CN106643006A - Freezing and drying preparation method and application of pomelo fruits - Google Patents
Freezing and drying preparation method and application of pomelo fruits Download PDFInfo
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- CN106643006A CN106643006A CN201611223739.4A CN201611223739A CN106643006A CN 106643006 A CN106643006 A CN 106643006A CN 201611223739 A CN201611223739 A CN 201611223739A CN 106643006 A CN106643006 A CN 106643006A
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
- F26B5/06—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/75—Rutaceae (Rue family)
- A61K36/752—Citrus, e.g. lime, orange or lemon
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B1/00—Preliminary treatment of solid materials or objects to facilitate drying, e.g. mixing or backmixing the materials to be dried with predominantly dry solids
- F26B1/005—Preliminary treatment of solid materials or objects to facilitate drying, e.g. mixing or backmixing the materials to be dried with predominantly dry solids by means of disintegrating, e.g. crushing, shredding, milling the materials to be dried
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
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Abstract
The invention discloses a freezing and drying preparation method and application of pomelo fruits. The preparation method comprises the step that pretreated pomelo fruits are frozen and dried, wherein the pomelo fruits which need to be molded are molded when being dried into semi-dried products, and continuously frozen and dried till the water content is lower than 8%. By adoption of the preparation method, the defects that a traditional processing method is long in production period and high in cost are overcome, the production efficiency is improved, the production cost is lowered, meanwhile, losses of effective components of a medical material are reduced, dried products subjected to freezing and drying are uniform in appearance color, attractive, easy to cut and prepare and convenient to use, and the quality stability of freezing and drying is improved; and the pomelo fruits prepared through the preparation method can be intact, or be cut in halves, or cut and prepared into slices or blocks or shreds, or smashed to use.
Description
Technical field
The present invention relates to a kind of manufacture field of Chinese medicine, especially a kind of preparation method and application of shaddock fruit.
Background technology
Shaddock fruit is dried green fruit for Citrus paradisi Macfadyen Citrus grandis (L.) Osbeck and its mutation.
Harvest when 3～April fruit is 3～7cm.Clean, be cut to two halves or piece, dry or low temperature drying.With eliminating dampness and eliminating phlegm, wide middle row
Gas, the effect for helping digestion, for cough due to wind-cold evil, larynx is itched abundant expectoration, and the obstruction of the circulation of vital energy is uncomfortable in chest, and dyspepsia is got sick from drinking too much wine, coldness and pain in the epigastrium, evil of vomitting is had loose bowels.Shaddock
Another name also has thunder shaddock, shaddock, Hu mandarin orange, bitter orange, smelly shaddock, fragrant goldenrain tree, bar, throwing, pomelo, tomentose pummelo fruit, Exocarpium Citri Rubrum tire.The mutation of shaddock is very
Many, modal kind has：1. Citrus grandis Citrus grandis Tomentosa, 2. pomelo shaddock Citrus grandis
Var.wentanyu Hort, 3. shatian pomelo Citrus grandis var.shatinyu Hort, 4. Pingshan shaddock Citrus
Grandis var.pinshanyu Hort, 5. the four seasons throw Citrus grandis var.szechipow Hort, 6. bright red throwing
Citrus grandis var.tahunpow Hort。
The source of shaddock fruit is Citrus paradisi Macfadyen Citrus grandis (L.) Osbeck, with《Chinese Pharmacopoeia》One change tangerine
One of two sources under red item " shaddock Citrus grandis (L.) Osbeck " is identical, but medicinal part is differed, Exocarpium Citri Grandis
Be its prematurity or it is maturescent be dried outside rind, and the medicine position of shaddock fruit is to be dried green fruit.
Contain aurantiin (naringin), Poncirus glycosides (poneirin), neohesperidin (neohesperi) and shaddock ped in shaddock
The new shaddock ped glucosides (nsringenin-4 '-glucoside-7-neohesperidoside) of element -4 '-glucoside -7-；Separately contain
Carrotene, Cobastab1, Cobastab2, vitamin C, Yan acid, calcium, phosphorus, iron, carbohydrate and volatile oil etc..Volatile oil content 0.3%
～0.9%, main component is citral (citral), Geraniol (geranilo), linalool (linalool) and adjacent amino
Methyl benzoate (methyl anthranilate) etc..
The existing preparation technology of shaddock fruit medicine materical crude slice is after the harvesting of shaddock fruit fresh fruit, impurity to be removed, after drying 2～3 days, at 80 DEG C
It is dried 4～5 days, is dried to half dry fruit that water content is 20%, requires according to processing, after carrying out artificial model or not moulding,
It is dried at 50 DEG C, after being less than 8% to water content, is placed in micro-wave oven and is dried 5 minutes, cut into slices, makes shaddock fruit
Medicine materical crude slice.The existing preparation technology cycle is long, and generally requiring more than 6 days to dry, and efficiency is low；Baking temperature is higher, time length, receive
Heat is uneven, and section carries out secondary microwave heating so that loss of effective components is larger, especially volatile oil loss of effective components
Totally.And made by shaddock fruit medicine materical crude slice color be brown, matter is hard, be difficult to cutting, and outward appearance is poor.
