CN102925283B - Preparation method of pepper oleoresin - Google Patents
Preparation method of pepper oleoresin Download PDFInfo
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- CN102925283B CN102925283B CN201210406498.2A CN201210406498A CN102925283B CN 102925283 B CN102925283 B CN 102925283B CN 201210406498 A CN201210406498 A CN 201210406498A CN 102925283 B CN102925283 B CN 102925283B
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Abstract
The invention relates to a preparation method of pepper oleoresin. According to the invention, flavor substances in pepper are quickly extracted through unique room temperature-program boosting in combination of an ultrasonic-microwave synergistic extraction method based on a field effect-accelerated solvent method, wherein the pressure range is 6-8 bars, the boosting extraction time is 10-30 minutes, the ultrasonic power is 50W, the frequency is 40KHz, the microwave power is 70-500W, the microwave frequency is 2450MHz, and the synergistic extraction time is 10-20 minutes; and the extracted flavor substances are subjected to filtering, solvent removing, drying and like processes to prepare the pepper oleoresin. The extraction method disclosed by the invention is safe and efficient, and has the advantages of short extracting time, high pepper oleoresin yield, higher piperine content, sufficient peppery taste and stronger fragrance compared with extraction methods such as ultrasonic extraction, microwave extraction, solvent extraction, Soxhlet extraction, hot reflux and the like.
Description
Technical field
The present invention relates to a kind of making method of pepper oleoresin.
Background technology
Pepper (Piper nigrum L.) is piperaceae, the important spice crop in the Piper perennial evergreen vine ，Shi world.The seed of pepper contains volatile oil, piperine, crude fat, crude protein, lignanoids, alkaloids, flavonoid, aromatic compound and amides etc.The traditional Chinese medical science thinks that pepper taste is pungent, hot in nature, nontoxic, can warming spleen and stomach for dispelling cold, promoting the circulation of QI to relieve pain, be applicable to that middle Jiao coldly contains, place food does not disappear, coldness and pain in the epigastrium, gastric disorder causing nausea vomiting, the diarrhea etc. of having loose bowels.In medical industries, pepper can be used as peptic, antipyretic and tunica mucosa bronchiorum stimulant etc., can treat maldigestion, cold phlegm, cough, enteritis, bronchitis, flu and rheumatosis etc., in addition, is also used as sanitas in foodstuffs industry.Research in recent years shows, pepper all has activity in analgesia, calmness, anti-inflammatory, anticonvulsion, antibacterial, desinsection, the many-side such as anticancer, after biotechnology transformation, also can be widely used in the fields such as modern pharmaceutical, smoking cessation, drug rehabilitation and military affairs, purposes is wide, economic worth is high.
Pepper products is mainly piper nigrum and white pepper both at home and abroad at present, account for the more than 90% of ultimate production, and pepper oleoresin is considerably less.But pepper oleoresin has strong fragrance and the pungency pungent of pepper concurrently, can be used as spices and drip, for the seasoning of flavoring industry soy sauce, fermented bean curd etc., the improvement of meat product taste, and the preparation etc. of seasoning powder in puffed food, ready-to-eat, extensive in food processing field application prospect.
Pepper oleoresin is mainly by solvent extration, the compositions such as color in pepper to be extracted, and gained extraction liquid obtains through filtration, desolvation, the technique such as dry.The water of pepper, ether or ethanol extraction have the tapeworm of killing, deodorizing, anticorrosion and antioxygenation.
The research of at present, extracting pepper oleoresin both at home and abroad relates to: solvent extraction method, Soxhlet extraction process, microwave method, supersonic method and supercritical methanol technology etc.Wherein fragrance in pepper and taste composition being retained to good method is supercritical methanol technology, and this method also has limitation: piperine extracts temperature mass crystallization at it, cause leaching process numerous and diverse, and extraction cost is high.By contrast, it is quick and convenient that the extract by solvents process that field-effect is accelerated seems, is particularly conducive to the extraction separation of the piper nigrum taste composition of high polarity and high level.
Summary of the invention
For above-mentioned situation, the object of this invention is to provide a kind of making method of pepper oleoresin.The solvent method that it accelerates based on field-effect, unique room temperature-program the supercharging of main employing, in conjunction with ultrasonic-microwave synergistic extraction by the flavour substances rapid extraction in pepper out, desolvation, the technique such as dry and obtain after filtration,, by white pepper machining, obtain pepper oleoresin and be tawny paste, piper nigrum machining obtains pepper oleoresin, and to be brown slightly brown, it is slightly green that black pepper machining obtains pepper oleoresin brown, there is certain mobility, after in the time of standing one section of room temperature, there is needle-like crystal to separate out, water insoluble, dissolve in 50 ℃ of above ethanol.Having the peculiar flavour of pepper concurrently, can be used as again the local flavor that foodstuff additive regulate food, is a kind of desirable seasoning food auxiliary material.
A making method for pepper oleoresin, adopts the quick solvent extraction of program supercharging and ultrasonic-microwave synergistic extraction method that the flavour substances in pepper is extracted, after filtration, desolvation, drying process make pepper oleoresin.
