpa, extraction temperature are to extract under 60 ℃ the condition, and the time is 1 hour; The pressure of knockout drum is that 5Mpa, temperature are 45 ℃, and the separated and collected extract gets xanthoxylum oleoresin, CO 2After the high-pressure pump pressurization, recycle; After xanthoxylum oleoresin separates fully, add entrainer ethanol, concentration is 80%, addition is 1% of a Pricklyash peel weight; Balance is 2 hours under the condition of 50 ℃ of extracting pressure 30Mpa, extraction temperature, carries out the extraction of spicy component; After spicy component extraction balance is finished, adjust CO 2The control parameter is that 7Mpa, temperature are 40 ℃ for knockout drum pressure, proceeds extraction separation process 3 hours, then the spicy component that obtains in the knockout drum is separated CO 2After the high-pressure pump pressurization, recycle.

Claims (3)

1, a kind of technology of utilizing supercritical fluid technique to separate the Chinese prickly ash spicy component is characterized in that comprising the following step:
A. pulverize: get the Chinese prickly ash pericarp and pulverize, sieve, choose 60~80 purpose Pricklyash peels;
B. the extract and separate of oleoresin: Pricklyash peel is added in the supercritical extract jar, adjust extractant flow velocity to extracting pressure and be under the condition of 40~60 ℃ of 30~35Mpa, extraction temperature and extract, the time is 1~3 hour; The pressure of adjusting knockout drum is that 5~8Mpa, temperature are 30~45 ℃, and the separated and collected extract gets xanthoxylum oleoresin, and xanthoxylum oleoresin is done him in addition and used;
C. add entrainer: after xanthoxylum oleoresin separates fully, add entrainer ethanol in the extractor, concentration is 70~95%, and addition is 1~4% of a Pricklyash peel weight;
D. the extraction of spicy component: balance is 0.5~2 hour under the condition of 40~60 ℃ of extracting pressure 28~35Mpa, extraction temperature, carries out the extraction of spicy component;
E. the separation of spicy component: after spicy component extraction balance is finished, adjust the extractant flow velocity, control knockout drum pressure is that 5~7Mpa, temperature are 30~40 ℃, proceeds extraction separation process 1~3 hour, then the spicy component that obtains in the knockout drum is separated.
2, the technology of utilizing supercritical fluid technique to separate the Chinese prickly ash spicy component according to claim 1 is characterized in that used extractant is that concentration is the CO of 99.5~99.9% food grade 2
3, the technology of utilizing supercritical fluid technique to separate the Chinese prickly ash spicy component according to claim 1 is characterized in that used extractant CO 2Flow velocity be 100~300kg/h.
CNB031323413A 2003-08-15 2003-08-15 Process for separating zanthookylum bungeanum ingredient using supercritical fluid technology Expired - Lifetime CN1220450C (en)

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CN1220450C CN1220450C (en) 2005-09-28

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Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101946886A (en) * 2010-08-12 2011-01-19 天津市双星香精香料有限公司 Method for preparing cooked pepper resin
CN102077969A (en) * 2009-11-26 2011-06-01 天津市春升清真食品有限公司 Numb-taste component of zanthoxylum
CN102077971A (en) * 2009-11-26 2011-06-01 天津市春升清真食品有限公司 Cooked fragrant pepper essential oil
CN102077970A (en) * 2009-11-26 2011-06-01 天津市春升清真食品有限公司 Method for preparing sanshoamides
CN102653705A (en) * 2012-04-16 2012-09-05 深圳波顿香料有限公司 Method for extracting essential oil and natural flavor 2-hendecanone from zanthoxylum bungeanum maxim fruit
CN104026538A (en) * 2014-05-19 2014-09-10 郑州雪麦龙食品香料有限公司 Preparing method for high-purity sanshoamides
CN106390514A (en) * 2016-12-01 2017-02-15 四川蓬溪建兴青花椒开发有限公司 Extraction method of green prickleyash fagaramide
CN106433986A (en) * 2016-10-12 2017-02-22 广东聿津食品有限公司 Chinese prickly ash essential oil and preparation method thereof
CN106753804A (en) * 2017-01-16 2017-05-31 峨眉山万佛绿色食品有限公司 Rattan green pepper extraction of essential oil technique
CN107418720A (en) * 2016-05-23 2017-12-01 贵州玄德生物科技股份有限公司 Supercritical CO2The technique for extracting Zanthoxylum essential oil
CN107488514A (en) * 2017-09-27 2017-12-19 四川帅青花椒开发有限公司 A kind of supercritical CO2Extract pericarpium zanthoxyli schinifolii resin process
CN108559631A (en) * 2018-01-25 2018-09-21 陈世湘 A kind of method of efficient extraction Chinese prickly ash flavor substance
CN109832597A (en) * 2019-03-25 2019-06-04 郑州雪麦龙食品香料有限公司 A kind of extraction process improving the numb-taste component of zanthoxylum rate of recovery
CN110236167A (en) * 2019-07-17 2019-09-17 四川省雅士科技有限公司 A kind of salt and pepper seasoning and preparation method thereof with strong numb taste
CN111205923A (en) * 2020-01-13 2020-05-29 四川嘉威德农业科技有限公司 Processing technology of pure zanthoxylum oil rich in linolenic acid
CN113073026A (en) * 2021-03-03 2021-07-06 汉源县昊业花椒产业研究院 Prickly ash compound wine and preparation process thereof
CN113170874A (en) * 2021-05-31 2021-07-27 四川省雅士科技有限公司 Preparation method of novel compound seasoning
CN113367312A (en) * 2021-06-29 2021-09-10 陇南利和萃取科技有限公司 Multifunctional pepper composite seasoning base material and preparation method thereof
CN113563975A (en) * 2021-07-09 2021-10-29 四川丁点儿食品开发股份有限公司 Fresh pepper oleoresin separation and purification process
CN115119931A (en) * 2022-07-12 2022-09-30 云南汉木森生物科技有限责任公司 Production method for producing four pepper products

