CN101591587B - Method for extracting onion essential oil through ultrahigh pressure regulation of alliinase reaction - Google Patents
Method for extracting onion essential oil through ultrahigh pressure regulation of alliinase reaction Download PDFInfo
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- CN101591587B CN101591587B CN200910031284XA CN200910031284A CN101591587B CN 101591587 B CN101591587 B CN 101591587B CN 200910031284X A CN200910031284X A CN 200910031284XA CN 200910031284 A CN200910031284 A CN 200910031284A CN 101591587 B CN101591587 B CN 101591587B
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Abstract
The invention discloses a method for extracting onion essential oil through ultrahigh pressure regulation of alliinase reaction, and belongs to fine and deep processing technology for farm products. The method is carried out according to the following steps: (1) pretreating onion under ultrahigh pressure; (2) preparing onion alliin solution; (3) preparing onion alliinase solution; (4) catalyzing alliinase zymolysis reaction under the ultrahigh voltage; and (5) decompressing water vapor to distill and extract the onion essential oil. The method is easier to control the production process, thereby improving the yield and the quality of the onion essential oil. Under the process condition, the yield of the onion essential oil is between 0.43 and 0.47 percent. The quality of the essential oil and the content of active substances are also improved; and the essential oil has wide market development prospect.
Description
Technical field
The invention belongs to agricultural-food intensive processing technology, relate to a kind of method of high efficiency extraction onion essential oil.
Background technology
Onion (Allium cepa L.) has another name called Onion, onion, round onions, belongs to the Liliaceae allium, is worldwide vegetables.Contain multiple nutritional components and physiologically active substance, contain abundant vitamin A, B in the fresh onion
1, B
2, C, mineral elements such as the copper of nicotinic acid, pantothenic acid and calcium, phosphorus and trace, iron, zinc, manganese, iodine.In addition, also containing volatile oil in the onion, mainly is sulfocompound, comprises mercaptan, thioether, dimethyl disulphide etc.These compounds have constituted distinctive local flavor of onion and physiological function, are one of focuses of at present the onion physiologically active ingredient being studied.The purposes of onion powder mainly contains: (1) functional seasonings.Along with the rapid rising of leisure, ready-to-eat, onion powder is as main non-harmful foodstuff additive, and its demand increases sharply, because its extraction process complicacy and yield are low, makes it on market, be in the state that supply falls short of demand.(2.) raw material of medicine and composition.Onion powder has pharmacological effects such as sterilization, reducing blood-fat, hypoglycemic, decreasing cholesterol, anti-oxidant, asthma, prevention and inhibition cancer, and many in the world countries have classified it as the pharmaceutical raw material and the composition of reducing blood-fat, preventing cancer.(3) makeup and functional food additives.The bacteriostasis of onion powder is stronger than other general plant.Sterilised products such as the oral liquid of processing based on the bacteriostatic action of onion powder, capsule, the effect with some Mycophyta diseases of prevention.
The method of extracting about onion powder at present mainly contains water vapour distillation method and supercritical carbon dioxide extraction method.At application number is to have adopted the reduced steam distillation and extraction method in 01113639.1 " a kind of process for extracting of onion powder " patent: onion is pulverized dry (30～50 ℃); Distillation gets onion essential oil after reclaim organic solvent under 55～60 ℃, the condition of 3～12kpa; Its impurity that exists in earlier stage can't effectively separate; And allinase enzyme digestion reaction efficient is also lower, alliin is reacted more fully generate unsaturated sulfocompound isoreactivity material.In application number 200410064680.X " a kind of method of extracting onion powder " patent, adopted supercritical carbon dioxide extraction method: onion is dry, broken back adopt supercritical carbon dioxide extraction (38 ℃, 19Mpa, 150kg/h) onion essential oil; This method is only carried out broken pre-treatment to onion; Can not make its precursor be converted into active substance well; And the supercritical extraction complicated operation, influence factor is many and be difficult to control.Present method is at first separated alliin and allinase from onion; Can extract and obtain the higher alliin reaction substrate of purity; Adopt the reaction of ultrahigh pressure regulation allinase catalysis alliin, reaction process is effectively controlled, help control and improve product quality; The reaction product effective constituent that obtains is high, steady quality.
