CN106509167A - Production technology for preparing fresh zanthoxylum bungeanum oil by pressing method - Google Patents
Production technology for preparing fresh zanthoxylum bungeanum oil by pressing method Download PDFInfo
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- CN106509167A CN106509167A CN201610980834.2A CN201610980834A CN106509167A CN 106509167 A CN106509167 A CN 106509167A CN 201610980834 A CN201610980834 A CN 201610980834A CN 106509167 A CN106509167 A CN 106509167A
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- pericarpium zanthoxyli
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
- A23D9/04—Working-up
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/007—Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
- A23D9/013—Other fatty acid esters, e.g. phosphatides
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Abstract
The invention discloses a production technology for preparing fresh zanthoxylum bungeanum oil by a pressing method. The production technology comprises the following steps of adding water to zanthoxylum bungeanum raw materials, crushing a mixture of the zanthoxylum bungeanum raw materials and the water to obtain zanthoxylum bungeanum pulp in a physical pressing manner; adding salad oil to the zanthoxylum bungeanum pulp, performing uniform stirring, placing the zanthoxylum bungeanum pulp and the salad oil after being uniformly stirred into an ultrasonic wave reaction tank for soaking, and then performing separation so as to obtain water, crude oil and zanthoxylum bungeanum cake impurities; and performing prefiltration and settling on the crude oil to remove zanthoxylum bungeanum dregs, and then performing rectification and separation to remove moisture so as to obtain high-purity zanthoxylum bungeanum refined oil. According to the production technology disclosed by the invention, fresh zanthoxylum bungeanum is used as a raw material, and a normal-temperature pressing manner is used for extracting the zanthoxylum bungeanum oil, so that the production technology of the zanthoxylum bungeanum oil is optimized, and original natural ingredients and physiological activators in the fresh zanthoxylum bungeanum can be reserved to the maximum extent. The condition that high temperature treatment enables substances of amides, protein and the like in volatile oil to be denatured and lost can be avoided, and the oxidative rancidity of quality of the zanthoxylum bungeanum oil can be effectively controlled; and in the processing technology, a cold pressing method is adopted, so that the extraction time can be shortened, and the economic benefits of products can be increased.
Description
Technical field
The present invention relates to the production technical field of flavoring agent, and in particular to produce the production of fresh zanthoxylum oil to a kind of milling process
Technique.
Background technology
Pericarpium Zanthoxyli (Zanthoxylum bungeanum Maxim.), is Rutaceae, Zanthoxylum machaka or dungarunga.Really
Real rounded, Semen phaseoli radiati size, during fruit maturation, peel takes on a red color or aubergine is red green pepper, and seed, Semen zanthoxyli, is Chinese crude drug, can
Aromatic oil is extracted, is the conventional flavoring agent of family.Pericarpium Zanthoxyli can remove the stink smell of various meats, promote salivation, increase appetite；In right amount
The expansible blood vessel of Pericarpium Zanthoxyli, reduce blood pressure.Fresh Pericarpium Zanthoxyli be difficult preserve, easily brown stain, go mouldy, the resting period is scattered under room temperature only
For 1～2 day, pilling up time was less than 1 day；The low-temp storage time occurred as soon as brown stain less than 5 days, occurred going mouldy within 7 days.Therefore, flower
Green pepper is more, and based on dry product, Jing after high temperature drying, effumability component damages are larger for fresh Pericarpium Zanthoxyli, make dry Pericarpium Zanthoxyli lack fresh Pericarpium Zanthoxyli
Distinctive fragrance.
Cold-squeezing is a kind of new Fructus Zanthoxyli oil extraction process, and normal temperature and pressure, raw material are direct without the need for steaming stir-fry, fresh Pericarpium Zanthoxyli
Jing mechanical expressions, are not required to any chemical reagent and refine, and enter to squeeze temperature for room temperature or slightly above room temperature, generally below 65 DEG C, can
Retain the original natural component of fresh pepper and biological active substanceies to greatest extent, can avoid because high-temperature process is to acyl in volatile oil
The materials such as amine, protein cause degeneration and loss；In processing technique, fresh Pericarpium Zanthoxyli can shorten extraction time using cold-press,
Improve product economy benefit.
The content of the invention
It is an object of the invention to above-mentioned dry Pericarpium Zanthoxyli, the shortcoming of high temperature extraction Fructus Zanthoxyli oil are solved, using above-mentioned cold-squeezing
Extract the advantage of fresh zanthoxylum oil, there is provided one kind can effectively keep fresh pepper peculiar clear with fresh pepper as raw material using cold-squeezing
The Fructus Zanthoxyli oil production technology of fragrant and numb taste.
