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CN1266226C - Process for separating capsorubin and capsaicine from hot pepper - Google Patents

Process for separating capsorubin and capsaicine from hot pepper Download PDF

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Publication number
CN1266226C
CN1266226C CNB2004100540078A CN200410054007A CN1266226C CN 1266226 C CN1266226 C CN 1266226C CN B2004100540078 A CNB2004100540078 A CN B2004100540078A CN 200410054007 A CN200410054007 A CN 200410054007A CN 1266226 C CN1266226 C CN 1266226C
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capsaicin
extraction
capsanthin
separator
capsicum
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Expired - Fee Related
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CNB2004100540078A
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CN1587321A (en
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于文利
赵亚平
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Shanghai Jiao Tong University
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Shanghai Jiao Tong University
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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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  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

本发明涉及一种从辣椒中分离辣椒红素和辣椒碱的方法,首先用高浓度乙醇把辣椒红素与辣椒碱从原料粉中全部萃取出来,经减压蒸馏浓缩,得到含辣椒红素与辣椒碱的油状物粗产品,然后使用超临界流体萃取技术纯化粗品,根据辣椒红素和辣椒碱在CO2中的溶解度不同的原理,进行萃取分离,同时得到高纯度、高收率、无溶剂残留、无异味的辣椒红素和辣椒碱。本发明工艺流程简单、经济、可操作性强,适于工业化生产,得到的辣椒红素可用于食品色素、化妆品、保健食品,辣椒碱可直接入药。The invention relates to a method for separating capsanthin and capsaicin from capsicum. First, all capsanthin and capsaicin are extracted from raw material powder with high-concentration ethanol, and concentrated by vacuum distillation to obtain capsanthin and capsaicin. The oily crude product of capsaicin is then purified by supercritical fluid extraction technology. According to the principle of different solubility of capsaicin and capsaicin in CO2 , the extraction and separation are carried out to obtain high-purity, high-yield, solvent-free Residual, odor-free capsanthin and capsaicin. The process of the invention is simple, economical and operable, and is suitable for industrial production. The obtained capsanthin can be used in food pigments, cosmetics and health foods, and the capsaicin can be directly used as medicine.