The content of the invention
It is an object of the invention to overcome above-mentioned the deficiencies in the prior art part and provide a kind of shaddock fruit cryodesiccated system
Preparation Method and application, the drying process of the preparation method replaces the solarization that prior art uses from the mode of vacuum freeze drying
Mode that is dry or drying, overcomes the long preparation period of prior art, efficiency low；Drying time length, temperature are high, loss of effective components
Larger and finished product color and luster, proterties are poor, be difficult to the deficiency of cutting.The reduction of erection time is reached, efficiency is improved, is reduced active ingredient
The purpose of loss, obtained freeze-drying product uniform color, attractive in appearance, user can the voluntarily purpose of cutting as needed.
Freeze-drying is the principle using ice crystal distillation, in the environment of high vacuum, by the water of frozen material
It is directly steam from ice solid sublimation to divide without the thawing of ice, therefore freeze-drying is also called drying bu sublimation, freeze-drying
Process includes material pre-treatment, prefreezing, freeze-drying and 4 stages of post processing.Because of moisture when the cortex of shaddock fruit is thicker lyophilized
Effusion is difficult, before freeze-drying is carried out, shaddock fruit is chosen, is gone the removal of impurity, should also carry out pricking place before hole or section etc.
Reason, finished product requires then carry out slicing treatment for whole fruit.Pre-freeze junction temperature is generally less than eutectic temperature 5～10
DEG C, eutectic temperature can be measured by electric-resistivity method, can reach pre-freeze junction temperature by 2 kinds of methods of slow freezing and quick freezing,
According to material and the difference of loading amount the time required to prefreezing, the time is also different, typically should at least protect after pre-freeze junction temperature is reached
Hold 1～2 hour, it is ensured that shaddock fruit carries out again vacuum freeze drying after all freezing.Vacuum freeze drying is divided into lyophilization reconciliation
Analysis is dried two stages, and lyophilization is dry first stage, main to remove the Free water freezed in material, can remove
90% or so moisture, the temperature requirement of this stage frozen crust have to be lower than temperature of eutectic point, and otherwise frozen crust material can occur
The bad phenomenons such as fusing, foaming, deformation, prevent being normally carried out for distillation；Drying layer temperature have to be lower than disintegration temperature, otherwise dry
Dry layer material can occur rigid decline, become sticky and cave in, and block spongy micropore, prevent distillation.Parsing-desiccation is dry the
It is two stages, main to remove not frozen absorption water, i.e., and the stronger combination water of solid bond, prevent from going bad, go mouldy, lead to
The water content of material is generally 0.5～4% after spending this stage, and this phase temperature have to be lower than disintegration temperature, hothouse vacuum
It is higher.The dry product that freeze-drying is obtained can carry out cutting into two or cutting is blocking or cutting is in blocks or cuts
Make silk or crushed after slightly cutting, the product of post processing is vacuum-packed, can also carry out nitrogen-filled packaging,
Various deep processing applications can be carried out to dry product.
Because vacuum freeze drying is carried out under low temperature, low pressure, and moisture directly distils, therefore gives product many spies
Different performance.As Vacuum Freezing ＆ Drying Technology also can be dehydrated than more thoroughly to heat sensitive material, and the finished product of drying is very steady
It is fixed, it is easy to long time stored.Because the drying of material is completed in the frozen state, compared with other drying means, the thing of material
Reason structure and molecule structure change are minimum, and its institutional framework and mode of appearance are preferably preserved.In vacuum freeze drying process
In, there is no Surface hardened layer in material, and it is internally formed the spongy of porous, thus with excellent rehydration, can be
Recover the state before being dried in short time.Because dry run is to carry out at quite low temperatures, and completely cut off air substantially,
Therefore restrained effectively heat-sensitive substance and chemistry, physics or biological change occur, and preferably save the activity in raw material
Material, and maintain the color and luster of raw material.
For achieving the above object, the technical scheme taken of the present invention is：The cryodesiccated preparation method of a kind of shaddock fruit and should
With the preparation method is the operation of pre-treatment, prefreezing, freeze-drying and post processing.
