CN101205502A - Ultrasonic-assisted method for extracting pepper oleoresin - Google Patents

Ultrasonic-assisted method for extracting pepper oleoresin Download PDF

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Publication number
CN101205502A
CN101205502A CNA2007101931000A CN200710193100A CN101205502A CN 101205502 A CN101205502 A CN 101205502A CN A2007101931000 A CNA2007101931000 A CN A2007101931000A CN 200710193100 A CN200710193100 A CN 200710193100A CN 101205502 A CN101205502 A CN 101205502A
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China
Prior art keywords
extraction
pepper
extract
ultrasonic
gained
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CNA2007101931000A
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Chinese (zh)
Inventor
方杰
王明奇
赵庆军
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ZHENGZHOU XOMOLON FLAVOR CO Ltd
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ZHENGZHOU XOMOLON FLAVOR CO Ltd
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Priority to CNA2007101931000A priority Critical patent/CN101205502A/en
Publication of CN101205502A publication Critical patent/CN101205502A/en
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Abstract

The invention provides a method for ultrasonic-assisted extraction of pepper oil resin which comprises the following procedures: peppers are cleaned, sundried or oven-dried, and pulverized into pepper powder; the pepper powder is put into the extraction solvent for dipping treatment to obtain the dipping solution; the dipping solution is put into ultrasonic equipment for ultrasonic enhanced extraction to obtain an extract I; the extract I is made a solid-liquid separation to obtain a liquid phase and a solid phase, and the liquid phase is the extract liquid I; the solid phase is put into the ultrasonic equipment for second ultrasonic enhanced extraction to obtain an extract II, then the extract II is made the solid-liquid separation, the obtained liquid phase is the extract liquid II; the extract liquid I and the extract liquid II are merged, then are made a pressure-reducing distillation, the extraction solvent is separated, and the brown pasty fluid, namely pepper oil resin, can be obtained. The method has simple operation, strong practicability, short time used to extract the pepper oil resin, convenience and quickness, high extraction yield, short production cycle and low cost.