Description

The method of separating pepper red pigment and capsicine from capsicum
Technical field
The present invention relates to a kind of from capsicum the method for separating pepper red pigment and capsicine, with solvent extraction and supercritical CO 2Abstraction technique combines, and extracts simultaneously, refining obtains Capsorubin and two kinds of products of capsicine, belongs to chemical engineering subject Separation of Natural Products field.
Background technology
Capsorubin and capsicine are two kinds and are present in noticeable composition in the capsicum that the former is good natural edible red pigment, has been widely used in fields such as food, high-grade feed; The latter is a kind of medicinal ingredients, and post-herpetic neuralgia, trigeminal neuralgia, diabetes nerve pain, rheumatic arthritis, osteoarthritis, psoriasis, baldness etc. are had significant curative effect.From red pepper, obtain this two kinds of materials, more generally adopt organic solvent extraction at present, comprise two kinds of technologies: one, only extract pigment, or only carry capsicine, do not consider to reclaim simultaneously another kind of composition, unreasonable on this process economics, can not be applied industrial; They are two years old, extract simultaneously and separate pigment and capsicine, a kind of " extracting the novel process of capsanthin and capsaicine in red pepper " disclosed as Chinese invention patent (CN1083083A), with the paprika powder is raw material, obtain containing the extracting solution of Capsorubin and capsaicine (being capsicine) with Petroleum ether extraction, with common salt aqueous solution and industrial acetone extracting solution is saltoutd-extraction treatment, standing demix obtains containing Capsorubin liquid layer and capsicine liquid layer respectively, removes solvent by underpressure distillation again and obtains Capsorubin and capsicine respectively.Though this technology is reasonable economically, products obtained therefrom dissolvent residual height has strange taste, and quality is lower, is difficult to satisfy the requirement of users at home and abroad.
Summary of the invention
The present invention seeks at above-mentioned the deficiencies in the prior art, provide a kind of from capsicum the method for separating pepper red pigment and capsicine, can from capsicum, extract simultaneously, separate and obtain high-quality Capsorubin and capsicine, be used for satisfying the needs that real life food, medicine and healthcare products etc. are produced.
For realizing such purpose, the present invention at first all extracts Capsorubin and capsicine from the raw material of hot pepper powder with high concentration ethanol, concentrate through underpressure distillation, obtain containing the thick product of oily matter of Capsorubin and capsicine, use supercritical liquid extraction technique purifying crude product then, according to Capsorubin and capsicine at CO 2In the principle of different solubility, carry out extracting and separating, obtain high-quality Capsorubin and capsicine product.
Concrete grammar of the present invention is as follows:
(1) organic solvent lixiviate Capsorubin and capsicine: be 95% ethanol lixiviate raw material of hot pepper powder with weight percentage, by raw material powder and alcoholic acid solid-liquid weight ratio is to feed intake at 1: 3, after 50-70 ℃ of following refluxing extraction 1-4 hour, filter, collect filtrate and filter residue, again with filter residue as raw material powder, mix ethanol and repeat said extracted process 2-5 time, then each filtrate is combined, reclaim ethanol by underpressure distillation, obtain being rich in the thick product of oily matter of capsochrome and capsicine.
(2) supercritical CO 2Extracting capsicum alkali: the thick product of above-mentioned oily matter is put in the extraction kettle of overcritical device, with high-pressure pump with CO 2Squeeze into extraction kettle, make it pressure and reach preset value 8~20MPa, temperature is controlled at 35~50 ℃, opens extraction cycle loop " extraction kettle-separator-extraction kettle " then and extracts, by adjusting CO 2Enter the inlet valve aperture of separator, make separator pressure be controlled at 5-7MPa, simultaneous temperature is controlled at 35~50 ℃, after extracting 1~4 hour, collects in extraction kettle and obtains Capsorubin, collects in separator and obtains the capsicine product.
Because capsicine is at supercritical CO 2In solubleness greater than Capsorubin, capsicine is by supercritical CO 2Extract from extraction kettle and enter separator, Capsorubin is then still stayed in the extraction kettle.In separator, because the pressure in the separator is lower, CO2 becomes gaseous phase again again and gets back to and carry out the next round extraction in the extraction loop, and capsicine then precipitates.After so extraction was carried out 1~4 hour, capsicine was all extracted from extraction kettle, and is deposited in the separator.Like this, can in extraction kettle, collect and obtain Capsorubin, in separator, collect and obtain the capsicine product.
The particle diameter of the raw material of hot pepper powder that the present invention adopts is the 60-150 order.
The present invention is carrying out supercritical CO 2During extraction, can be with CO 2Squeeze into extraction kettle earlier by refrigeration liquefying, and then through high-pressure pump.