Cryodesiccated shaddock fruit is carried out, is applied according to the later stage of dry product, whole shaddock fruit can be carried out freeze-drying,
Cutting can be carried out into two, carry out freeze-drying after block, piece or silk.Whole fruit carry out it is cryodesiccated, because of the cortex of shaddock fruit
It is thicker, it is unfavorable for the effusion of moisture, in order to improve cryodesiccated efficiency, whole fruit should be carried out to prick the pre-treatment in hole, can adopt
Hole is pricked with penetration, centrosymmetric half through bundle hole may also be employed.Whole fruit carries out cryodesiccated, and having to the diameter of dry fruit will
Ask, plastotype process should be carried out when being refrigerated to half-dried to the shaddock fruit being relatively large in diameter, Jing Experimental Comparisons, water content be 20%～
30% carries out plastotype works well.General fresh fruit needs to carry out plastotype with diameter greater than 7cm, and plastic type is in a diameter of 4cm
Can be ellipse, star, rhombus, the heart also dependent on plastotype is required in the hollow of other numerical value diametric requirements in empty cylinder
Shape etc..
As the preferred embodiment of the cryodesiccated preparation method and application of shaddock of the present invention fruit, it is characterised in that
Including following processing step：
(1) pre-treatment：Selection, impurity elimination, bundle hole or cutting；
(2) pre-freeze junction temperature is -10 DEG C～-40 DEG C；
(3) freeze-drying to water content is 20%～30% semi-dried product；
(4) dry product of the freeze-drying to water content less than 8%；
(5) post-process.
As the preferred embodiment of the cryodesiccated preparation method and application of shaddock of the present invention fruit, the step (1)
The cutting operation of middle pre-treatment is included the cutting of shaddock fruit is for two halves or cutting is in blocks or cutting is blocking or cuts into silk.
As the preferred embodiment of the cryodesiccated preparation method and application of shaddock of the present invention fruit, the step (2)
Middle pre-freeze junction temperature is -10 DEG C～-40 DEG C, and the time is 2 hours～24 hours.
As the preferred embodiment of the cryodesiccated preparation method and application of shaddock of the present invention fruit, the step (3)
In step (4) freeze-drying operation：Condenser temperature be -10 DEG C～-50 DEG C, drying chamber pressure be 10～100Pa, temperature of heating plate
For 20 DEG C～80 DEG C.
As the preferred embodiment of the cryodesiccated preparation method and application of shaddock of the present invention fruit, it is characterised in that
Shaddock fruit needs plastotype, can carry out semi-dried product plastotype between step described in claim 3 (3) and step (4).Such as shaddock fruit is straight
Footpath is larger, more than 7cm, can be placed on the cylinder of a diameter of 4cm when freeze-drying to water content is 20～30%
It is interior, freeze-drying is further continued for finished product.Also dependent on requiring plastotype in the cylinder of a diameter of 4cm～6cm, or major diameter is
In the oval cylinder of 4cm～6cm, or in the hollow of other shapes.
As the preferred embodiment of the cryodesiccated preparation method and application of shaddock of the present invention fruit, the step (5)
Post processing, comprising following processing step：
(1) cutting or crushing：Cutting is two halves or piece or block or silk or not cutting or crushes；
(2) pack：Vacuum packaging or vacuum pack with nitrogen.
It is as the more preferably embodiment of the shaddock of the present invention cryodesiccated preparation method and application of fruit including following
Processing step：
(1) pre-treatment：Selection, impurity elimination, bundle hole or cutting；
(2) pre-freeze junction temperature is -10 DEG C～-40 DEG C, and the time is 2 hours～24 hours；
(3) freeze-drying condenser temperature is -10 DEG C～-50 DEG C, and drying chamber pressure is 10～100Pa, and temperature of heating plate is
20 DEG C～80 DEG C, the time is 2 hours～24 hours；
(4) post-process：It is vacuum-packed after cutting or crushing, or vacuum pack with nitrogen.
It is as the more preferably embodiment of the shaddock of the present invention cryodesiccated preparation method and application of fruit including following
Processing step：
(1) pre-treatment：Selection, impurity elimination, bundle hole；
(2) pre-freeze junction temperature is -10 DEG C～-40 DEG C, and the time is 2 hours～24 hours；
(3) freeze-drying condenser temperature is -10 DEG C～-50 DEG C, and drying chamber pressure is 10～100Pa, and temperature of heating plate is
20 DEG C～80 DEG C, the time is 2 hours～24 hours；
(4) when freeze-drying to water content is 20%～30% semi-dried product, by shaddock fruit plastotype in diameter or major diameter be 4cm
In the cylinder of～6cm, continue dry product of the freeze-drying to water content less than 8%；
(5) post-process：It is vacuum-packed after cutting or crushing, or vacuum pack with nitrogen.
As the preferred embodiment of the shaddock of the present invention cryodesiccated preparation method and application of fruit, claim 1～
Shaddock fruit freeze-drying described in 11 any one obtained by preparation method.
As the preferred embodiment of the shaddock of the present invention cryodesiccated preparation method and application of fruit, claim 1～
Application of the shaddock fruit freeze-drying described in 11 any one in deep processed product is prepared.
