[go: up one dir, main page]

CN1911902A - Extraction technology of capsanthin and capsicine - Google Patents

Extraction technology of capsanthin and capsicine Download PDF

Info

Publication number
CN1911902A
CN1911902A CN 200610040907 CN200610040907A CN1911902A CN 1911902 A CN1911902 A CN 1911902A CN 200610040907 CN200610040907 CN 200610040907 CN 200610040907 A CN200610040907 A CN 200610040907A CN 1911902 A CN1911902 A CN 1911902A
Authority
CN
China
Prior art keywords
capsanthin
capsaicine
mutually
ethanol
phase
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN 200610040907
Other languages
Chinese (zh)
Inventor
乔世伟
沈永林
沈雁青
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SUZHOU HONGSHENG OIL CHEMICAL MACHINERY CO Ltd
Original Assignee
SUZHOU HONGSHENG OIL CHEMICAL MACHINERY CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by SUZHOU HONGSHENG OIL CHEMICAL MACHINERY CO Ltd filed Critical SUZHOU HONGSHENG OIL CHEMICAL MACHINERY CO Ltd
Priority to CN 200610040907 priority Critical patent/CN1911902A/en
Publication of CN1911902A publication Critical patent/CN1911902A/en
Pending legal-status Critical Current

Links

Landscapes

  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The capsanthin and capsaicin extracting process includes the following steps: soaking red chili grain in the mixed solvent of ethanol and n-hexane and filtering to obtain filtrate; stilling the filtrate for delaminating phase A of mixture liquid of n-hexane and capsanthin and phase B of mixture liquid of ethanol and capsaicin; heating the phase A to evaporate n-hexane, purifying left capsanthin with ethanol and introducing CO2, N2 or inert gas except radon gas to obtain purified capsanthin; heating the phase B to evaporate ethanol, mixing the left concentrated capsaicin with acetone solution, heating to separate out acetone and obtain purified capsaicin. The present invention has high purity of prepared capsanthin and capsaicin, wide product applying range, low production cost, great output and convenient operation.