It is, up to above-mentioned purpose, in one embodiment of the present of invention, to provide the production work that a kind of milling process produces fresh zanthoxylum oil
Skill, comprises the following steps：
(1), the green pepper leaf of fresh Pericarpium Zanthoxyli is extractd, goes to clean after the removal of impurity, obtain Pericarpium Zanthoxyli raw material；
(2), at normal temperatures and pressures, water is added in Pericarpium Zanthoxyli raw material, Pericarpium Zanthoxyli raw material and water are crushed using physical squeezing mode
Mixture obtain Pericarpium Zanthoxyli slurry；
(3), in Pericarpium Zanthoxyli slurry salad oil is added to be placed in enter in ultrasonic response tank and soak and remain a constant speed after stirring
Stirring, the frequency for controlling ultrasound wave are 25kHz～35kHz；Stirring is miscellaneous through isolated water, crude oil and Pericarpium Zanthoxyli cake after finishing
Matter；
(4), detached Pericarpium Zanthoxyli cake impurity is further centrifuged, is settled and isolate crude oil therein；
(5) all of crude oil is removed into zanthoxylum slag through coarse filtration, sedimentation, then moisture is separated off through rectification obtain height
The Pericarpium Zanthoxyli refined oil of purity；
(6), salad oil exchange is added into Fructus Zanthoxyli oil finished product in Pericarpium Zanthoxyli refined oil；
The content of erucic acid of salad oil is 0.05%w/w～1%w/w, and the preparation method of salad oil comprises the following steps：
A, Oleum Brassicae campestriss are warming up to 50 DEG C～60 DEG C, add final concentration of 10%w/w～20% of ammonia spirit to ammonia
W/w, obtains just mixed thing；
B, by first mixed thing stirring and evenly mixing and 60 DEG C～70 DEG C are warming up to, after adding acetic acid 5%～10%, continue stirring 30min
More than, add sodium bicarbonate regulation pH value crude oil is obtained to neutrality；
C, in crude oil temperature is added to be that 80 DEG C～90 DEG C of Klorvess Liquid is followed by stirring and washing, the matter of Klorvess Liquid
Amount fraction is 10%～20%；Klorvess Liquid washing finish after separate oil phase, thereafter in oil phase add temperature be 80 DEG C～
90 DEG C of distilled water is washed, and separates oil phase again；Repeat Klorvess Liquid and distilled water wash 2～3 times, be finally separating
The quintessence oil for arriving；
D, quintessence oil is dried to obtain into salad oil.
One of prioritization scheme as the present invention, in step (2), Pericarpium Zanthoxyli raw material and the weight ratio for adding water are 1：3～5；It is excellent
In selecting step (2), physical squeezing uses pressafiner；More preferably in step (2), the temperature of squeezing is less than 65 DEG C.
One of prioritization scheme as the present invention, the control temperature in step (2) in ultrasonic Treatment immersion process is not high
In 60 DEG C, the time is not less than 30min.
One of prioritization scheme as the present invention, in step (3), Pericarpium Zanthoxyli slurry and the weight ratio of salad oil are 2～3:1.
Device therefor is centrifuged in one of prioritization scheme as the present invention, step (4) for oil-water separator, rotating speed 9000r/
Min, crude oil standing sedimentation 2d at room temperature after centrifugation；Above step secondary centrifuging, sedimentation are repeated, the secondary settlement time is
30d；In step (5), the aperture of filter operation is 120 mesh～150 mesh.
One of prioritization scheme as the present invention, the final concentration of 15%w/w of ammonia in step A；The speed stirred in step C
All 20～the 30rpm of rate.
The production technology that a kind of milling process produces fresh zanthoxylum oil is provided in an alternative embodiment of the invention, including it is following
Step：
(1), the green pepper leaf of fresh Pericarpium Zanthoxyli is extractd, goes to clean after the removal of impurity, obtain Pericarpium Zanthoxyli raw material；
(2), at normal temperatures and pressures, water is added in Pericarpium Zanthoxyli raw material, Pericarpium Zanthoxyli raw material and water are crushed using physical squeezing mode
Mixture obtain Pericarpium Zanthoxyli slurry；
(3) stir after, salad oil and sodium citrate 1%w/w～5%w/w being added in Pericarpium Zanthoxyli slurry, then be placed in ultrasound
Enter stirring of soaking and remain a constant speed in ripple retort, the frequency for controlling ultrasound wave is 25kHz～35kHz；Stirring finish after through
Isolated water, crude oil and Pericarpium Zanthoxyli cake impurity；
(4), detached Pericarpium Zanthoxyli cake impurity is further centrifuged, is settled and isolate crude oil therein；
(5) all of crude oil is removed into zanthoxylum slag through coarse filtration, sedimentation, then moisture is separated off through rectification obtain height
The Pericarpium Zanthoxyli refined oil of purity；
(6), salad oil exchange is added into Fructus Zanthoxyli oil finished product in Pericarpium Zanthoxyli refined oil.
The content of erucic acid of salad oil is 0.05%～1%, and the preparation method of salad oil is comprised the following steps：
A, Oleum Brassicae campestriss are warming up to 50 DEG C～60 DEG C, add final concentration of 10%w/w～20% of ammonia spirit to ammonia
W/w, obtains just mixed thing；
B, by first mixed thing stirring and evenly mixing and 60 DEG C～70 DEG C are warming up to, after adding acetic acid 5%～10%, continue stirring 30min
More than, add sodium bicarbonate regulation pH value crude oil is obtained to neutrality；
C, in crude oil temperature is added to be that 80 DEG C～90 DEG C of Klorvess Liquid is followed by stirring and washing, the matter of Klorvess Liquid
Amount fraction is 10%～20%；Klorvess Liquid washing finish after separate oil phase, thereafter in oil phase add temperature be 80 DEG C～
90 DEG C of distilled water is washed, and separates oil phase again；Repeat Klorvess Liquid and distilled water wash 2～3 times, be finally separating
The quintessence oil for arriving；
D, quintessence oil is dried to obtain into salad oil.