The really cryodesiccated preparation method and application of shaddock of the present invention, compares with following excellent with traditional processing mode
Gesture：By technical study and contrast test to vacuum freeze drying, preferred key process parameter.It is dry using vacuum refrigeration
It is dry, the production cycle is shortened, the efficiency of shaddock fruit freeze-drying preparation is improve, production cost is reduced, reduce active ingredient
Loss, it is ensured that the content of active ingredient, the dry product color of preparation is faint yellow to yellowish-brown, and color and luster is evenly, smell virtue
Perfume (or spice), proterties more preferably, and person's cutting easy to use.Vacuum packaging to dry product is processed, and improves the stability of product, it is ensured that
Quality, makes shaddock fruit preferably be applied in various product.
Specific embodiment
To better illustrate the object, technical solutions and advantages of the present invention, below in conjunction with specific embodiment to the present invention
It is described further.
Embodiment 1
A kind of embodiment of the cryodesiccated preparation method and application of shaddock of the present invention fruit, is to shaddock described in the present embodiment
Really whole fruit carries out cryodesiccated preparation, is prepared from using following methods：
(1) pre-treatment：The shaddock fruit of a diameter of 3～7cm is chosen, impurity is removed, 2 groups are divided into after cleaning, penetrated respectively
Formula pricks hole and the half through bundle hole of Central Symmetry；
(2) prefreezing：The shaddock fruit of pre-treatment is placed in freezer, Jing is refrigerated to -35 DEG C for 8～12 hours, and holding freezes 2
Hour；
(3) freeze-drying：Prefreezing shaddock fruit is placed in vacuum freeze drier, condenser temperature is -35 DEG C～-40 DEG C,
Hothouse vacuum is 40Pa, sets temperature of heating plate as 50 DEG C, to temperature of charge curve and temperature of heating plate oriented parallel, is frozen
Dry and hard beam；
(4) pack：It is 35% in humidity by dried whole fruit, temperature is to be vacuum-packed in 20 DEG C of environment, per bag
Fill 1.
As a result：The result that is dried of two kinds of bundle hole modes is more or less the same, and outer surface is light yellowish brown, and tangent plane is light yellow, sponge
Shape micropore distribution uniform, it is easy to cut into slices.Meanwhile, the density to pricking hole is compared, and is pricked hole density and is slightly had to rate of drying
Affect, density is big, and drying time is slightly shorter.But density is excessive, the outward appearance of dry fruit is slightly poor, and pricking hole density should be appropriate.
Embodiment 2
A kind of embodiment of the cryodesiccated preparation method and application of shaddock of the present invention fruit, is shaddock fruit described in the present embodiment
The preparation of whole fruit, is prepared from using following methods：
(1) pre-treatment：The shaddock fruit of a diameter of 3～7cm is chosen, impurity is removed, penetration is carried out after cleaning and is pricked hole；
(2) prefreezing：The shaddock fruit of pre-treatment is placed in freezer, Jing is refrigerated to -35 DEG C for 4～8 hours, and holding freezes 4
Hour；
(3) freeze-drying：Prefreezing shaddock fruit is placed in vacuum freeze drier, condenser temperature is -35 DEG C～-40 DEG C,
Hothouse vacuum is 40Pa, sets temperature of heating plate as 50 DEG C, to temperature of charge curve and temperature of heating plate oriented parallel, is frozen
Dry and hard beam；
(4) pack：It is 35% in humidity by dried whole fruit, temperature is to be vacuum-packed in 20 DEG C of environment, per bag
Fill 1.
As a result：Embodiment 1 and 2 is the comparison of two kinds of prefreezing modes, and dried frozen aquatic products result is more or less the same.Proterties is appearance
Face is light yellowish brown, and tangent plane is light yellow, it is easy to cut into slices.To carrying out freeze-drying, the knot of two kinds of prefreezing modes after shaddock fruit cutting
Fruit is also identical.
Embodiment 3
A kind of embodiment of the cryodesiccated preparation method and application of shaddock of the present invention fruit, is shaddock fruit described in the present embodiment
The preparation of whole fruit, is prepared from using following methods：
(1) pre-treatment：The shaddock fruit of a diameter of 3～7cm is chosen, impurity is removed, penetration is carried out after cleaning and is pricked hole；
(2) prefreezing：The shaddock fruit of pre-treatment is placed in freezer, Jing is refrigerated to -35 DEG C for 18～20 hours, prefreezing journey
Sequence is set as：0～4 hour temperature is -10 DEG C and kept for 1 hour, reduces within 6～9 hours temperature to -20 DEG C and is kept for 1 hour, 11
Temperature is reduced within～14 hours to -30 DEG C and is kept for 1 hour, reduced temperature to -35 DEG C and kept for 1 hour within 16～19 hours；
(3) freeze-drying：Prefreezing shaddock fruit is placed in vacuum freeze drier, condenser temperature is -35 DEG C～-40 DEG C,
Hothouse vacuum is 40Pa, sets temperature of heating plate as 50 DEG C, to temperature of charge curve and temperature of heating plate oriented parallel, is frozen
Dry and hard beam；
(4) pack：It is 35% in humidity by dried whole fruit, temperature is to be vacuum-packed in 20 DEG C of environment, per bag
Fill 1.