The making method of described pepper oleoresin, comprises the steps:
(1) prepare pepper powder, choosing white pepper, piper nigrum or black pepper grain is raw material, with pulverizer, is ground into pepper powder;
(2) add solvent, selecting edible ethanol is solvent, adds the solvent of 10-50 part (preferably 20-50 part) according to 1 part of pepper powder raw material;
(3) the quick solvent extraction of program supercharging;
(4) extraction, adopts ultrasonic-microwave synergistic extraction;
(5) filter, adopt vacuum filtration fast filtering pepper powder, collect filtrate;
(6) desolvation, adopts the concentrated desolvation of vacuum rotating;
(7) dry, adopt vacuum-drying;
(8) bottling, sealing, lucifuge, lower than 25 ℃ of storages.
The moisture content of white pepper, black pepper or the piper nigrum of selecting in step (1) is lower than 12%; Step is crushed to diameter at 0.15-0.85mm in (1).
In step (2), edible ethanol concentration is 60%～95%.
In step (3), pressure range is controlled at 6-8bar, and the pressure extraction time is 1.0-3.0min at every turn, interrupted extraction 1.0-3.0min, and recirculation 5-10 time, extraction finishes rear collection raw material and filtrate.
In step (4), ultrasonic power is 50W, and frequency is 40KHz, and microwave power is 70-500W, and microwave frequency is 2450MHz, and the synergistic extraction time is 10-20min.
In step (5), filter membrane aperture is less than 0.15mm.
In step (6), vacuum degree control is at 0.07～0.08MPa, and temperature is controlled at 40～60 ℃.
In step (7), vacuum degree control is at 0.08～0.09MPa, and temperature is controlled at 40～60 ℃.
Preferably bottling while hot in step (8), container is Brown Glass Brown glass bottles and jars only.
Beneficial effect of the present invention: safe and efficient, under the same conditions, compare with extracting method such as ultrasonic extraction, microwave extraction, extraction, Soxhlet extractings, the method extraction time is short, gained pepper oleoresin yield is high, content of piperine is wherein also high compared with additive method, and pungent is sufficient, aromatising flavour is stronger.
Embodiment
Below in conjunction with embodiment, further set forth the present invention:
Embodiment 1
The making method of pepper oleoresin, its raw material is: 10 parts of piper nigrum grains, 95% 400 parts of edible ethanols.
The making method of described pepper oleoresin, comprises the steps:
(1) prepare pepper powder, selecting moisture content is raw material lower than 12% piper nigrum, with pulverizer, is crushed to diameter at 0.50mm;
(2) add solvent, in 10 portions of pepper powders, add 400 part of 95% edible ethanol;
(3) the quick solvent extraction of program supercharging, pressure range is controlled at 6-8bar, adopts room temperature-program supercharging mode, and the pressure extraction time is 1.5min at every turn, interrupted extraction 1.5min, recirculation 5 times, extraction finishes rear collection raw material and filtrate;
(4) ultrasonic-microwave synergistic extraction, ultrasonic power/frequency: 50W/40KHz, microwave power: 70W, microwave frequency: 2450MHz, synergistic extraction 10min;
(5) filter, adopt the naked eyes visibles such as vacuum filtration fast filtering pepper powder, filter membrane aperture is less than 0.15mm, collects filtrate;
(6) desolvation, adopts the concentrated desolvation of vacuum and low temperature rotation, and vacuum degree control is at 0.07～0.08MPa, and temperature is controlled at 40 ℃;
(7) dry, vacuum-drying, vacuum degree control is at 0.08MPa, and temperature is controlled at 50 ℃;
(8) bottling, bottling while hot, container is Brown Glass Brown glass bottles and jars only, sealing, lucifuge, lower than 25 ℃ of storages.
Compare with extracting method such as ultrasonic extraction, microwave extraction, solvent extraction, Soxhlet extracting, thermal backflows, the results are shown in following table:
The different extracting process comparisons of table 1 pepper oleoresin
Embodiment 2
Pepper oleoresin, its raw material is: 10 parts of white pepper grains, 95% 100 parts of edible ethanols.
The making method of described pepper oleoresin, comprises the steps:
(1) prepare pepper powder, selecting moisture content is raw material lower than 12% white pepper, with pulverizer, is crushed to diameter at 0.15mm;
(2) add solvent, in 10 parts of white pepper powders, add 100 part of 95% edible ethanol;
(3) the quick solvent extraction of program supercharging, pressure range is controlled at 6-8bar, adopts room temperature-program supercharging mode, and the pressure extraction time is 2.0min at every turn, interrupted extraction 1.0min, recirculation 10 times, extraction finishes rear collection raw material and filtrate;
(4) ultrasonic-microwave synergistic extraction, ultrasonic power/frequency: 50W/40KHz, microwave power: 300W, microwave frequency: 2450MHz, synergistic extraction 10min;
(5) filter, adopt the naked eyes visibles such as vacuum filtration fast filtering pepper powder, filter membrane aperture is less than 0.15mm, collects filtrate;
(6) desolvation, adopts the concentrated desolvation of vacuum and low temperature rotation, and vacuum degree control is at 0.07～0.08MPa, and temperature is controlled at 40 ℃;
(7) dry, vacuum-drying, vacuum degree control is at 0.08MPa, and temperature is controlled at 50 ℃;
(8) bottling, bottling while hot, container is Brown Glass Brown glass bottles and jars only, sealing, lucifuge, lower than 25 ℃ of storages.