In sum, the present invention has advantages below：
The present invention by the way of room temperature squeezing extracts Fructus Zanthoxyli oil, optimizes the production of Fructus Zanthoxyli oil with fresh pepper as raw material
Technique, can retain the original natural component of fresh pepper and biological active substanceies to greatest extent, can avoid because of high-temperature process pair
In volatile oil, the material such as amide-type, protein causes degeneration and loss, the oxidative rancidity of effective control Pericarpium Zanthoxyli oil quality；Processing work
In skill, cold-press can shorten extraction time, improve product economy benefit.
Specific embodiment
The determinate technological process be given with reference to embodiment, is further explained to the present invention.Implement
In example, technological process is as follows：
(1), the green pepper leaf of fresh Pericarpium Zanthoxyli is extractd, goes to clean after the removal of impurity, obtain Pericarpium Zanthoxyli raw material；
(2), at normal temperatures and pressures, water is added in Pericarpium Zanthoxyli raw material, Pericarpium Zanthoxyli raw material and water are crushed using physical squeezing mode
Mixture obtain Pericarpium Zanthoxyli slurry；
(3), in Pericarpium Zanthoxyli slurry salad oil is added to be placed in enter in ultrasonic response tank and soak and remain a constant speed after stirring
Stirring, the frequency for controlling ultrasound wave are 25kHz～35kHz；Stirring is miscellaneous through isolated water, crude oil and Pericarpium Zanthoxyli cake after finishing
Matter；
(4), detached Pericarpium Zanthoxyli cake impurity is further centrifuged, is settled and isolate crude oil therein；
(5) all of crude oil is removed into zanthoxylum slag through coarse filtration, sedimentation, then moisture is separated off through rectification obtain height
The Pericarpium Zanthoxyli refined oil of purity；
(6), salad oil exchange is added into Fructus Zanthoxyli oil finished product in Pericarpium Zanthoxyli refined oil；
The preparation method of salad oil includes：
A, Oleum Brassicae campestriss are warming up to 50 DEG C～60 DEG C, add final concentration of 10%w/w～20% of ammonia spirit to ammonia
W/w, obtains just mixed thing；
B, by first mixed thing stirring and evenly mixing and 60 DEG C～70 DEG C are warming up to, after adding acetic acid 5%～10%, continue stirring 30min
More than, add sodium bicarbonate regulation pH value crude oil is obtained to neutrality；
C, in crude oil temperature is added to be that 80 DEG C～90 DEG C of Klorvess Liquid is followed by stirring and washing, the matter of Klorvess Liquid
Amount fraction is 10%～20%；Klorvess Liquid washing finish after separate oil phase, thereafter in oil phase add temperature be 80 DEG C～
90 DEG C of distilled water is washed, and separates oil phase again；Repeat Klorvess Liquid and distilled water wash 2～3 times, be finally separating
The quintessence oil for arriving；
D, quintessence oil is dried to obtain into salad oil.
First, impact of the ultrasonic Treatment to active component amide substance result of extraction in fresh pepper
Embodiment 1
Part I：The preparation of raw material
A, Oleum Brassicae campestriss are warming up to 55 DEG C, add the final concentration of 15%w/w of ammonia spirit to ammonia, obtain just mixed thing；
B, by first mixed thing stirring and evenly mixing and 65 DEG C are warming up to, add acetic acid to final mass fraction to be to continue stirring after 8%
45min, adds sodium bicarbonate regulation pH value and obtains crude oil to neutrality；
C, in crude oil temperature is added to be that 85 DEG C of Klorvess Liquid is followed by stirring and washing, the mass fraction of Klorvess Liquid
For 10%；Klorvess Liquid washing separates oil phase after finishing, and adds the distilled water that temperature is 80 DEG C to be washed thereafter in oil phase
Wash, separate oil phase again；Repeat Klorvess Liquid and distilled water wash 3 times, the quintessence oil being finally separating to obtain；The speed of all stirrings
All 20～the 30rpm of rate；
D, quintessence oil drying to water content is obtained into salad oil less than 0.1%w/w, the content of erucic acid of salad oil is 0.5%.
Part II：Prepare Fructus Zanthoxyli oil
(1) sorting
The green pepper leaf of fresh Pericarpium Zanthoxyli is extractd, goes to clean after the removal of impurity, obtain Pericarpium Zanthoxyli raw material.
(2) prepare Pericarpium Zanthoxyli slurry
At normal temperatures and pressures, the water of Pericarpium Zanthoxyli 4 times of weight of raw material is added in Pericarpium Zanthoxyli raw material, to be added water and equipment purification is filtered for Jing
Purified water afterwards, the mixture for crushing Pericarpium Zanthoxyli raw material and water using pressafiner obtain Pericarpium Zanthoxyli slurry, and pressing temperature is 60 DEG C.