Summary of the invention
The purpose of this invention is to provide a kind of through ultrahigh pressure regulation allinase enzyme digestion reaction and adopt the method for reduced steam distillation extraction onion essential oil; The active substance loss that exists with the solution prior art is big; Reaction process is wayward, problems such as unstable product quality.Technical scheme of the present invention is following:
(1) raw material is handled
Take by weighing a certain amount of onion and pack in the special-purpose bag of ultra-high voltage, put into pressure chamber after the vacuum-sealing, at pressure 600～660Mpa, carry out uhp treatment under the condition of time 5～15min, passivation allinase activity is to improve the extracted amount of alliin.Taking-up places under-20 ℃ of environment subsequent use.
(2) extraction of onion alliin solution
Methyl alcohol, chloroform, water are made into the mixed system (being called for short MCW) of certain volume in 12: 5: 3 ratio, take by weighing onion that a certain amount of uhp treatment crosses behind the mixing and put into and wherein soak 2h.Then onion being taken out places 80% ethanolic soln to soak 2h; (volume ratio 9: the 11) mixed solution that adds chloroform isopyknic and water in the MCW extracting solution after taking out onion with it; Standing demix behind the vibration mixing in separating funnel; Get the phase methanol/water solution, add again after 80% alcohol extraction liquid mixes, in rotatory evaporator, be evaporated to certain volume; With 0.01mol/L pH7.5 phosphoric acid buffer dilution constant volume, get onion alliin solution then.
(3) preparation of onion allinase solution
Take by weighing the certain quantity of fresh onion, add ready-formed 0.01mol/L pH7.5 phosphoric acid buffer, tissue mashing machine smashs after-filtration, centrifugal (5000r/min to pieces; 20min, 4 ℃), get supernatant after centrifugal and add 35% ammoniumsulphate soln; Leave standstill 30min after stirring; Centrifugal (10000r/min, 20min, 4 ℃) remove foreigh protein removing; Get supernatant and add 65% ammoniumsulphate soln, mix and be placed on 4 ℃ and place centrifugal (10000r/min, 20min, 4 ℃) behind the 30min; Get deposition with the phosphoric acid buffer of 0.01mol/L pH7.5 dilution constant volume, collect dialyzate after the dialysis 4 times down for 0～4 ℃ in the dialysis tubing of packing into, dilute constant volume, get onion allinase liquid with 0.01mol/L pH7.5 phosphoric acid buffer.
(4) enzymic catalytic reaction extracts onion essential oil
Alliin solution that extracts and allinase solution are mixed with volume ratio at 4: 1; Under the condition of pH6.6, pressure 150～200Mpa, 35～45 ℃ of temperature, dwell time 20～40min; In pressure chamber, carry out enzymic catalytic reaction; This reaction can improve the amount of enzymic activity and product, makes reaction process have controllability, can guarantee the effective constituent and the quality of reaction product.Reaction product adopts reduced steam distillation extraction (distillation vacuum tightness 6～8kpa, extraction time 4～5h adds proper amount of sodium chloride solution) to make onion essential oil.
Present method advantage:
1. present method is at first separated alliin and allinase from onion, has avoided the interference of impurity and residual; Adopt the reaction of ultrahigh pressure regulation allinase catalysis alliin, improved the efficient of reaction, make the alliin substrate more fully be converted into active substance, improved the yield and the quality of onion powder, yield is 0.43～0.47%, and its pungency is little, and mouthfeel is gentle.
2. the onion of equal in quality (1kg), the yield of present method gained onion powder is higher, (GC-MS) detects its activeconstituents through gas chromatography-mass spectrum, with other method gained result relatively like following table:
Last table explanation present method gained onion essential oil active substance destroys less.Do not detect pungency composition thiomethyl alcohol class material in present method gained onion powder, then two kinds of methods reach 0.41% and 0.20% respectively, explain that its quality is softer, more are prone to accepted by the human consumer.
Description of drawings
Fig. 1 extracting onion essential oil through ultrahigh pressure regulation of alliinase reaction process flow sheet.
Embodiment
Embodiment 1
1. raw material is handled: the purple skin onion of choosing 0.75kg is respectively charged in the special-purpose bag of ultra-high voltage for three parts and carries out uhp treatment (pressure 660Mpa, time 5min), and taking-up places under-20 ℃ of environment subsequent use.