Description

Capsanthin and capsaicine extraction process
Technical field
The present invention relates to a kind of technology of from red pepper, extracting capsanthin and capsaicine.
Background technology
In the prior art, capsanthin and capsaicine are natural foodstuff additive, the method of extraction separation capsaicine and capsanthin mainly is a solvent-extraction process from red pepper at present, adopt the red chilly powder of pulverizing to be the leaching object, the extraction of use single-solvent process, perhaps use saltout isolating method and alkali lye saponification to carry out the method for purification processes, the method for successively using two kinds of solvents to extract is also arranged.There are various impurity in the product that solvent-extraction process obtains, especially tarry odour, pungent etc., if it is it is further refining, general method is to adopt highly basic, strong acid or salt to wash, this method is easily brought heavy metal ion in capsaicine and capsanthin, product purity is low, and yield is low, the production cost height.
Summary of the invention
The object of the invention provides a kind of capsanthin and capsaicine extraction process, the rate of recovery height of capsanthin and capsaicine, and the dna purity height, the yield height, production cost is low, and operation is simple.
Technical scheme of the present invention is: a kind of capsanthin and capsaicine extraction process, and it may further comprise the steps;
1., with the mixing solutions of ethanol and normal hexane the red pepper particle is soaked after-filtration and obtain filtrate;
2., filtrate left standstill layering separates after 30-60 minute, telling normal hexane is that A reaches ethanol mutually and the capsaicine blended liquid phase is the B phase with the capsanthin blended liquid phase, respectively A is handled mutually obtaining capsanthin and reach B handled mutually and obtain capsaicine;
A handled mutually be: heating A phase earlier, the normal hexane volatilization is separated, stay spissated capsanthin liquid; Capsanthin liquid is mixed with ethanol, leave standstill the back layering and separate, obtain ethanol and capsaicine blended liquid phase and capsanthin liquid phase and be C mutually; Feed CO at C in mutually 2Or nitrogen or the rare gas element except that radon gas, residual solvent and the assorted flavor of C in mutually is removed, make purified capsanthin;
B handled mutually be: heating B phase, the ethanol volatilization is separated, stay the capsaicine concentrated solution; The capsaicine concentrated solution is mixed with acetone solvent, leaves standstill the back layering and separate, tell capsaicine and acetone blended liquid phase and be D mutually with other impurity liquid phase; Heating D phase makes the acetone volatilization be separated, and makes purified capsaicine.
Step 1. before, red pepper dry powder is broken into 30-50 purpose red chilly powder, red chilly powder is contacted with water vapor earlier is ripened the cylindricality capsicum particle that is pressed growth 1-2cm, diameter 3-5mm again.
Step 1. in, the concentration of ethanolic soln is 95-97%, preferred concentration is 95%, hexane solution concentration is 90-99%, preferred concentration is 99%, the weight ratio of capsicum particle, ethanol and normal hexane is: 1: 3-4: 2-3.
Step 1. in, the soak time scope is 150-200 minute, the drought condition down capsicum of growth is difficult to extraction, and is long slightly to the time of its immersion.Soaking temperature is 50~65 ℃.
In the processing that A is carried out mutually, with capsanthin liquid phase blended concentration of ethanol be 75-80%, preferred concentration is 75%, capsanthin liquid and alcoholic acid weight ratio are: 1: 3-5.
In the processing that A is carried out mutually, capsanthin liquid mixes the back and was left standstill 200-300 minute with ethanol.
Feeding CO to C in mutually 2Or before nitrogen or the rare gas element except that radon gas, C and ethanol are mixed and layering separates, repeat repeatedly, the remaining capsaicine of C in mutually is separated.
In the processing that B is carried out mutually, the weight ratio of capsaicine concentrated solution and acetone solvent is 1: 3-6.
In the processing that B is carried out mutually, the capsaicine concentrated solution is with after acetone solvent mixes, and the temperature range that leaves standstill is 30-40 ℃.
Step 1., filtrate is heated with D mutually mutually by standing demix, A phase, B and to C mutually in feeding CO 2Or the process of nitrogen or the rare gas element except that radon gas is carried out under vacuum condition.
The present invention compared with prior art has the following advantages: with the red pepper dry grinding, slaking and compressed granulate, improve the total yield of haematochrome and capsaicine, adopt two kinds of solvents: ethanol and normal hexane carry out the leaching of capsanthin and capsaicine simultaneously, simplified operation, and the remaining capsaicine in the capsanthin is carried out the layering separation and purification with ethanol, adopt assorted flavor and trace solvent in the CO2 gas removal capsanthin residual, dissolve peppery plain phase with acetone solvent, the capsanthin that proposes and the purity and the yield height of capsaicine, and production cost is low, is convenient to operation.