(3) add rape salad oil
In Pericarpium Zanthoxyli slurry, add the salad oil of Pericarpium Zanthoxyli slurry weight 1/3rd to stir, be subsequently placed in ultrasonic response tank
Inside enter stirring of soaking and remain a constant speed, the frequency for controlling ultrasound wave is 30kHz；Control temperature in ultrasonic Treatment immersion process
58 DEG C, time 45min.Stir after finishing through isolated water, crude oil and Pericarpium Zanthoxyli cake impurity.
(4) centrifugal sedimentation
Detached Pericarpium Zanthoxyli cake impurity is further centrifuged, is settled and crude oil therein is isolated；Centrifugation device therefor is oil
Water separator, rotating speed 9000r/min, crude oil standing sedimentation 2d at room temperature after centrifugation；Repeat above step secondary centrifuging, sink
Drop, secondary settlement time are 30d.
(5) Pericarpium Zanthoxyli refined oil
All of crude oil is removed into zanthoxylum slag through coarse filtration, sedimentation, then moisture is separated off through rectification obtain high-purity
Pericarpium Zanthoxyli refined oil.Adopt aperture for 120 mesh filter filter centrifugation, sedimentation after crude oil, cross oil strain again adopt sheet frame pressure
Filter is filtered except middle fine impurities of deoiling, 150 mesh of filter cloth aperture, two-layer, 20 DEG C of filtration temperature.
(6) detect
Filter pressed oil is sampled, by volatile ingredient and main constituent in prescriptive procedure detection oil, by class standard
In formulated product, Volatility Levels are to required standard.
(7) fine straining
Further to remove Pericarpium Zanthoxyli well cuts, fine straining before Fructus Zanthoxyli oil fill, 200 mesh of filter opening footpath, 20 DEG C of filtration temperature.
(8) metering filling
After fine straining, institute's oil-producing is high-purity semi-finished product Fructus Zanthoxyli oil, before fill, should be according to consumer group's demand, by fresh zanthoxylum oil
Semi-finished product and rape salad oil are allocated as finished product in proportion；Filling bottle is cleaned up；Accurately measure by product specification, using automatic
Filling machine fill Fructus Zanthoxyli oil；Sealing bottleneck, without damaged lid, special-shaped cover；Accurate location is labelled, without deformation label and crooked mark
Sign；The date of manufacture is sprayed in coding, body specified location.
(9) inspection, vanning, warehouse-in
Using manually by bottle detection case, detection content whether have in including oil foreign body, oil color and luster, oil filling amount,
Airtightness of bottle cap etc.；Qualified products are neatly cased, enough vannings, fill out put the quality certification, joint sealing, record warehouse-in；Substandard product point
Class process.Product is deposited under lucifuge, shady and cool room temperature.
Embodiment 2
Part I：The preparation of raw material
Rape salad oil is prepared using method same as Example 1.
Part II：Prepare Fructus Zanthoxyli oil
(1) sorting
(2) prepare Pericarpium Zanthoxyli slurry
(3) add rape salad oil
In Pericarpium Zanthoxyli slurry, add the salad oil of Pericarpium Zanthoxyli slurry weight 1/3rd to stir, sodium citrate is added to quality point
Number is 2%w/w, is subsequently placed in ultrasonic response tank and enters stirring of soaking and remain a constant speed, and the frequency for controlling ultrasound wave is
30kHz；58 DEG C of control temperature in ultrasonic Treatment immersion process, time 45min.Stirring finish after through isolated water,
Crude oil and Pericarpium Zanthoxyli cake impurity.
(4) centrifugal sedimentation
Detached Pericarpium Zanthoxyli cake impurity is further centrifuged, is settled and crude oil therein is isolated；Centrifugation device therefor is oil
Water separator, rotating speed 9000r/min, crude oil standing sedimentation 2d at room temperature after centrifugation；Repeat above step secondary centrifuging, sink
Drop, secondary settlement time are 30d.
(5) Pericarpium Zanthoxyli refined oil
All of crude oil is removed into zanthoxylum slag through coarse filtration, sedimentation, then moisture is separated off through rectification obtain high-purity
Pericarpium Zanthoxyli refined oil.Adopt aperture for 120 mesh filter filter centrifugation, sedimentation after crude oil, cross oil strain again adopt sheet frame pressure
Filter is filtered except middle fine impurities of deoiling, 150 mesh of filter cloth aperture, two-layer, 20 DEG C of filtration temperature.
Embodiment 3
Part I：The preparation of raw material
Rape salad oil is prepared using method same as Example 1.
Part II：Prepare Fructus Zanthoxyli oil
(1) sorting
(2) prepare Pericarpium Zanthoxyli slurry
(3) add rape salad oil
In Pericarpium Zanthoxyli slurry, add the salad oil of Pericarpium Zanthoxyli slurry weight 1/3rd to stir, sodium citrate is added to quality point
Number is 2% and then stirring 90min.Stir after finishing through isolated water, crude oil and Pericarpium Zanthoxyli cake impurity.
(4) centrifugal sedimentation
Detached Pericarpium Zanthoxyli cake impurity is further centrifuged, is settled and crude oil therein is isolated；Centrifugation device therefor is oil
Water separator, rotating speed 9000r/min, crude oil standing sedimentation 2d at room temperature after centrifugation；Repeat above step secondary centrifuging, sink
Drop, secondary settlement time are 30d.