Technical process of the present invention is simple, economical, workable, is suitable for suitability for industrialized production, and the product that obtains is the Capsorubin and the capsicine of high yield, high purity, no solvent residue, free from extraneous odour.Capsorubin can be used for food color, makeup, protective foods, and capsicine can directly be used as medicine.
Embodiment
Below by specific embodiment technical scheme of the present invention and the effect that reaches thereof are further described.
Embodiment 1:
Take by weighing 60 order dry paprika 100g, the adding weight percentage is 95% ethanol lixiviate, by raw material powder and alcoholic acid solid-liquid weight ratio is to feed intake at 1: 3,50 ℃ of following refluxing extraction 1 hour, afterwards, filter and collect filtrate and filter residue, again with filter residue as raw material powder, by raw material powder and alcoholic acid solid-liquid weight ratio is to mix ethanol at 1: 3 to feed intake again, repeat the said extracted process, obtain secondary filtrate and filter residue, twice filtrate is combined, reclaim ethanol by underpressure distillation, obtain being rich in the thick product of oily matter of capsochrome and capsicine.
The thick product of above-mentioned oily matter is put in the extraction kettle of overcritical device, before extracting, CO 2Squeeze into extraction kettle earlier by refrigeration liquefying, and then through high-pressure pump, make it pressure and reach preset value 8MPa, temperature is controlled at 35 ℃, opens extraction cycle loop " extraction kettle-separator-extraction kettle " then and extracts, and adjusts CO 2Enter the inlet valve aperture of separator, make separator pressure be controlled at 5MPa, simultaneous temperature is controlled at 35 ℃, after so extraction was carried out 1 hour, stop extraction, open the vent valve release, obtain capsicine purity from separator and reach 88%, yield is 35% to obtain the Capsorubin product from extraction kettle, purity reaches 40%, 95%, two kind of equal free from extraneous odour of product of yield, dissolvent residual reaches pharmaceutical grade.
Embodiment 2:
Take by weighing 150 purpose dry paprika 100g, the adding weight percentage is 95% ethanol lixiviate, by raw material powder and alcoholic acid solid-liquid weight ratio is to feed intake at 1: 3,70 ℃ of following refluxing extraction 1 hour, afterwards, filter and collect filtrate and filter residue, with filter residue as raw material powder, mix ethanol and repeat the said extracted process, obtain secondary filtrate and filter residue, repeat the said extracted process by mode like this and amount to 5 times, then the filtrate that obtains for 5 times is combined, reclaim ethanol by underpressure distillation, obtain being rich in the thick product of oily matter of capsochrome and capsicine.
The thick product of above-mentioned oily matter is put in the extraction kettle of overcritical device, before extracting, CO 2Squeeze into extraction kettle earlier by refrigeration liquefying, and then through high-pressure pump, make it pressure and reach preset value 20MPa, temperature is controlled at 50 ℃, opens extraction cycle loop " extraction kettle-separator-extraction kettle " then and extracts, and adjusts CO 2Enter the inlet valve aperture of separator, make separator pressure be controlled at 7MPa, simultaneous temperature is controlled at 50 ℃, after so extraction was carried out 4 hours, stop extraction, open the vent valve release, obtain capsicine purity from separator and reach 45%, yield is 90% to obtain the Capsorubin product from extraction kettle, purity reaches 87%, 35%, two kind of equal free from extraneous odour of product of yield, dissolvent residual reaches pharmaceutical grade.
Embodiment 3:
Take by weighing 100 purpose dry paprika 100g, the adding weight percentage is 95% ethanol lixiviate, by raw material powder and alcoholic acid solid-liquid weight ratio is to feed intake at 1: 3,60 ℃ of following refluxing extraction 3 hours, afterwards, filter and collect filtrate and filter residue, again with filter residue as raw material powder, mix ethanol and repeat the said extracted process, obtain secondary filtrate and filter residue, so repeat the said extracted process and amount to 4 times, the filtrate that obtains for 4 times is combined, reclaim ethanol by underpressure distillation, obtain being rich in the thick product of oily matter of capsochrome and capsicine.
The thick product of above-mentioned oily matter is put in the extraction kettle of overcritical device, before extracting, CO 2Squeeze into extraction kettle earlier by refrigeration liquefying, and then through high-pressure pump, make it pressure and reach preset value 15MPa, temperature is controlled at 40 ℃, opens extraction cycle loop " extraction kettle-separator-extraction kettle " then and extracts, and adjusts CO 2Enter the inlet valve aperture of separator, make separator pressure be controlled at 7MPa, simultaneous temperature is controlled at 40 ℃, after so extraction was carried out 3 hours, stop extraction, open the vent valve release, obtain capsicine purity from separator and reach 66%, yield is 70% to obtain the Capsorubin product from extraction kettle, purity reaches 77%, 65%, two kind of equal free from extraneous odour of product of yield, dissolvent residual reaches pharmaceutical grade.