As a result：The comparison of embodiment 3 and the gained finished product of embodiment 1 and 2, the dried frozen aquatic products outer surface of embodiment 3 is pale yellow palm fibre
Color, tangent plane is light yellow, and spongy micropore size is uneven, has partial destruction, it is easy to cut into slices.
Embodiment 4
A kind of embodiment of the cryodesiccated preparation method and application of shaddock of the present invention fruit, is shaddock fruit described in the present embodiment
The preparation of whole fruit plastotype, is prepared from using following methods：
(1) pre-treatment：Shaddock fruit of the selection with diameter greater than 7cm, removes impurity, and the half through bundle of Central Symmetry is carried out after cleaning
Hole；
(2) prefreezing：The shaddock fruit of pre-treatment is placed in freezer, Jing is refrigerated to -35 DEG C for 6～10 hours, and holding freezes 4
Hour；
(3) freeze-drying：Prefreezing shaddock fruit is placed in vacuum freeze drier, condenser temperature is -35 DEG C～-40 DEG C,
Hothouse vacuum program setting is：Pressure is increased to 40Pa and keeps in 30min, and temperature of heating plate program setting is：
Temperature raises 55 DEG C and keeps in 30min, is being dried to 8 hours, 10 hours, 12 hours, 14 hours, 16 hours respectively, will be partly
Dry shaddock fruit is taken out, and is 35% in humidity, and temperature is that in 20 DEG C of environment, after taking out the sample for determining water content, remaining shaddock fruit is rapid
It is placed in the cylinder of diameter 4cm, is further continued for being placed in freeze-drying in drying machine bent to material dynamic temperature curve and temperature of heating plate
Line is parallel, freezes and terminates；
(4) pack：It is 35% in humidity by dried whole fruit, temperature is to be vacuum-packed in 20 DEG C of environment, per bag
Fill 1.
As a result：Determine 5 plastotype time points and take out the water content of sample, and determine 5 plastotype time point gained dry product shaddocks
Skin glycosides content and volatilization oil mass, carry out proterties contrast, as a result as shown in the table：
Conclusion：Plastotype is carried out to semi-dried product during different moisture content, its naringin content, volatilization oil mass, color odor trait
It is more or less the same, the irregular wrinkle situation of outward appearance of whole fruit, water content is less, and wrinkle lines is deeper, and fold is more obvious.Plastotype is imitated
The fruit preferably time is 8～10 hours after freeze-drying.
Embodiment 5
A kind of embodiment of the cryodesiccated preparation method and application of shaddock of the present invention fruit, is shaddock fruit described in the present embodiment
The preparation of whole fruit, is prepared from using following methods：
(1) pre-treatment：The shaddock fruit of a diameter of 3～7cm is chosen, impurity is removed, the half through bundle of Central Symmetry is carried out after cleaning
Hole；
(2) prefreezing：The shaddock fruit of pre-treatment is placed in freezer, Jing is refrigerated to -35 DEG C for 6～10 hours, and holding freezes 4
Hour；
(3) freeze-drying：Prefreezing shaddock fruit is placed in vacuum freeze drier, condenser temperature is -35 DEG C～-40 DEG C,
Hothouse vacuum program setting is：Pressure rises to 40Pa in 1 hour, keeps 40Pa pressure to carry out lyophilization in 6 hours, so
Afterwards in 1 hour pressure be down to 35Pa carry out parsing-desiccation to drying terminate；Temperature of heating plate program setting is：In 1 hour
Temperature rises to 55 DEG C, keeps 55 DEG C of temperature to carry out lyophilization in 6 hours, and then temperature is down to 50 DEG C and is parsed in 1 hour
It is dried to drying and terminates；
(4) pack：It is 35% in humidity by dried whole fruit, temperature is to be vacuum-packed in 20 DEG C of environment, per bag
Fill 1.
As a result：Embodiment 1 and 2 is freeze-drying constant temperature level pressure, and embodiment 3 and embodiment 4 are freeze-drying alternating temperature transformation,
Two ways compares, and the freezing rate of alternating temperature transformation is higher, and energy consumption is relatively low.The equal outward appearance of proterties of dried frozen aquatic products, moisture, shaddock ped
Glycosides content and volatile oil content are more or less the same.