(5) Pericarpium Zanthoxyli refined oil
All of crude oil is removed into zanthoxylum slag through coarse filtration, sedimentation, then moisture is separated off through rectification obtain high-purity
Pericarpium Zanthoxyli refined oil.Adopt aperture for 120 mesh filter filter centrifugation, sedimentation after crude oil, cross oil strain again adopt sheet frame pressure
Filter is filtered except middle fine impurities of deoiling, 150 mesh of filter cloth aperture, two-layer, 20 DEG C of filtration temperature.
Embodiment 4
Part I：The preparation of raw material
Rape salad oil is prepared using method same as Example 1.
Part II：Prepare Fructus Zanthoxyli oil
(1) sorting
(2) prepare Pericarpium Zanthoxyli slurry
(3) add rape salad oil
The salad oil stirring 90min of Pericarpium Zanthoxyli slurry weight 1/3rd is added in Pericarpium Zanthoxyli slurry.Stir after finishing through separating
Obtain water, crude oil and Pericarpium Zanthoxyli cake impurity.
(4) centrifugal sedimentation
Detached Pericarpium Zanthoxyli cake impurity is further centrifuged, is settled and crude oil therein is isolated；Centrifugation device therefor is oil
Water separator, rotating speed 9000r/min, crude oil standing sedimentation 2d at room temperature after centrifugation；Repeat above step secondary centrifuging, sink
Drop, secondary settlement time are 30d.
(5) Pericarpium Zanthoxyli refined oil
All of crude oil is removed into zanthoxylum slag through coarse filtration, sedimentation, then moisture is separated off through rectification obtain high-purity
Pericarpium Zanthoxyli refined oil.Adopt aperture for 120 mesh filter filter centrifugation, sedimentation after crude oil, cross oil strain again adopt sheet frame pressure
Filter is filtered except middle fine impurities of deoiling, 150 mesh of filter cloth aperture, two-layer, 20 DEG C of filtration temperature.
The Pericarpium Zanthoxyli refined oil for generating out in 1～embodiment of embodiment 4 is surveyed into Fructus Zanthoxyli oil using ultraviolet spectrophotometer method
Middle amide substance content, concrete grammar are as follows：
1) pretreatment：Sample application methanol is extracted into 4h under the conditions of 40 DEG C, lixiviating solution is detected in 3h；
2) the fagaramide class material for preparing HPLC is configured to a series of concentration with methanol as standard substance
Fagaramide solution, its absorbance is surveyed under 254nm, with absorbance as vertical coordinate, correspondence standard sample content be horizontal seat
Mark, makes standard curve.
3) appropriate amount of sample is accurately taken, methanol is added to scale, take supernatant and survey its absorbance at 254nm after centrifugation；In detail
See《Food Additives Used in China》In " ultraviolet spectrophotometer method survey Fructus Zanthoxyli oil in amide substance content ".
Learn through detection, amide substance content respectively 2.14% (ml/g) of 1～embodiment of embodiment 4,
3.98% (ml/g), 1.82% (ml/g), 1.84% (ml/g).As can be seen here, although the technique in embodiment 3 and embodiment 4
It is slightly different, but both is to the extraction ratio of amide constituents in Pericarpium Zanthoxyli and have no significant effect, illustrates that addition sodium citrate can not
It is enough individually to improve dissolution rate of the amide substance in salad oil, but which can be significantly improved when being used in conjunction with ultrasonic technique
Dissolution rate, illustrates that sodium citrate is dissolved with facilitation to the material of the present invention to ultrasound wave.Fragrance ingredient, numb taste in serosity
The materials such as element are soluble in oils and fatss, by the main constituent in rapeseed oil extraction Pericarpium Zanthoxyli.
Ultrasonic Treatment is employed in embodiment 1, embodiment 3 is compared and embodiment 4 is significantly improved dissolution rate, embodiment
2 optimize technique compared with Example 1 after improve the dissolution rate of active component, illustrating in this case can be with ultrasound wave
Handling process cooperates, and synergism is improving the dissolution rate of amide substance.
2nd, impact of the salad oil to Fructus Zanthoxyli oil storage life
Embodiment 5
Part I：The preparation of raw material
A, Oleum Brassicae campestriss are warming up to 60 DEG C, add the final concentration of 185%w/w of ammonia spirit to ammonia, obtain just mixed thing；
B, by first mixed thing stirring and evenly mixing and 68 DEG C are warming up to, add acetic acid to final mass fraction to be to continue stirring after 10%
45min, adds sodium bicarbonate regulation pH value and obtains crude oil to neutrality；
C, in crude oil temperature is added to be that 90 DEG C of Klorvess Liquid is followed by stirring and washing, the mass fraction of Klorvess Liquid
For 10%；Klorvess Liquid washing separates oil phase after finishing, and adds the distilled water that temperature is 85 DEG C to be washed thereafter in oil phase
Wash, separate oil phase again；Repeat Klorvess Liquid and distilled water wash 3 times, the quintessence oil being finally separating to obtain；The speed of all stirrings
The all 30rpm of rate；
D, quintessence oil drying to water content is obtained into salad oil less than 0.1%w/w, the content of erucic acid of salad oil is 0.48%.
Part II：Prepare Fructus Zanthoxyli oil
(1) sorting
The green pepper leaf of fresh Pericarpium Zanthoxyli is extractd, goes to clean after the removal of impurity, obtain Pericarpium Zanthoxyli raw material.