Description

The method of ultrasonic assisted extraction pepper oleoresin
Technical field
The present invention relates to a kind of method of extracting pepper oleoresin, specifically, related to a kind of method of ultrasonic assisted extraction pepper oleoresin.
Background technology
The evergreen dungarunga plant of Piper has the branch of white pepper and piper nigrum, and it has special fragrance, intensive sharp flavor; The main component that pepper contains is multiple amidess such as piperine, pepper woods alkali, contains the volatile oil of compositions such as being mainly piperonylaldehyde and tetrahydrogeraniol again, i.e. volatile oil.
In foodstuffs industry, according to 2003 No. four file of Ministry of Health of the People's Republic of China, pepper oleoresin, pepper oil are approved for the foodstuff additive new variety; Pepper oleoresin is white pepper or piper nigrum natural extract, and cost is low, is easy to store, transport, and American-European countries has very long use history.
The preparation of traditional pepper oleoresin adopts organic solvent to carry out the mode of simply immersing, and its leaching yield is lower, and need repeatedly repeat to extract, the operating process more complicated, and efficient is low.
China Patent No. is " 00130396.1 ", Granted publication number is " CN1128194C ", and denomination of invention is carried out pepper powder lixiviate, separation through two or more mixed organic solvents, obtained the extraction process of pepper oleoresin after concentrating for disclosing in the patent of " process for preparing pepper oil resin ";
Chinese patent application number is " 02119671.0 ", publication number is CN1458253A, and name is called to disclose in the patent application of " a kind of extracting method of pepper oleoresin " pepper powder stirred through alcohol to be extracted the back, separate the concentrated extraction process that obtains pepper oleoresin;
In the above-mentioned patent documentation, the extraction of pepper oleoresin mainly is to adopt organic solvent directly to soak the extraction process that pepper powder extracts, and the problem of its existence is that extraction process used extraction time is long, and pepper oleoresin extraction income rate is relatively low, the cost height, production efficiency is low.
In order to overcome the above problems, people are seeking a kind of ideal technical solution always.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, thereby a kind of method of ultrasonic assisted extraction pepper oleoresin is provided, this method has overcome extracts the shortcoming that the pepper oleoresin time is long, extraction yield is relatively low in the prior art.
To achieve these goals, the invention provides a kind of method of ultrasonic assisted extraction pepper oleoresin, comprise following extraction step:
Step 1, the pepper dry fruit is cleaned up, dry or dry, pulverize, make pepper powder;
Step 2, step 1 gained pepper powder put into extracts solvent and carry out immersion treatment, soaking solution;
Step 3, step 2 gained soaking solution put into ultrasonic device carry out ultrasound-enhanced extraction, extract I;
Step 4, the extract obtained I of step 3 is carried out solid-liquid separation, liquid phase and solid phase, the gained liquid phase is extracting solution I;
Step 5, step 4 gained solid phase put into ultrasonic device carry out ultrasound-enhanced extraction again, extract II, then, again extract II is carried out solid-liquid separation, the gained liquid phase is extracting solution II;
Step 6, step 4 gained extracting solution I and step 5 gained extracting solution II are merged, then, carry out underpressure distillation, isolate the extraction solvent, obtain brown paste fluid, be pepper oleoresin.
Based on above-mentioned, in step 1, the pepper dry fruit is pulverized the back cross 40~80 mesh sieves, make pepper powder.
Based on above-mentioned, in step 2, described extraction solvent is any one in acetone, ethanol, the sherwood oil.
Based on above-mentioned, in step 2, the part by weight of described extraction solvent and described pepper powder is 6~12: 1, and soaking temperature is 40 ℃~60 ℃.
Based on above-mentioned, in step 3 and step 5, in the ultrasound-enhanced leaching process, the supersound extraction frequency is 20~60KHz, and ultrasound intensity is 5~40W/cm 2
Based on above-mentioned, in step 3 and step 5, in the ultrasound-enhanced leaching process, extracting temperature is 40 ℃~60 ℃, and extraction time is 40 minutes~120 minutes.
Based on above-mentioned, in step 4 and step 5, described solid-liquid separation adopts the vacuum filtration mode.
Based on above-mentioned, in step 6, the temperature range of described underpressure distillation is 35 ℃~60 ℃.
Based on above-mentioned, in step 6, the pressure range of described underpressure distillation is 0.065Mpa~0.09Mpa.