Embodiment
A kind of novel process of extracting capsanthin and capsaicine from red pepper may further comprise the steps:
1., dried with red pepper is raw material, with the chillies fragmentation, remove chilli seed, be ground into the red chilly powder of 40 orders (particle diameter 0.45mm), red chilly powder is contacted with the 0.2Mpa saturated vapor, make the red chilly powder thermalization 35 seconds action time, then the red chilly powder after the slaking suppressed the cylindricality capsicum particle of growth 1.5cm, diameter 4mm;
2., the capsicum particle is soaked in the solvent, soak after-filtration and obtain filtrate; Solvent is that concentration is that 95% ethanol and concentration are the mixture of 96% normal hexane, according to the weight ratio of capsicum particle, ethanol, normal hexane is that 1: 3: 3 ratio is mixed the three, soaking temperature is 55 ℃, soak time 150 minutes, under vacuum condition, carry out vacuum tightness 0.015Mpa, the different solubility in ethanol and normal hexane because of haematochrome in the capsicum particle and capsaicine, can extract, promptly haematochrome is dissolved in normal hexane and capsaicine is dissolved in ethanol;
Because of the decomposition temperature of capsanthin is 60 ℃, the temperature of extraction is too high, can cause capsanthin to be decomposed, so extraction process need keep lesser temps, extracts simultaneously at vacuum state and carries out preventing that capsanthin is oxidized.
3., resulting filtrate was left standstill 40 minutes, layering separates, telling the upper strata normal hexane is that A is the B phase with lower floor's 95% ethanol and capsaicine blended liquid phase mutually with the capsanthin blended liquid phase, A is handled mutually obtaining capsanthin and B handled mutually obtaining capsaicine respectively;
The step that A is handled mutually is:
(1), under vacuum state heating A phase, reclaim normal hexane, obtain spissated capsanthin liquid, the boiling point of normal hexane is 68 ℃, its boiling point lowering during vacuum state, with A heat phase three times, Heating temperature is 60 ℃;
(2), the ethanol of capsanthin liquid with 75% concentration is mixed, leave standstill that layering separates after 240 minutes, capsanthin liquid and alcoholic acid weight ratio are: 1: 4, obtain upper strata ethanol and capsaicine blended liquid phase and lower floor's capsanthin liquid phase and be C mutually;
(3), the ethanol of C and 75% concentration is mixed and layering separates, blending ratio repeats 4 times with (2), and the remaining capsaicine of C in mutually is separated;
(4), feed CO at C in mutually 2Gas, CO 2Gas and C residual solvent and the assorted flavor mixed volatilization in mutually, thus residual solvent and the assorted flavor of C in mutually removed, make purified capsanthin;
The step that B is handled mutually is:
(1), under vacuum state heating B phase, reclaim ethanol, obtain the capsaicine concentrated solution; The alcoholic acid boiling point of 95% concentration is 78 ℃, its boiling point lowering of vacuum state, and the decomposition temperature of capsaicine is 100 ℃, with B heat phase three times, Heating temperature is 75 ℃.
(2), with capsaicine concentrated solution and acetone solvent with 1: 5 mixed of weight ratio, under 35 ℃ of temperature condition, leave standstill, layering separates again, tell capsaicine and acetone blended liquid phase and be D mutually with other impurity liquid phase;
(3), under reduced pressure heating D phase, reclaim acetone, make purified capsaicine.
Adopt pulverizing, steam cure among the present invention, the method that reaches compressed granulate makes capsanthin and capsaicine in the raw material of hot pepper be easy to more leach, and is applicable to the continuous countercurrent leaching process, thereby improves total recovery yield of capsanthin and capsaicine.
Adopt two kinds of solvents simultaneously: ethanol and normal hexane carry out the leaching of capsanthin and capsaicine, and with ethanol the remaining capsaicine in the capsanthin are carried out the layering separation and purification, and adopt CO 2Assorted flavor and dissolvent residual in the gas removal capsanthin are further purified capsanthin.
Adopt acetone solvent to dissolve to the capsaicine concentrated solution, layering, separation, thus obtain the higher capsaicine product of purity.
Capsanthin that the present invention makes and capsaicine purity height, its index all reaches the regulation of GB10783-89 after testing, and the assorted flavor of inclusion-free is applied widely, can be used for industries such as food, chemical industry, medicine and makeup.Rate of recovery height of the present invention, the total yield of capsanthin are 95-97%, and the capsaicine total yield is 90-95%, each step reaction is stable, is suitable for scale operation, the output height, simple to operate, ethanol, normal hexane, acetone are all recyclable to be utilized again, and production cost is low.