(2) prepare Pericarpium Zanthoxyli slurry
At normal temperatures and pressures, the water of Pericarpium Zanthoxyli 4 times of weight of raw material is added in Pericarpium Zanthoxyli raw material, to be added water and equipment purification is filtered for Jing
Purified water afterwards, the mixture for crushing Pericarpium Zanthoxyli raw material and water using pressafiner obtain Pericarpium Zanthoxyli slurry, and pressing temperature is 60 DEG C.
(3) add rape salad oil
In Pericarpium Zanthoxyli slurry, add the salad oil of Pericarpium Zanthoxyli slurry weight 1/3rd to stir, be subsequently placed in ultrasonic response tank
Inside enter stirring of soaking and remain a constant speed, the frequency for controlling ultrasound wave is 25kHz；Control temperature in ultrasonic Treatment immersion process
60 DEG C, time 40min.Stir after finishing through isolated water, crude oil and Pericarpium Zanthoxyli cake impurity.
(4) centrifugal sedimentation
Detached Pericarpium Zanthoxyli cake impurity is further centrifuged, is settled and crude oil therein is isolated；Centrifugation device therefor is oil
Water separator, rotating speed 9000r/min, crude oil standing sedimentation 2d at room temperature after centrifugation；Repeat above step secondary centrifuging, sink
Drop, secondary settlement time are 30d.
(5) Pericarpium Zanthoxyli refined oil
All of crude oil is removed into zanthoxylum slag through coarse filtration, sedimentation, then moisture is separated off through rectification obtain high-purity
Pericarpium Zanthoxyli refined oil.Adopt aperture for 120 mesh filter filter centrifugation, sedimentation after crude oil, cross oil strain again adopt sheet frame pressure
Filter is filtered except middle fine impurities of deoiling, 150 mesh of filter cloth aperture, two-layer, 20 DEG C of filtration temperature.
(6) detect
Filter pressed oil is sampled, by volatile ingredient and main constituent in prescriptive procedure detection oil, by class standard
In formulated product, Volatility Levels are to required standard.
(7) fine straining
Further to remove Pericarpium Zanthoxyli well cuts, fine straining before Fructus Zanthoxyli oil fill, 200 mesh of filter opening footpath, 20 DEG C of filtration temperature.
(8) metering filling
After fine straining, institute's oil-producing is high-purity semi-finished product Fructus Zanthoxyli oil, before fill, should be according to consumer group's demand, by fresh zanthoxylum oil
Semi-finished product and rape salad oil are allocated as finished product in proportion；Filling bottle is cleaned up；Accurately measure by product specification, using automatic
Filling machine fill Fructus Zanthoxyli oil；Sealing bottleneck, without damaged lid, special-shaped cover；Accurate location is labelled, without deformation label and crooked mark
Sign；The date of manufacture is sprayed in coding, body specified location.
(9) inspection, vanning, warehouse-in
Using manually by bottle detection case, detection content whether have in including oil foreign body, oil color and luster, oil filling amount,
Airtightness of bottle cap etc.；Qualified products are neatly cased, enough vannings, fill out put the quality certification, joint sealing, record warehouse-in；Substandard product point
Class process.Product is deposited under lucifuge, shady and cool room temperature.
Embodiment 6
(1) sorting
The green pepper leaf of fresh Pericarpium Zanthoxyli is extractd, goes to clean after the removal of impurity, obtain Pericarpium Zanthoxyli raw material.
(2) prepare Pericarpium Zanthoxyli slurry
At normal temperatures and pressures, the water of Pericarpium Zanthoxyli 4 times of weight of raw material is added in Pericarpium Zanthoxyli raw material, to be added water and equipment purification is filtered for Jing
Purified water afterwards, the mixture for crushing Pericarpium Zanthoxyli raw material and water using pressafiner obtain Pericarpium Zanthoxyli slurry, and pressing temperature is 60 DEG C.
(3) add rape salad oil
In Pericarpium Zanthoxyli slurry, add the salad oil of Pericarpium Zanthoxyli slurry weight 1/3rd to stir, be subsequently placed in ultrasonic response tank
Inside enter stirring of soaking and remain a constant speed, the frequency for controlling ultrasound wave is 25kHz；Control temperature in ultrasonic Treatment immersion process
60 DEG C, time 40min.Stir after finishing through isolated water, crude oil and Pericarpium Zanthoxyli cake impurity.
(4) centrifugal sedimentation
Detached Pericarpium Zanthoxyli cake impurity is further centrifuged, is settled and crude oil therein is isolated；Centrifugation device therefor is oil
Water separator, rotating speed 9000r/min, crude oil standing sedimentation 2d at room temperature after centrifugation；Repeat above step secondary centrifuging, sink
Drop, secondary settlement time are 30d.
(5) Pericarpium Zanthoxyli refined oil
All of crude oil is removed into zanthoxylum slag through coarse filtration, sedimentation, then moisture is separated off through rectification obtain high-purity
Pericarpium Zanthoxyli refined oil.Adopt aperture for 120 mesh filter filter centrifugation, sedimentation after crude oil, cross oil strain again adopt sheet frame pressure
Filter is filtered except middle fine impurities of deoiling, 150 mesh of filter cloth aperture, two-layer, 20 DEG C of filtration temperature.