The relative prior art of the present invention has outstanding substantive distinguishing features and obvious improvement, specifically, the method of this ultrasonic assisted extraction pepper oleoresin is simple to operate, practical, extract the used time weak point of pepper oleoresin, convenient and swift, and extract the income rate height, economize in raw materials, with short production cycle, cost is low; Adopt this extracting method to heat, technology is simple, and the effective ingredient of pepper oleoresin is not destroyed, and the oil flavor is pure and fresh pure, and color and luster is limpid.
This method adopts sonic oscillation to strengthen and extracts, its principle mainly is to produce quick mechanical vibration wave by PZT (piezoelectric transducer) to come the accelerating medium particle movement, thereby generation cavatition, and utilize hyperacoustic vibration homogenize to make the effect unanimity that each point is subjected in the sample media, thereby reduce the reactive force between target extract and the sample matrices, and then realize solid-liquid extracting and separating.
Description of drawings
Fig. 1 is the process flow diagram of the method for ultrasonic assisted extraction pepper oleoresin of the present invention.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment one
As shown in Figure 1, a kind of method of ultrasonic assisted extraction pepper oleoresin comprises following extraction step:
Step 1, selected double centner white pepper dry fruit is cleaned up, dry or dry, pulverize, then, cross 40 mesh sieves, make pepper powder;
Step 2, step 1 gained pepper powder is put into 800 kilograms 95% ethanol soak half an hour, soaking temperature is 40 ℃, soaking solution;
Step 3, step 2 gained soaking solution is put into ultrasonic device carry out ultrasound-enhanced extraction, wherein, the supersound extraction frequency is 40KHz, and ultrasound intensity is 20W/cm 2, extracting temperature is 48 ℃, extraction time is 50 minutes, gets extract I;
Step 4, adopt the vacuum filtration mode to carry out solid-liquid separation the extract obtained I of step 3, liquid phase and solid phase, the gained liquid phase is extracting solution I;
Step 5, step 4 gained solid phase put into the described ultrasonic device of step 3 carry out ultrasound-enhanced extraction again, extract after 60 minutes extract II, then, again extract II is adopted the vacuum filtration mode to carry out solid-liquid separation, the gained liquid phase is extracting solution II;
Step 6, step 4 gained extracting solution I and step 5 gained extracting solution II being merged, then, is that 0.075MPa, temperature are under 50 ℃ the condition at pressure, carry out underpressure distillation, isolate ethanol, obtain about about 10 kilograms brown paste fluid, be pepper oleoresin.
Embodiment two
A kind of method of ultrasonic assisted extraction pepper oleoresin comprises following extraction step:
Step 1,120 kilograms of selected white pepper dry fruits are cleaned up, dry or dry, pulverize, then, cross 60 mesh sieves, make pepper powder;
Step 2, step 1 gained pepper powder is put into 1000 kilograms acetone soln soaked 40 minutes, soaking temperature is 50 ℃, soaking solution;
Step 3, step 2 gained soaking solution is put into ultrasonic device carry out ultrasound-enhanced extraction, wherein, the supersound extraction frequency is 45KHz, and ultrasound intensity is 25W/cm 2, extracting temperature is 50 ℃, extraction time is 60 minutes, gets extract I;
Step 4, adopt the vacuum filtration mode to carry out solid-liquid separation the extract obtained I of step 3, liquid phase and solid phase, the gained liquid phase is extracting solution I;
Step 5, step 4 gained solid phase put into the described ultrasonic device of step 3 carry out ultrasound-enhanced extraction again, extract after 80 minutes extract II, then, again extract II is adopted the vacuum filtration mode to carry out solid-liquid separation, the gained liquid phase is extracting solution II;
Step 6, step 4 gained extracting solution I and step 5 gained extracting solution II being merged, then, is that 0.08MPa, temperature are under 55 ℃ the condition at pressure, carry out underpressure distillation, isolate ethanol, obtain about about 12 kilograms brown paste fluid, be pepper oleoresin.
Should be noted that at last: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; Although with reference to preferred embodiment the present invention is had been described in detail, those of ordinary skill in the field are to be understood that: still can make amendment or the part technical characterictic is equal to replacement the specific embodiment of the present invention; And not breaking away from the spirit of technical solution of the present invention, it all should be encompassed in the middle of the technical scheme scope that the present invention asks for protection.