Embodiment 6
The gained dry product of embodiment 1～4 is contrasted with the shaddock fruit medicine materical crude slice obtained by traditional preparation methods respectively, inclusive
Shape, moisture, naringin content and volatile oil content, moisture and determination of volatile oil method are measured according to current edition pharmacopeia, shaddock
Skin glycosides content assaying method is as follows：
Chromatographic condition is with system suitability with octadecylsilane chemically bonded silica as filler；With methanol-acetic acid-water
(35: 4: 61) are mobile phase；Detection wavelength 238nm.Theoretical cam curve is calculated by aurantiin peak and should be not less than 3000.
The preparation precision of reference substance solution weighs aurantiin reference substance in right amount, plus methyl alcohol makes solution of every 1ml containing 60 μ g,
Obtain final product.
The preparation of need testing solution：This product powder about 1g is taken, it is accurately weighed, in putting apparatus,Soxhlet's, plus petroleum ether (60～
90 DEG C) 100ml, it is heated to reflux 2 hours, petroleum ether liquid is discarded, the dregs of a decoction fling to solvent, plus methyl alcohol 150ml, are heated to reflux 3 hours
To extracting liquid colourless, let cool, filter, filtrate put in 200ml measuring bottles, with a small amount of methyl alcohol gradation washing container, in being incorporated to measuring bottle, plus
Methyl alcohol shakes up to scale.Precision measures 2ml, and in putting 25ml measuring bottles, plus methyl alcohol is to scale, shakes up, and obtains final product.
Determination method：It is accurate respectively to draw reference substance solution and each 10 μ l of need testing solution, liquid chromatograph is injected, determine,
Obtain final product.
The results are shown in Table shown in following table.
From result, dry product is obtained using preparation method of the present invention, naringin content, volatile oil content have and show very much
The raising of work, and moisture requires that proterties outward appearance is more attractive less than standard.
Embodiment 7
A kind of embodiment of the cryodesiccated preparation method and application of shaddock of the present invention fruit, is shaddock fruit described in the present embodiment
Cryodesiccated preparation is carried out after cutting is in blocks, is prepared from using following methods：
(1) pre-treatment：The shaddock fruit of a diameter of 3cm～7cm is chosen, impurity is removed, the piece of different-thickness is cut into after cleaning,
Thickness is respectively 0.5cm, 1.0cm and 1.5cm；
(2) prefreezing：The shaddock fruit of pre-treatment is placed in freezer, Jing is refrigerated to -35 DEG C for 6～10 hours, and holding freezes 4
Hour；
(3) freeze-drying：Prefreezing shaddock fruit is placed in vacuum freeze drier, condenser temperature is -35 DEG C～-40 DEG C,
Hothouse vacuum is respectively set as 40Pa, 50Pa and 60Pa, and temperature of heating plate is respectively set as 40 DEG C, 50 DEG C and 60 DEG C, point
Freeze-drying is not carried out to material dynamic temperature curve and temperature of heating plate oriented parallel, is freezed and is terminated；
(5) pack：It is 35% in humidity by dried dry product, temperature is to be vacuum-packed in 20 DEG C of environment, per bag
Dress 10g.
According to preliminary result, with naringin content as evaluation index, to freeze-drying operation after shaddock fruit cutting in flakes
Influence factor：Slice thickness, drying chamber pressure, temperature of heating plate, carry out L9(33) orthogonal test investigates, factor level table is as follows：
Factor level table
Tested according to factor level table arrangement, determine naringin content in dry product, as a result be see the table below：
Orthogonal experiments
Orthogonal experiment results are carried out into variance analysis, as a result be see the table below：
Naringin content detects the results of analysis of variance
Analysis of variance result shows that A, B, C factor of orthogonal experiment is respectively provided with significant difference.Knowable to analysis directly perceived,
Investigation factor importance is followed successively by A ＞ C ＞ B, and the integrated survey condition of production determines that freeze drying process is A2B2C2, as：Cut
Piece thickness 1.0cm, drying chamber pressure 50Pa, 50 DEG C of temperature of heating plate.
The preferred orthogonal test of the present embodiment freeze drying process, can be combined with considering the factor of production cost, with shaddock
Skin glycosides is main inspection target, and optimization test arrangement is carried out as secondary inspection target with rate of drying, energy consumption.Drying chamber pressure
Horizontal extent can also expand 10Pa～100Pa to, and temperature of heating plate scope can also expand 20 DEG C～80 DEG C to, arrange test to carry out
It is preferred that.And can be according to preferred experimental condition, further preferred drying chamber pressure and temperature of heating plate in freezing dry process
Change program setting, to obtain that content is higher, proterties more preferably, rate of drying is higher, the preparation freeze-drying life of consuming energy lower
Produce the parameter of operation.
Shaddock fruit cutting is blocking or silk after carry out the technique optimum condition of freeze-drying preparation, influence factor is that stripping and slicing is big
Little (or tobacco cut width), drying chamber pressure, temperature of heating plate, carry out L9(33) orthogonal test investigation.