(6) detect
(7) fine straining
Further to remove Pericarpium Zanthoxyli well cuts, fine straining before Fructus Zanthoxyli oil fill, 200 mesh of filter opening footpath, 20 DEG C of filtration temperature.
(8) metering filling
6～embodiment of embodiment 10 adopts experiment parameter same as Example 5 and technique, while in order to verify Semen Allii Tuberosi color
Impact of the oil to the shelf-life is drawn, the rape salad oil for selecting content of erucic acid different is used as salad oil raw material, wherein 6～reality of embodiment
Apply the content of erucic acid such as following table of salad oil in example 10.
Table 1：Content of erucic acid in different embodiments
| Embodiment is numbered | Content of erucic acid (w/w) |
| Embodiment 6 | 1% |
| Embodiment 7 | 1.5% |
| Embodiment 8 | 2% |
| Embodiment 9 | 3% |
| Embodiment 10 | 4% |
The present invention verifies the Fructus Zanthoxyli oil finished product for the preparing putrid and deteriorated time under conditions of accelerated test；During test
For open environment, actual conditions is as follows：
Temperature：60℃；Oxygen concentration：30%；Air humidity：80%RH；Intensity of illumination：3000LX.
The oil of Fructus Zanthoxyli oil can evaluate its degree of spoilage, oils and fatss by acid value, peroxide value, carbonyl valency, TBA values etc.
After corruption, its corresponding index can be raised, therefore the present invention evaluates the spoilage rate of Fructus Zanthoxyli oil by acid value and peroxide value,
And then judge the relative mode for being conducive to preserving.The detection mode of acid value and peroxide value can be using national examination criteria
It is middle by the way of, the present invention adopt detection method it is as follows.
1st, the measure of acid value
1.1 reagent：
(1) 0.1mol/L standard potassium hydroxides solution；
(2) neutral diethylether-ethanol (2:1) mix reagent；Neutrality is titrated to 0.1mol/L aqueous slkalis before use；
(3) indicator：1% ethanolic phenolphthalein solution.
1.2 operational approach
Mixed solution 50ml dissolvings are added in weighing sample 5g injection conical flasks, 3 drop phenolphthalein indicators is added, is used
0.1mol/L alkali-titrations do not disappear in 30s to there is blush, write down the alkali liquor milliliter number of consumption, and parallel titration takes for three times
Meansigma methodss.
2nd, the measure of peroxide value
2.1 reagents and solution
Saturated solution of potassium iodide；
Chloroform glacial acetic acid mixed liquor；
0.01mol/L sodium thiosulfate standard solutions；
Starch reagent.
2.2 assay method
Weighing 5g samples claims standard to 0.0002g in iodine flask, plus 30ml chloroform glacial acetic acid mixed liquors make sample complete
CL.1ml saturated solution of potassium iodide is added closely to be stoppered bottle cap and gently shake 0.5min and then place 3min in the dark.
Take out plus 100ml water shakes up and indigo plant is titrated to by indicator 0.01mol/L sodium thiosulfate standard solution of starch test solution immediately
Decoloration is terminal.Do blank assay simultaneously.
3rd, test experience result such as following table
Table 2：Testing result
By above-mentioned testing result, with reference to other contrast tests that the present invention does, inventor is had found when content of erucic acid exceedes
After 1%, the preservation quality of meeting appreciable impact oils and fatss, in the corrupt speed of identical holding time internal oxidition faster, within 1%
Corrupt speed substantially reduce, the substantially content onrelevant with erucic acid.Embodiment 6 and do not contain erucic acid embodiment in carry out
After control, under same time and the same terms, both acid values and peroxide value testing result are close to, not poor with significance
It is different.Meanwhile, after more than 1%, even if the content of erucic acid increases, spoilage rate is also no to be accelerated with the increase of content of erucic acid,
But with 1% or so as critical point, improve more than corrupt efficiency after the critical point.Simultaneously as the process of erucic acid is also needs
Other technique, therefore in the case where production cost is not increased, selection is less than the Fructus Zanthoxyli oil of 1% content of erucic acid in storage life
Substantially preferably, and can also have good economy.