2. the extraction of onion alliin:
Methyl alcohol, chloroform, water are made into 1000mL mixed system (being called for short MCW) in 12: 5: 3 ratio, and the onion that behind the mixing uhp treatment is crossed is put into wherein, places to soak 2h under-20 ℃ of low temperature.Then onion is taken out and place 80% alcohol solution dipping 2h; Add about 450mL chloroform and 550mL water in the MCW extracting solution after taking out onion; Standing demix behind the vibration mixing in separating funnel; Get the phase methanol/water solution, after the adding alcohol extraction liquid mixes, in rotatory evaporator, be evaporated to 500mL (50 ℃); With 0.01mol/L pH7.5 phosphoric acid buffer dilution constant volume, obtain onion alliin solution 1000mL then.
3. the preparation of the allinase liquid of onion:
Take by weighing three parts of the fresh onions of 0.25kg, each adds the phosphoric acid buffer 500mL of 0.01mol/L pH7.5, and tissue mashing machine smashs after-filtration, centrifugal (5000r/min to pieces; 20min, 4 ℃), get the ammoniumsulphate soln of supernatant adding 35%; Centrifugal (10000r/min, 20min, 4 ℃) remove foreigh protein removing after mixing placement 30min; Get supernatant and add 65% ammoniumsulphate soln, mix and place centrifugal (10000r/min, 20min behind the 30min; 4 ℃), get deposition with the phosphoric acid buffer of pH7.5 dilution constant volume 250mL, dialyse down and collect dialyzate (3h changes primary water) after 4 times for 0-4 ℃ in the dialysis tubing of packing into; Phosphoric acid buffer dilution with pH7.5 is settled to 250mL again, obtains onion allinase liquid.
4. enzymic catalytic reaction extracts onion essential oil
1000mL alliin solution that extracts and 250mL allinase liquid are mixed, in pH6.6, pressure 150Mpa; 35 ℃ of hydrolysis temperatures; Under the condition of enzymolysis time 20min, in pressure chamber, carry out enzymic catalytic reaction, reaction finishes the back and adopts reduced steam distillation technique (distillation vacuum tightness 7kpa; Extraction time 4.5h, sodium-chlor addition are 90g/1000mL) extract onion essential oil.The onion essential oil yield of method extraction is 0.47% thus.
Embodiment 2
Raw material is handled: the silver skin onion of choosing 0.75kg is respectively charged in the special-purpose bag of ultra-high voltage for three parts and carries out uhp treatment (processing pressure 630Mpa, time 10min), takes out to place-20 ℃ of environment subsequent use.
The preparation of the allinase liquid of onion and the extraction of onion alliin are with embodiment one.
Enzymic catalytic reaction extracts onion essential oil
1000mL alliin solution that extracts and 250mL allinase solution are mixed, at pH6.6, pressure 180MPa; 40 ℃ of hydrolysis temperatures; Under the condition of enzymolysis time 30min, in pressure chamber, carry out enzymic catalytic reaction, reaction finishes the back and adopts reduced steam distillation technique (distillation vacuum tightness 6kPa; Extraction time 5h, sodium-chlor addition are 80g/1000mL) extract onion essential oil.The onion essential oil yield of method extraction is 0.45% thus.
Embodiment 3
Raw material is handled: the yellow onion of choosing 0.75kg is respectively charged in the special-purpose bag of ultra-high voltage for three parts and carries out uhp treatment (processing pressure 600Mpa, time 15min), takes out to place-20 ℃ of environment subsequent use.
The preparation of the allinase liquid of onion and the extraction of onion alliin are with embodiment one.
Enzymic catalytic reaction extracts onion essential oil
1000mL alliin solution that extracts and 250mL allinase liquid are mixed, at pH6.6, pressure 200MPa; 45 ℃ of hydrolysis temperatures; Under the condition of enzymolysis time 40min, in pressure chamber, carry out enzymic catalytic reaction, reaction finishes the back and adopts reduced steam distillation technique (distillation vacuum tightness 8kPa; Extraction time 4h, sodium-chlor addition are 70g/1000mL) extract onion essential oil.The onion essential oil yield of method extraction is 0.43% thus.