Claims (9)

1. the method for a ultrasonic assisted extraction pepper oleoresin is characterized in that, comprises following extraction step:
Step 1, the pepper dry fruit is cleaned up, dry or dry, pulverize, make pepper powder;
Step 2, step 1 gained pepper powder put into extracts solvent and carry out immersion treatment, soaking solution;
Step 3, step 2 gained soaking solution put into ultrasonic device carry out ultrasound-enhanced extraction, extract I;
Step 4, the extract obtained I of step 3 is carried out solid-liquid separation, liquid phase and solid phase, the gained liquid phase is extracting solution I;
Step 5, step 4 gained solid phase put into ultrasonic device carry out ultrasound-enhanced extraction again, extract II, then, again extract II is carried out solid-liquid separation, the gained liquid phase is extracting solution II;
Step 6, step 4 gained extracting solution I and step 5 gained extracting solution II are merged, then, carry out underpressure distillation, isolate the extraction solvent, obtain brown paste fluid, be pepper oleoresin.
2. the method for ultrasonic assisted extraction pepper oleoresin according to claim 1 is characterized in that: in step 1, the pepper dry fruit is pulverized the back cross 40~80 mesh sieves, make pepper powder.
3. the method for ultrasonic assisted extraction pepper oleoresin according to claim 1 is characterized in that: in step 2, described extraction solvent is any one in acetone, ethanol, the sherwood oil.
4. the method for ultrasonic assisted extraction pepper oleoresin according to claim 1 is characterized in that: in step 2, the part by weight of described extraction solvent and described pepper powder is 6~12: 1, and soaking temperature is 40 ℃~60 ℃.
5. the method for ultrasonic assisted extraction pepper oleoresin according to claim 1 is characterized in that: in step 3 and step 5, in the ultrasound-enhanced leaching process, the supersound extraction frequency is 20~60KHz, and ultrasound intensity is 5~40W/cm 2
6. the method for ultrasonic assisted extraction pepper oleoresin according to claim 1 is characterized in that: in step 3 and step 5, in the ultrasound-enhanced leaching process, extracting temperature is 40 ℃~60 ℃, and extraction time is 40 minutes~120 minutes.
7. the method for ultrasonic assisted extraction pepper oleoresin according to claim 1 is characterized in that: in step 4 and step 5, described solid-liquid separation adopts the vacuum filtration mode.
8. the method for ultrasonic assisted extraction pepper oleoresin according to claim 1 is characterized in that: in step 6, the temperature range of described underpressure distillation is 35 ℃~60 ℃.
9. the method for ultrasonic assisted extraction pepper oleoresin according to claim 1 is characterized in that: in step 6, the pressure range of described underpressure distillation is 0.065Mpa~0.09Mpa.
CNA2007101931000A 2007-12-13 2007-12-13 Ultrasonic-assisted method for extracting pepper oleoresin Pending CN101205502A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101928463A (en) * 2010-07-08 2010-12-29 天津春发食品配料有限公司 Method for preparing black pepper oil resin
CN102925059A (en) * 2012-11-12 2013-02-13 中国热带农业科学院香料饮料研究所 Preparation method of pepper oleoresin
CN102925283A (en) * 2012-10-23 2013-02-13 中国热带农业科学院香料饮料研究所 Preparation method of pepper oleoresin
CN103396889A (en) * 2013-07-10 2013-11-20 红云红河烟草(集团)有限责任公司 Preparation method of vetiveria zizanioides L. oil and application of vetiver vetiveria zizanioides L. oil in cigarettes
CN107245372A (en) * 2017-07-14 2017-10-13 云南宏绿辣素有限公司 A kind of tsaoko oleoresin extracting method

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101928463A (en) * 2010-07-08 2010-12-29 天津春发食品配料有限公司 Method for preparing black pepper oil resin
CN101928463B (en) * 2010-07-08 2012-09-12 天津春发生物科技集团有限公司 Method for preparing black pepper oil resin
CN102925283A (en) * 2012-10-23 2013-02-13 中国热带农业科学院香料饮料研究所 Preparation method of pepper oleoresin
CN102925283B (en) * 2012-10-23 2014-01-22 中国热带农业科学院香料饮料研究所 Preparation method of pepper oleoresin
CN102925059A (en) * 2012-11-12 2013-02-13 中国热带农业科学院香料饮料研究所 Preparation method of pepper oleoresin
CN103396889A (en) * 2013-07-10 2013-11-20 红云红河烟草(集团)有限责任公司 Preparation method of vetiveria zizanioides L. oil and application of vetiver vetiveria zizanioides L. oil in cigarettes
CN107245372A (en) * 2017-07-14 2017-10-13 云南宏绿辣素有限公司 A kind of tsaoko oleoresin extracting method

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