Claims (3)

1、一种从辣椒中分离辣椒红素和辣椒碱的方法,其特征在于包括如下步骤:1, a method for separating capsanthin and capsaicin from capsicum, is characterized in that comprising the steps: 1)有机溶剂浸提辣椒红素和辣椒碱:用重量百分数为95%的乙醇浸提辣椒原料粉,按原料粉与乙醇的固液重量比为1∶3投料,在50-70℃下回流提取1-4小时之后过滤,收集滤液和滤渣,再将滤渣作为原料粉,配上乙醇重复上述提取过程2-5次,然后将每次的滤液合并在一起,通过减压蒸馏回收乙醇,得到富含辣椒色素和辣椒碱的油状物产品;1) Extraction of capsanthin and capsaicin with organic solvents: extract capsicum raw material powder with 95% ethanol by weight, feed the material according to the solid-to-liquid weight ratio of raw material powder and ethanol as 1:3, and reflux at 50-70°C After extracting for 1-4 hours, filter, collect the filtrate and filter residue, then use the filter residue as raw material powder, add ethanol and repeat the above extraction process for 2-5 times, then combine each filtrate together, and recover ethanol by vacuum distillation to obtain Oil products rich in capsaicin and capsaicin; 2)超临界CO2萃取辣椒碱:把上述油状物产品放入超临界装置中的萃取釜里,用高压泵将CO2打入萃取釜,使之压力达到预设值8~20MPa,温度控制在35~50℃,然后打开萃取循环回路“萃取釜—分离器—萃取釜”进行萃取,通过调整CO2进入分离器的入口阀门开度,使分离器压力控制在5-7MPa,同时温度控制在35~50℃,萃取1~4小时之后,在萃取釜中收集得到辣椒红素,在分离器中收集得到辣椒碱产品。2) Supercritical CO2 extraction of capsaicin: Put the above oily product into the extraction kettle in the supercritical device, inject CO2 into the extraction kettle with a high-pressure pump, make the pressure reach the preset value of 8-20MPa, and control the temperature At 35 ~ 50 ° C, then open the extraction cycle "extraction kettle-separator-extraction kettle" for extraction, by adjusting the opening of the inlet valve where CO2 enters the separator, the pressure of the separator is controlled at 5-7MPa, and the temperature is controlled at the same time After extraction at 35-50° C. for 1-4 hours, capsanthin is collected in an extraction kettle, and capsaicin product is collected in a separator. 2、如权利要求1的从辣椒中分离辣椒红素和辣椒碱的方法,其特征在于所述辣椒原料粉的粒径为60-150目。2. The method for separating capsaicin and capsaicin from capsicum according to claim 1, characterized in that the particle size of said raw capsicum powder is 60-150 mesh. 3、如权利要求1的从辣椒中分离辣椒红素和辣椒碱的方法,其特征在于超临界CO2萃取时,CO2先通过制冷液化,然后再经高压泵打入萃取釜。3. The method for separating capsaicin and capsaicin from capsicum as claimed in claim 1, characterized in that during supercritical CO2 extraction, CO2 is first liquefied by refrigeration, and then injected into the extraction kettle through a high-pressure pump.
CNB2004100540078A 2004-08-26 2004-08-26 Process for separating capsorubin and capsaicine from hot pepper Expired - Fee Related CN1266226C (en)

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Families Citing this family (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1318391C (en) * 2005-07-08 2007-05-30 上海雷辣婆食品有限公司 Method of extracting capsaicin and capsaithin from red pepper
CN101747660B (en) * 2009-12-22 2013-07-17 晨光生物科技集团股份有限公司 Method for removing noxious substances in natural extract
CN102150820B (en) * 2010-12-14 2013-08-28 中国科学院新疆理化技术研究所 Method for preparing capsorubin and lycopene soft capsules
CN103254092A (en) * 2013-05-19 2013-08-21 常州亚当生物技术有限公司 Production process of capsaicin
CN104529805A (en) * 2014-11-27 2015-04-22 安徽省万顺现代农业科技有限公司 Method for extracting capsicine from capsicum
CN104530748A (en) * 2014-11-27 2015-04-22 安徽省万顺现代农业科技有限公司 Method for extracting capsicum haematochrome from capsicum
CN104535705B (en) * 2014-12-23 2017-01-25 中州大学 Method for synchronously measuring capsaicin and capsorubin in capsicum oleoresin
CN107022202A (en) * 2017-03-31 2017-08-08 浙江汇能生物股份有限公司 A kind of supercritical CO2The technique of capsorubin and capsaicine in continuous extraction capsicum
CN107118121A (en) * 2017-05-31 2017-09-01 江苏师范大学 A kind of method of capsaicine pre-treatment
CN108689873A (en) * 2018-03-27 2018-10-23 佛山市飞程信息技术有限公司 A kind of process for super-critical extracting of capsaicine
CN110108653B (en) * 2019-04-18 2022-12-13 重庆市农业科学院 A method for analyzing the change rule of capsanthin in the pretreatment process of fresh pepper
CN110156627B (en) * 2019-05-27 2021-07-02 山西大学 Method for simultaneous separation of capsanthin and capsaicin by three-phase salting-out extraction
CN113603607A (en) * 2020-12-17 2021-11-05 贵州玄德生物科技股份有限公司 Extraction process and production line of natural capsaicin
CN114159826A (en) * 2021-11-30 2022-03-11 李志军 Supercritical CO of black tea2Extraction method

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