Claims (11)

1, a kind of capsanthin and capsaicine extraction process, it is characterized in that: it may further comprise the steps;
1., with the mixing solutions of ethanol and normal hexane the red pepper particle is soaked after-filtration and obtain filtrate;
2., described filtrate left standstill the back layering separate, telling normal hexane is that A reaches ethanol mutually and the capsaicine blended liquid phase is the B phase with the capsanthin blended liquid phase, respectively A is handled mutually obtaining capsanthin and reach B handled mutually and obtain capsaicine;
Described A handled mutually be: the described A phase of heating earlier, described normal hexane volatilization is separated, stay spissated capsanthin liquid; Described capsanthin liquid is mixed with ethanol, leave standstill the back layering and separate, obtain ethanol and capsaicine blended liquid phase and capsanthin liquid phase and be C mutually; Feed CO at described C in mutually 2Or nitrogen or the rare gas element except that radon gas, residual solvent and the assorted flavor of described C in mutually is removed, make purified capsanthin;
Described B handled mutually be: heat described B phase, described ethanol volatilization is separated, stay the capsaicine concentrated solution; Described capsaicine concentrated solution is mixed with acetone solvent, leaves standstill the back layering and separate, tell capsaicine and acetone blended liquid phase and be D mutually with other impurity liquid phase; Heat described D phase, make described acetone volatilization be separated, make purified capsaicine.
2, capsanthin according to claim 1 and capsaicine extraction process, it is characterized in that: described step 1. before, red pepper dry powder is broken into 30-50 purpose red chilly powder, described red chilly powder is contacted with water vapor earlier be ripened the cylindricality capsicum particle that is pressed growth 1-2cm, diameter 3-5mm again.
3, capsanthin according to claim 1 and capsaicine extraction process, it is characterized in that: described step 1. in, the concentration of described ethanolic soln is 95-97%, described hexane solution concentration is 90-99%, and the weight ratio of described capsicum particle, described ethanol and described normal hexane is: 1: 3-4: 2-3.
4, capsanthin according to claim 1 and capsaicine extraction process is characterized in that: described step 1. in, the soak time scope is 150-200 minute, soaking temperature is 50~65 ℃.
5, capsanthin according to claim 1 and capsaicine extraction process, it is characterized in that: in the processing that described A is carried out mutually, with the described concentration of ethanol of described capsanthin liquid phase blended be 75-80%, described capsanthin liquid and described alcoholic acid weight ratio are: 1: 3-5.
6, capsanthin according to claim 1 and capsaicine extraction process is characterized in that: in the processing that described A is carried out mutually, described capsanthin liquid mixes the back and was left standstill 200-300 minute with ethanol.
7, capsanthin according to claim 1 and capsaicine extraction process is characterized in that: feeding CO to described C in mutually 2Or before nitrogen or the rare gas element except that radon gas, described C and ethanol are mixed and layering separates, repeat repeatedly, the remaining capsaicine of C in mutually is separated.
8, capsanthin according to claim 1 and capsaicine extraction process is characterized in that: in the processing that described B is carried out mutually, the weight ratio of described capsaicine concentrated solution and acetone solvent is 1: 3-6.
9, capsanthin according to claim 1 and capsaicine extraction process is characterized in that: in the processing that described B is carried out mutually, described capsaicine concentrated solution is with after acetone solvent mixes, and the temperature range that leaves standstill is 30-40 ℃.
10, capsanthin according to claim 1 and capsaicine extraction process is characterized in that: described filtrate was left standstill 30-60 minute.
11, capsanthin according to claim 1 and capsaicine extraction process is characterized in that: described step 1., described filtrate is heated with described D mutually mutually by standing demix, described A phase, described B and to described C mutually in feeding CO 2Or the process of nitrogen or the rare gas element except that radon gas is carried out under vacuum condition.
CN 200610040907 2006-08-04 2006-08-04 Extraction technology of capsanthin and capsicine Pending CN1911902A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 200610040907 CN1911902A (en) 2006-08-04 2006-08-04 Extraction technology of capsanthin and capsicine

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 200610040907 CN1911902A (en) 2006-08-04 2006-08-04 Extraction technology of capsanthin and capsicine

Publications (1)

Publication Number Publication Date
CN1911902A true CN1911902A (en) 2007-02-14

Family

ID=37720995

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 200610040907 Pending CN1911902A (en) 2006-08-04 2006-08-04 Extraction technology of capsanthin and capsicine

Country Status (1)

Country Link
CN (1) CN1911902A (en)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101696327A (en) * 2009-10-27 2010-04-21 青岛赛特香料有限公司 Method for removing phospholipid from capsanthin by using low-molecular-weight fatty acid as entrainer
CN101906254A (en) * 2010-07-20 2010-12-08 安阳市晶华油脂工程有限公司 Method for extracting capsaicin ointment from dimethyl ether
CN102079883A (en) * 2010-11-22 2011-06-01 武城县英潮经贸有限公司 Novel process for extracting capsanthin and chilli extract by composite solvent
CN101338080B (en) * 2008-05-05 2011-09-21 苏州市兴科现代中药工艺装备开发有限公司 Method for removing capsaicin in production process of capsanthin pigment
CN102516802A (en) * 2011-12-12 2012-06-27 山东凯斯达机械制造有限公司 Method for extracting capsicum red pigment and capsaicin
CN102604417A (en) * 2011-12-15 2012-07-25 武城县英潮经贸有限公司 New technology for separating haematochrome and pectin from capsanthin centrifugate
CN102827491A (en) * 2012-08-22 2012-12-19 孙华田 Method for extracting paprika red pigment by concentrated liquid detergent
CN101747657B (en) * 2009-12-22 2013-01-09 晨光生物科技集团股份有限公司 Industrial method for improving quality of capsicum red pigment
CN102898865A (en) * 2012-11-12 2013-01-30 河北东之星生物科技股份有限公司 Method for preparing capsanthin
CN109181353A (en) * 2018-09-28 2019-01-11 晨光生物科技集团股份有限公司 A method of improving capsicum red pigment absorption ratio