Embodiment 3
Pepper oleoresin, its raw material is: 10 parts of black pepper grains, 60% 500 parts of edible ethanols.
The making method of described pepper oleoresin, comprises the steps:
(1) prepare pepper powder, selecting moisture content is raw material lower than 12% black pepper, with pulverizer, is crushed to diameter at 0.85mm;
(2) add solvent, in 10 parts of black pepper powder, add 500 part of 60% edible ethanol;
(3) the quick solvent extraction of program supercharging, pressure range is controlled at 6-8bar, adopts room temperature-program supercharging mode, and the pressure extraction time is 2.0min at every turn, interrupted extraction 1.0min, recirculation 10 times, extraction finishes rear collection raw material and filtrate;
(4) ultrasonic-microwave synergistic extraction, ultrasonic power/frequency: 50W/40KHz, microwave power: 500W, microwave frequency: 2450MHz, synergistic extraction 20min;
(5) filter, adopt the naked eyes visibles such as vacuum filtration fast filtering pepper powder, filter membrane aperture is less than 0.15mm, collects filtrate;
(6) desolvation, adopts the concentrated desolvation of vacuum and low temperature rotation, and vacuum degree control is at 0.07～0.08MPa, and temperature is controlled at 60 ℃;
(7) dry, vacuum-drying, vacuum degree control is at 0.09MPa, and temperature is controlled at 50 ℃;
(8) bottling, bottling while hot, container is Brown Glass Brown glass bottles and jars only, sealing, lucifuge, lower than 25 ℃ of storages.
Claims (1)
1. the making method of a pepper oleoresin, the quick solvent extraction of employing program supercharging and ultrasonic-microwave synergistic extraction method extract the flavour substances in pepper, after filtration, desolvation, drying process make pepper oleoresin, it is characterized in that, concrete steps are:
(1) prepare pepper powder, choosing white pepper, piper nigrum or black pepper grain is raw material, and the moisture content of described white pepper, black pepper or piper nigrum is lower than 12%; With pulverizer, be ground into diameter at 0.15-0.85mm pepper powder;
(2) add solvent, selecting concentration is that 60%～95% edible ethanol is solvent, adds the solvent of 10-50 part according to 1 part of pepper powder raw material;
(3) the quick solvent extraction of program supercharging, pressure range is controlled at 6-8bar, and the pressure extraction time is 1.0-3.0min at every turn, interrupted extraction 1.0-3.0min, recirculation 5-10 time, extraction finishes rear collection raw material and filtrate;
(4) extraction, adopts ultrasonic-microwave synergistic extraction, and ultrasonic power is 50W, and frequency is 40KHz, and microwave power is 70-500W, and microwave frequency is 2450MHz, and the synergistic extraction time is 10-20min;
(5) filter, adopt vacuum filtration fast filtering pepper powder, filter membrane aperture is less than 0.15mm, collects filtrate;
(6) desolvation, adopts the concentrated desolvation of vacuum rotating, and vacuum degree control is at 0.07～0.08MPa, and temperature is controlled at 40～60 ℃;
(7) dry, adopt vacuum-drying, vacuum degree control is at 0.08～0.09MPa, and temperature is controlled at 40～60 ℃;
(8) bottling while hot, container is Brown Glass Brown glass bottles and jars only, sealing, lucifuge, lower than 25 ℃ of storages.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103610010B (en) * | 2013-11-14 | 2015-06-24 | 扬州大学 | Fabrication method of pepper oleoresin microcapsule |
| CN104263504B (en) * | 2014-10-22 | 2016-08-17 | 江西省粮油科学技术研究所 | A kind of extracting method of smooth bark wood fruit oil |
| CN105454465A (en) * | 2015-12-14 | 2016-04-06 | 长沙理工大学 | Coriander spice flavoring oil and preparation method thereof |
| CN107223943B (en) * | 2017-06-20 | 2021-06-15 | 中国热带农业科学院香料饮料研究所 | Fresh pepper fruit composite sauce and preparation method thereof |
| CN108967994B (en) * | 2018-09-30 | 2022-03-04 | 中国热带农业科学院香料饮料研究所 | Preparation method of pepper flavor substance |
| CN113209662A (en) * | 2021-04-27 | 2021-08-06 | 中国热带农业科学院香料饮料研究所 | Preparation method and application of tsaoko flavor substance |
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| CN102504823A (en) * | 2011-11-08 | 2012-06-20 | 江南大学 | Method for preparing olive phenol natural antioxidant |
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| CN1290730A (en) * | 2000-11-03 | 2001-04-11 | 海南绿田园高新技术发展有限公司 | Process for preparing pepper oil resin |
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