Cited By (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102077969A (en) * 2009-11-26 2011-06-01 天津市春升清真食品有限公司 Numb-taste component of zanthoxylum
CN102077971A (en) * 2009-11-26 2011-06-01 天津市春升清真食品有限公司 Cooked fragrant pepper essential oil
CN102077970A (en) * 2009-11-26 2011-06-01 天津市春升清真食品有限公司 Method for preparing sanshoamides
CN101946886A (en) * 2010-08-12 2011-01-19 天津市双星香精香料有限公司 Method for preparing cooked pepper resin
CN102653705A (en) * 2012-04-16 2012-09-05 深圳波顿香料有限公司 Method for extracting essential oil and natural flavor 2-hendecanone from zanthoxylum bungeanum maxim fruit
CN102653705B (en) * 2012-04-16 2013-12-11 深圳波顿香料有限公司 Method for extracting essential oil and natural flavor 2-hendecanone from zanthoxylum bungeanum maxim fruit
CN104026538A (en) * 2014-05-19 2014-09-10 郑州雪麦龙食品香料有限公司 Preparing method for high-purity sanshoamides
CN104026538B (en) * 2014-05-19 2016-02-24 郑州雪麦龙食品香料有限公司 A kind of preparation method of high-purity numb-taste component of zanthoxylum
CN107418720A (en) * 2016-05-23 2017-12-01 贵州玄德生物科技股份有限公司 Supercritical CO2The technique for extracting Zanthoxylum essential oil
CN106433986A (en) * 2016-10-12 2017-02-22 广东聿津食品有限公司 Chinese prickly ash essential oil and preparation method thereof
CN106390514A (en) * 2016-12-01 2017-02-15 四川蓬溪建兴青花椒开发有限公司 Extraction method of green prickleyash fagaramide
CN106753804A (en) * 2017-01-16 2017-05-31 峨眉山万佛绿色食品有限公司 Rattan green pepper extraction of essential oil technique
CN107488514A (en) * 2017-09-27 2017-12-19 四川帅青花椒开发有限公司 A kind of supercritical CO2Extract pericarpium zanthoxyli schinifolii resin process
CN107488514B (en) * 2017-09-27 2021-03-30 四川帅青花椒开发有限公司 Supercritical CO2Process for extracting green pepper resin
CN108559631A (en) * 2018-01-25 2018-09-21 陈世湘 A kind of method of efficient extraction Chinese prickly ash flavor substance
CN109832597A (en) * 2019-03-25 2019-06-04 郑州雪麦龙食品香料有限公司 A kind of extraction process improving the numb-taste component of zanthoxylum rate of recovery
CN110236167A (en) * 2019-07-17 2019-09-17 四川省雅士科技有限公司 A kind of salt and pepper seasoning and preparation method thereof with strong numb taste
CN111205923A (en) * 2020-01-13 2020-05-29 四川嘉威德农业科技有限公司 Processing technology of pure zanthoxylum oil rich in linolenic acid
CN113073026A (en) * 2021-03-03 2021-07-06 汉源县昊业花椒产业研究院 Prickly ash compound wine and preparation process thereof
CN113170874A (en) * 2021-05-31 2021-07-27 四川省雅士科技有限公司 Preparation method of novel compound seasoning
CN113367312A (en) * 2021-06-29 2021-09-10 陇南利和萃取科技有限公司 Multifunctional pepper composite seasoning base material and preparation method thereof
CN113563975A (en) * 2021-07-09 2021-10-29 四川丁点儿食品开发股份有限公司 Fresh pepper oleoresin separation and purification process
CN115119931A (en) * 2022-07-12 2022-09-30 云南汉木森生物科技有限责任公司 Production method for producing four pepper products
CN115119931B (en) * 2022-07-12 2023-10-03 云南汉木森生物科技有限责任公司 Production method for producing four pricklyash peel products

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Application publication date: 20040414

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