Claims (1)
1. the method for an extracting onion essential oil through ultrahigh pressure regulation of alliinase reaction is characterized in that carrying out according to following step:
(1) raw material is handled:
Take by weighing a certain amount of onion and pack in the special-purpose bag of ultra-high voltage, put into pressure chamber after the vacuum-sealing,, carry out uhp treatment under the condition of time 5～15min at pressure 600～660MPa, take out place under-20 ℃ of environment subsequent use;
(2) extraction of onion alliin solution:
Methyl alcohol, chloroform, water are made into the mixed extract of certain volume in 12: 5: 3 ratio, take by weighing onion that a certain amount of uhp treatment crosses behind the mixing and put into and wherein soak 2h; Then onion being taken out places 80% ethanolic soln to soak 2h; The mixed solution that adds 9: 11 chloroform of volume ratio isopyknic and water in the mixed extract after taking out onion with it; Standing demix behind the vibration mixing in separating funnel; Get the phase methanol/water solution, add again after 80% alcohol extraction liquid mixes, in rotatory evaporator, be evaporated to certain volume; With 0.01mol/L pH7.5 phosphoric acid buffer dilution constant volume, get onion alliin solution then;
(3) preparation of onion allinase solution:
Take by weighing the certain quantity of fresh onion, add ready-formed 0.01mol/L pH7.5 phosphoric acid buffer, tissue mashing machine smashs after-filtration, 5000r/min to pieces; 20min, 4 ℃ are centrifugal, get supernatant after centrifugal and add 35% ammoniumsulphate soln; Leave standstill 30min after stirring; 10000r/min, 20min, 4 ℃ of centrifugal foreigh protein removings that remove; Get supernatant and add 65% ammoniumsulphate soln, mix be placed on 4 ℃ place 30min after, 10000r/min, 20min, 4 ℃ are centrifugal; Get deposition with the phosphoric acid buffer of 0.01mol/L pH7.5 dilution constant volume, collect dialyzate after the dialysis 4 times down for 0～4 ℃ in the dialysis tubing of packing into, dilute constant volume, get onion allinase liquid with 0.01mol/L pH7.5 phosphoric acid buffer;
(4) enzymic catalytic reaction extracts onion essential oil:
Alliin solution that extracts and allinase solution are mixed with volume ratio at 4: 1; Under the condition of pH6.6, pressure 150～200MPa, 35～45 ℃ of temperature, dwell time 20～40min; In pressure chamber, carry out enzymic catalytic reaction, reaction product adopts the reduced steam distillation extraction to make onion essential oil, and reduced steam distillatory condition is distillation vacuum tightness 6～8kpa; Extraction time 4～5h adds proper amount of sodium chloride solution.
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| CN101985578B (en) * | 2010-10-30 | 2013-02-06 | 暨南大学 | Method for improving garlic oil yield |
| CN103160558B (en) * | 2011-12-13 | 2014-10-08 | 中国农业科学院农产品加工研究所 | Method for preparing lactalbumin hydrolysate |
| TWI494063B (en) * | 2013-01-24 | 2015-08-01 | Kee Fresh & Safe Foodtech Co Ltd | Method of combining pressure and enzyme to extract hydrolysate of non-animal-derived composition |
| CN104087627A (en) * | 2014-07-29 | 2014-10-08 | 江南大学 | Method for preparing gram-level high-purity natural thiosulfinate |
| CN104127354B (en) * | 2014-08-06 | 2016-08-17 | 阎昭良 | The onion essential oil composition for oral cavity of preventing pharyngitis and periodontitis |
| CN104277915A (en) * | 2014-09-25 | 2015-01-14 | 齐鲁工业大学 | Method for extracting peony essential oil from peony |
| CN104818255A (en) * | 2015-05-25 | 2015-08-05 | 安徽省怀远县华夏药械有限责任公司 | Method for extracting scallion enzyme from scallion stalk |
| CN109609272A (en) * | 2018-11-23 | 2019-04-12 | 盐城工学院 | A kind of extracting method for the galic essential oil reducing cholesterol micella solubility |
| MX2020014291A (en) * | 2020-12-18 | 2022-06-20 | Jose Luis Escobedo Embriz | Alcoholic extract of onion bulbs (allium spp.) and its extraction method. |
| CN114836485B (en) * | 2022-04-19 | 2023-12-05 | 齐鲁工业大学 | Method for extracting and separating ajoene from garlic |
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| CN1320387A (en) * | 2001-04-25 | 2001-11-07 | 潘见 | Process for preparing deodourized garlic cloves |
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| CN1320387A (en) * | 2001-04-25 | 2001-11-07 | 潘见 | Process for preparing deodourized garlic cloves |
Non-Patent Citations (3)
| Title |
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| JP昭59-196064A 1984.11.07 |
| JP特开2009-22305A 2009.02.05 |
| 江霆等.温度协同超高压处理对洋葱的蒜氨酸酶的影响.《食品工业》.2008,(第2期),17-19. * |
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