Embodiment 8
A kind of embodiment of the cryodesiccated preparation method and application of shaddock of the present invention fruit, is shaddock fruit described in the present embodiment
The research of freeze-drying product and traditional drying product cough suppressing effect, it is specific as follows：
1st, material and method
1.1st, medicine and reagent
Test sample：Freeze-drying shaddock fruit water extracting liquid.
Traditional drying shaddock fruit water extracting liquid.(shaddock fruit is purchased from Guangdong Yi Kang Pharmaceuticals Ltds)
Reference substance：Dextromethorphan hydrobromide oral liquid, Zhuhai Federated Pharmaceutical Co., Ltd. Zhongshan Branch.
Fritillary and loquat cough mixture, Beijing Tongrentang Technology Development Co.ltd. Pharmaceutical Factory.
Reagent：Ammoniacal liquor, Xilong Chemical Co., Ltd.
Citric acid, Xilong Chemical Co., Ltd.
1.2nd, animal
Kunming mouse, male and female half and half, 18～22g of body weight, SPF levels；Cavy, male and female half and half, 180～200g of body weight.
1.3rd, instrument
CC2170A type constant pressure ultrasonic atomizers (Chinese-foreign joint Chengdu Weixin Electronic Keda New Technology Co. Ltd.)
2nd, method and result
2.1 ammoniacal liquor induced mice cough models and therapeutic evaluation
Take Kunming mouse 135, be randomly divided into 9 groups, i.e. blank group, the basic, normal, high dosage group of 2 kinds of test sample concentrates,
Positive control medicine (dextromethorphan hydrobromide oral liquid, fritillary and loquat cough mixture) group, 15 per group, water is can't help in mouse fasting before experiment
12h, then each group mouse press 0.1mLg-1Body weight gastric infusion, once a day, common 3d, wherein blank group distill to equal-volume
Water.1h after last dose, mouse is put into fixed container, and makes mouse receive the stimulation of constant pressure ammoniacal liquor, ammonia mist stimulation time
20s, stimulates and takes out mouse after stopping immediately, cough number of times in observation 3min.
As a result show, the need testing solution of 2 kinds of shaddock fruits can extend in the cough latent period of mouse, the 3min of reduction mouse
Cough number of times, shows with obvious antitussive action.Freeze-drying shaddock fruit water extracting liquid (water extracting liquid i.e. of the invention)
Cough suppressing effect is substantially better than the shaddock fruit water extracting liquid of traditional drying mode.
Guinea pig cough's model and therapeutic evaluation caused by 2.2 citric acids
Cavy 200 is taken, is one by one placed in it in 3L bell jars in experiment the previous day, with supersonic spraying with 600mmHg's
Pressure sprays into 17.5% citric acid soln by glass shower nozzle, continues 1min, and record self-spray plays cough number of times in 5min, selects
Cavy of the cough number of times more than 10 times is that qualified animal is used to test.Take qualified cavy 90 and be randomly divided into 9 groups with 2.1, per group
10, water 12h is can't help in fasting before experiment, and 0.1mLg is then pressed respectively-1Body weight body weight gastric infusion, blank group gives equal-volume
Distilled water, once a day, continuous 3d, 1h after last time administration are placed in cavy in the glass bell jar of 3L volumes, receive
17.5% citric acid soln stimulates (method is the same), continues 1min, and record self-spray plays cough number of times and cough in 5min and hides
Phase.
As a result show, in the need testing solution cough latent period of energy prolonged guinea pig, the 5min of reduction cavy of 2 kinds of shaddock fruits
Cough number of times, shows with obvious antitussive action.Freeze-drying shaddock fruit water extracting liquid (water extracting liquid i.e. of the invention)
Cough suppressing effect is substantially better than the shaddock fruit water extracting liquid of traditional drying mode.
Finally it should be noted that above example is only to illustrate technical scheme rather than the present invention is protected
The restriction of scope, although being explained in detail to the present invention with reference to preferred embodiment, one of ordinary skill in the art should manage
Solution, technical scheme can be modified or equivalent, without deviating from technical solution of the present invention essence and
Scope.
Claims (13)
1. the cryodesiccated preparation method and application of a kind of shaddock fruit, it is characterised in that the preparation method is will to choose pre-treatment
Shaddock fruit afterwards is obtained from cryodesiccated mode.
2. the cryodesiccated preparation method of shaddock as claimed in claim 1 fruit, it is characterised in that processing step includes：Pre-treatment,
Prefreezing, freeze-drying, post processing.
3. the cryodesiccated preparation method of shaddock as claimed in claim 1 or 2 fruit, it is characterised in that walk including following technique
Suddenly：
(1) pre-treatment：Selection, impurity elimination, bundle hole or cutting；
(2) pre-freeze junction temperature is -10 DEG C～-40 DEG C；
(3) freeze-drying to water content is 20%～30% semi-dried product；
(4) dry product of the freeze-drying to water content less than 8%；
(5) post-process.