Claims (10)
1. a kind of milling process produces the production technology of fresh zanthoxylum oil, comprises the following steps：
（1）, the green pepper leaf of fresh Pericarpium Zanthoxyli extractd, goes to clean after the removal of impurity, obtain Pericarpium Zanthoxyli raw material；
（2）, at normal temperatures and pressures, add water in Pericarpium Zanthoxyli raw material, the mixed of Pericarpium Zanthoxyli raw material and water crushed using physical squeezing mode
Compound obtains Pericarpium Zanthoxyli slurry；
（3）, in Pericarpium Zanthoxyli slurry add salad oil to be placed in ultrasonic response tank and enter stirring of soaking and remain a constant speed after stirring,
The frequency for controlling ultrasound wave is 25kHz ~ 35kHz；Stir after finishing through isolated water, crude oil and Pericarpium Zanthoxyli cake impurity；
（4）, detached Pericarpium Zanthoxyli cake impurity is further centrifuged, settled and crude oil therein is isolated；
（5）, all of crude oil removed zanthoxylum slag, then is separated off moisture through rectification and obtains high-purity through coarse filtration, sedimentation
Pericarpium Zanthoxyli refined oil；
（6）, in Pericarpium Zanthoxyli refined oil add salad oil exchange into Fructus Zanthoxyli oil finished product；
The content of erucic acid of the salad oil is 0.05%w/w ~ 1%w/w, and the preparation method of salad oil comprises the following steps：
A, Oleum Brassicae campestriss are warming up to 50 DEG C ~ 60 DEG C, add the final concentration of 10%w/w ~ 20%w/w of ammonia spirit to ammonia, obtain
Thing is mixed just；
B, by first mixed thing stirring and evenly mixing and 60 DEG C ~ 70 DEG C are warming up to, after adding acetic acid 5% ~ 10%, continue stirring more than 30min, then
Add sodium bicarbonate to adjust pH value crude oil is obtained to neutrality；
C, in crude oil temperature is added to be followed by stirring and washing for 80 DEG C ~ 90 DEG C of Klorvess Liquid, the quality point of Klorvess Liquid
Number is 10% ~ 20%；Klorvess Liquid washing separates oil phase after finishing, and in oil phase, addition temperature is 80 DEG C ~ 90 DEG C of steaming thereafter
Distilled water is washed, and separates oil phase again；Repeat Klorvess Liquid and distilled water wash 2 ~ 3 times, the quintessence oil being finally separating to obtain；
D, quintessence oil is dried to obtain into salad oil.
2. production technology as claimed in claim 1, it is characterised in that：The step（2）Middle Pericarpium Zanthoxyli raw material and the weight for adding water
Amount is than being 1：3~5.
3. production technology as claimed in claim 1, it is characterised in that：The step（2）Middle physical squeezing uses spiral
Squeezer.
4. production technology as claimed in claim 1, it is characterised in that：The step（2）The temperature of middle squeezing is less than 65 DEG C.
5. production technology as claimed in claim 1, it is characterised in that：The step（2）In middle ultrasonic Treatment immersion process
Not higher than 60 DEG C of control temperature, the time is not less than 30min.
6. production technology as claimed in claim 1, it is characterised in that：The step（3）The weight of middle Pericarpium Zanthoxyli slurry and salad oil
Than for 2 ~ 3:1.
7. production technology as claimed in claim 1, it is characterised in that：The step（4）Middle centrifugation device therefor is profit point
Disembark, rotating speed 9000r/min, crude oil standing sedimentation 2d at room temperature after centrifugation；Above step secondary centrifuging, sedimentation are repeated,
The secondary settlement time is 30d.
8. production technology as claimed in claim 1, it is characterised in that：The step（5）The aperture of middle filter operation is 120 mesh
~ 150 mesh.
9. production technology as claimed in claim 1, it is characterised in that：The final concentration of 15%w/w of ammonia in step A.
10. production technology as claimed in claim 1, it is characterised in that：The speed that stirs in step C is all 20 ~
30rpm。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106889187A (en) * | 2017-03-27 | 2017-06-27 | 陕西司马迁旅游文化（集团）有限公司 | A kind of Yoghourt containing Japan pepper essential oil and preparation method thereof |
| CN107502446A (en) * | 2017-10-18 | 2017-12-22 | 湖南大三湘油茶生态产业有限公司 | Camellia oleifera fruit split-phase process |
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| CN109233998A (en) * | 2018-09-26 | 2019-01-18 | 四川省汉源大自然有限公司 | A kind of extraction process of Zanthoxylum essential oil |
| CN110003979A (en) * | 2019-05-17 | 2019-07-12 | 卓士鸿 | The method that fresh Chinese prickly ash extracts pure Zanthoxylum essential oil |
| CN110628503A (en) * | 2019-11-15 | 2019-12-31 | 贵州土司农业发展有限公司 | Processing method for preparing fresh zanthoxylum oil by squeezing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106889187A (en) * | 2017-03-27 | 2017-06-27 | 陕西司马迁旅游文化（集团）有限公司 | A kind of Yoghourt containing Japan pepper essential oil and preparation method thereof |
| CN107502446A (en) * | 2017-10-18 | 2017-12-22 | 湖南大三湘油茶生态产业有限公司 | Camellia oleifera fruit split-phase process |
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| CN109233998A (en) * | 2018-09-26 | 2019-01-18 | 四川省汉源大自然有限公司 | A kind of extraction process of Zanthoxylum essential oil |
| CN110003979A (en) * | 2019-05-17 | 2019-07-12 | 卓士鸿 | The method that fresh Chinese prickly ash extracts pure Zanthoxylum essential oil |
| CN110628503A (en) * | 2019-11-15 | 2019-12-31 | 贵州土司农业发展有限公司 | Processing method for preparing fresh zanthoxylum oil by squeezing method |
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| CN113142314A (en) * | 2021-03-05 | 2021-07-23 | 四川五丰黎红食品有限公司 | Zanthoxylum oil cake meal resin microcapsule and preparation method thereof |
| CN113755236A (en) * | 2021-08-16 | 2021-12-07 | 河北法曼食品科技有限公司 | Rattan pepper oil with delicious taste and natural and mellow fragrance, and preparation method and application thereof |
| CN114410379A (en) * | 2021-12-17 | 2022-04-29 | 太仓市宝马油脂设备有限公司 | Preparation process of low-temperature cold-pressed original-fragrance garlic fruit oil |
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