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101338080B (en) * 2008-05-05 2011-09-21 苏州市兴科现代中药工艺装备开发有限公司 Method for removing capsaicin in production process of capsanthin pigment
CN101696327B (en) * 2009-10-27 2012-10-17 青岛赛特香料有限公司 Method for removing phospholipid from capsanthin by using low-molecular-weight fatty acid as entrainer
CN101696327A (en) * 2009-10-27 2010-04-21 青岛赛特香料有限公司 Method for removing phospholipid from capsanthin by using low-molecular-weight fatty acid as entrainer
CN101747657B (en) * 2009-12-22 2013-01-09 晨光生物科技集团股份有限公司 Industrial method for improving quality of capsicum red pigment
CN101906254A (en) * 2010-07-20 2010-12-08 安阳市晶华油脂工程有限公司 Method for extracting capsaicin ointment from dimethyl ether
CN102079883A (en) * 2010-11-22 2011-06-01 武城县英潮经贸有限公司 Novel process for extracting capsanthin and chilli extract by composite solvent
CN102079883B (en) * 2010-11-22 2013-05-22 武城县英潮经贸有限公司 Novel process for extracting capsanthin and chilli extract by composite solvent
CN102516802A (en) * 2011-12-12 2012-06-27 山东凯斯达机械制造有限公司 Method for extracting capsicum red pigment and capsaicin
CN102604417A (en) * 2011-12-15 2012-07-25 武城县英潮经贸有限公司 New technology for separating haematochrome and pectin from capsanthin centrifugate
CN102827491A (en) * 2012-08-22 2012-12-19 孙华田 Method for extracting paprika red pigment by concentrated liquid detergent
CN102898865A (en) * 2012-11-12 2013-01-30 河北东之星生物科技股份有限公司 Method for preparing capsanthin
CN102898865B (en) * 2012-11-12 2014-06-04 河北东之星生物科技股份有限公司 Method for preparing capsanthin
CN109181353A (en) * 2018-09-28 2019-01-11 晨光生物科技集团股份有限公司 A method of improving capsicum red pigment absorption ratio

Similar Documents

Publication Publication Date Title
Chen et al. Selective extraction of nitric and acetic acids from etching waste acid using N235 and MIBK mixtures
CN1911902A (en) Extraction technology of capsanthin and capsicine
JP2021532178A (en) A method for binding and recovering an organic acid in an aqueous organic acid solution
CN101805261A (en) Method for preparing competitive product of chlorogenic acid by folium cortex eucommiae
CN113773184B (en) Method for extracting curcumin compounds
CN111348633A (en) Wet phosphoric acid purifying process and its extraction liquid regenerating method
CN1259310C (en) Process for extracting and separating caprolactam from amide oil
US9073889B2 (en) Process for the manufacture of taxifolin from wood
JPH0316602A (en) Continuous method of partial separation of water- soluble component from slurry
CN115260005A (en) Method for purifying and extracting cannabidiol and application
CN104497057A (en) Process for extracting tea polyphenols from Yunan dayezhong tea leaves
CN1106892C (en) Process for extracting pure tobacco oil, melanoid and nicotine and preparing composite fertilizer
CN220277839U (en) Device for recycling hexachlorocyclo triphosphazene synthetic waste residues
CN103012512A (en) Separation and purification method of salidroside in natural rhodiola sachalinensis
CN1008821B (en) Making method of natural blue total saponin
CN1267684A (en) Supercritical CO2 refining process of deodored capsanthin
CN1405211A (en) Method for preparing high-purity xanthohumic acid using supercritical CO2
CN100590187C (en) Extraction method of effective components in capsicum and potato
CN101121663A (en) Method for preparing rosmarinic acid from folium perillae acutae
CN112694409B (en) Method and device for recycling triethylamine in wastewater
CN113402987A (en) Extraction method of bayberry tannin extract
CN1074761C (en) Process for separating and concentrating formic acid with phosphorus-contained extractant
CN107827738A (en) Method for separating carnosic acid from rosemary extract
KR102831509B1 (en) Method for preparation of acrylic acid
CN114315546B (en) Method for treating waste electronic solvent containing water, propylene glycol methyl ether and cyclopentanone

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C12 Rejection of a patent application after its publication
RJ01 Rejection of invention patent application after publication