4. the cryodesiccated preparation method of shaddock fruit as described in Claims 2 or 3, it is characterised in that pre-treatment in the step (1)
Cutting operation include being two halves or cutting in flakes by the cutting of shaddock fruit or cutting is blocking or cut into silk.
5. the cryodesiccated preparation method of shaddock fruit as described in Claims 2 or 3, it is characterised in that prefreezing in the step (2)
Temperature is -10 DEG C～-40 DEG C, and the time is 1 hour～24 hours.
6. the cryodesiccated preparation method of shaddock fruit as described in Claims 2 or 3, it is characterised in that the step (3) step (4)
In freeze-drying operation：Condenser temperature is -10 DEG C～-50 DEG C, and drying chamber pressure is 10～100Pa, and temperature of heating plate is 20 DEG C
～80 DEG C.
7. the cryodesiccated preparation method and application of a kind of shaddock fruit, it is characterised in that shaddock fruit needs plastotype, can be in claim
(3) freeze-drying of step described in 3 carries out plastotype to semi-dried product to the semi-dried product that water content is 20%～30%, continues to freeze and does
The dry dry product to water content less than 8%.
8. the cryodesiccated preparation method of shaddock as claimed in claim 7 fruit, it is characterised in that the semi-dried product plastotype in diameter or
Major diameter is in the cylinder of 4cm～6cm.
9. the cryodesiccated preparation method of shaddock fruit as described in Claims 2 or 3 or 7, it is characterised in that the step (5) includes
Following processing step：
(1) cutting or crushing：Cutting is two halves or piece or block or silk or not cutting or crushes；
(2) pack：Vacuum packaging or vacuum pack with nitrogen.
10. the cryodesiccated preparation method of shaddock as claimed in claim 1 or 2 fruit, it is characterised in that walk including following technique
Suddenly：
(1) pre-treatment：Selection, impurity elimination, bundle hole or cutting；
(2) pre-freeze junction temperature is -10 DEG C～-40 DEG C, and the time is 2 hours～24 hours；
(3) freeze-drying condenser temperature is -10 DEG C～-50 DEG C, and drying chamber pressure is 10～100Pa, and temperature of heating plate is 20 DEG C
～80 DEG C, the time is 2 hours～24 hours；
(4) post-process：It is vacuum-packed after cutting or crushing, or vacuum pack with nitrogen.
The really cryodesiccated preparation method of 11. shaddocks as claimed in claim 1 or 2, it is characterised in that walk including following technique
Suddenly：
(1) pre-treatment：Selection, impurity elimination, bundle hole；
(2) pre-freeze junction temperature is -10 DEG C～-40 DEG C, and the time is 2 hours～24 hours；
(3) freeze-drying condenser temperature is -10 DEG C～-50 DEG C, and drying chamber pressure is 10～100Pa, and temperature of heating plate is 20 DEG C
～80 DEG C, the time is 2 hours～24 hours；
(4) when freeze-drying to water content is 20%～30% semi-dried product, by shaddock fruit plastotype in diameter or major diameter be 4cm～
In the cylinder of 6cm, continue dry product of the freeze-drying to water content less than 8%；
(5) post-process：It is vacuum-packed after cutting or crushing, or vacuum pack with nitrogen.
Shaddock fruit described in a kind of 12. any one of claim 1～11 obtained by preparation method.
Application of the 13. shaddock fruit freeze-dryings according to claim 12 in deep processed product is prepared.
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| CN108041361A (en) * | 2017-11-28 | 2018-05-18 | 安徽砀山海升果业有限责任公司 | A kind of preparation method of the turbid juice of shaddock |
| CN108498608A (en) * | 2017-09-01 | 2018-09-07 | 广西壮族自治区农业科学院园艺研究所 | A kind of processing method of Exocarpium Citri Rubrum piece |
| CN108719878A (en) * | 2018-06-13 | 2018-11-02 | 西南大学 | A kind of vacuum freezing-drying preparation method thereof of citrus piece |
| CN111067000A (en) * | 2020-01-10 | 2020-04-28 | 江南大学 | Method for debitterizing processing and moisture absorption resistance of freeze-dried grapefruit |
| CN112190621A (en) * | 2020-09-22 | 2021-01-08 | 四川涪丰药业有限公司 | Method and equipment for processing fructus aurantii decoction pieces |
| CN113357880A (en) * | 2021-05-17 | 2021-09-07 | 云南易门丛山食用菌有限责任公司 | Processing technology of semi-freeze-dried tricholoma matsutake |
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| CN113357880A (en) * | 2021-05-17 | 2021-09-07 | 云南易门丛山食用菌有限责任公司 | Processing technology of semi-freeze-dried tricholoma matsutake |
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