CN106117285A - High-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin technique - Google Patents
High-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin technique Download PDFInfo
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- CN106117285A CN106117285A CN201610423454.9A CN201610423454A CN106117285A CN 106117285 A CN106117285 A CN 106117285A CN 201610423454 A CN201610423454 A CN 201610423454A CN 106117285 A CN106117285 A CN 106117285A
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- anthocyanin
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- lonicera edulis
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- 150000004636 anthocyanins Chemical class 0.000 title claims abstract description 79
- 229930002877 anthocyanin Natural products 0.000 title claims abstract description 78
- 235000010208 anthocyanin Nutrition 0.000 title claims abstract description 78
- 239000004410 anthocyanin Substances 0.000 title claims abstract description 78
- 235000016813 Lonicera caerulea var edulis Nutrition 0.000 title claims abstract description 47
- 240000007893 Lonicera caerulea var. edulis Species 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000002481 ethanol extraction Methods 0.000 title claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 230000005684 electric field Effects 0.000 claims abstract description 41
- 235000013399 edible fruits Nutrition 0.000 claims abstract description 31
- 235000000177 Indigofera tinctoria Nutrition 0.000 claims abstract description 26
- 229940097275 indigo Drugs 0.000 claims abstract description 26
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 claims abstract description 26
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 238000000605 extraction Methods 0.000 claims abstract description 20
- 230000002378 acidificating effect Effects 0.000 claims abstract description 19
- 238000012545 processing Methods 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000013461 design Methods 0.000 claims abstract description 10
- 230000008569 process Effects 0.000 claims abstract description 10
- 230000031700 light absorption Effects 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000005457 optimization Methods 0.000 claims abstract description 6
- 238000012360 testing method Methods 0.000 claims description 19
- 239000000243 solution Substances 0.000 claims description 13
- 230000004044 response Effects 0.000 claims description 10
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 6
- 239000000872 buffer Substances 0.000 claims description 6
- 239000001632 sodium acetate Substances 0.000 claims description 6
- 235000017281 sodium acetate Nutrition 0.000 claims description 6
- 239000004677 Nylon Substances 0.000 claims description 4
- 239000007853 buffer solution Substances 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 229920001778 nylon Polymers 0.000 claims description 4
- 230000002572 peristaltic effect Effects 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003643 water by type Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000011017 operating method Methods 0.000 claims description 3
- KVMLCRQYXDYXDX-UHFFFAOYSA-M potassium;chloride;hydrochloride Chemical compound Cl.[Cl-].[K+] KVMLCRQYXDYXDX-UHFFFAOYSA-M 0.000 claims description 3
- 210000002966 serum Anatomy 0.000 claims description 3
- 235000011869 dried fruits Nutrition 0.000 claims description 2
- 238000007710 freezing Methods 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 230000008033 biological extinction Effects 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000000205 computational method Methods 0.000 claims 1
- 230000001186 cumulative effect Effects 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 239000001103 potassium chloride Substances 0.000 claims 1
- 235000011164 potassium chloride Nutrition 0.000 claims 1
- 238000000926 separation method Methods 0.000 claims 1
- 229910052708 sodium Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 abstract 1
- 230000008859 change Effects 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 7
- 238000004090 dissolution Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000002904 solvent Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 229930182470 glycoside Natural products 0.000 description 4
- 150000002338 glycosides Chemical class 0.000 description 4
- 210000000170 cell membrane Anatomy 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 238000000540 analysis of variance Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
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- 238000001035 drying Methods 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 230000003834 intracellular effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000007619 statistical method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000628799 Brachybotrys paridiformis Species 0.000 description 1
- 241000208828 Caprifoliaceae Species 0.000 description 1
- 241000245240 Lonicera Species 0.000 description 1
- 241000282453 Ursus americanus Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 235000021028 berry Nutrition 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 229940068517 fruit extracts Drugs 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 231100000753 hepatic injury Toxicity 0.000 description 1
- 210000003701 histiocyte Anatomy 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 235000019462 natural additive Nutrition 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- WVULZDFWPQCPPJ-UHFFFAOYSA-N potassium;hydrochloride Chemical compound Cl.[K] WVULZDFWPQCPPJ-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000611 regression analysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000020254 sheep milk Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Abstract
The problem low for solving Lonicera edulis anthocyanin extraction ratio, the invention provides high-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin technique, and this detailed process is: step a, pretreatment of raw material；Step b, acidic ethanol mixes with raw material；Step c, high voltage pulse electric field processing；Step d, separates；Step e, constant volume；Step f, surveys light absorption value.This technique arranges 4 variablees: concentration of alcohol, electric field intensity, umber of pulse and solid-liquid ratio；Design expert software is utilized to go out optimum extraction process for concentration of alcohol 68.12% according to Box Behnken design optimization, electric field intensity 21.31kV/cm, umber of pulse 9.38, solid-liquid ratio 1:79.27g/mL, Lonicera edulis anthocyanin content prediction value is 33.1877mg/g indigo fruit powder.The present invention produces indigo fruit as raw material with Changbai Mountain, with 0.1% (v/v) acidic alcohol as extractant, through high voltage pulse electric field processing, it is substantially shorter extraction time, it is effectively improved anthocyanin content, extract for Lonicera edulis anthocyanin and new method is provided, there is preferable using value and wide DEVELOPMENT PROSPECT.
Description
Technical field:The present invention relates to a kind of Lonicera edulis anthocyanin extracting method, particularly to a kind of high-pressure pulse electric
Auxiliary acidization ethanol extraction Lonicera edulis anthocyanin technique.
Background technology:Indigo fruit (Loniceraedulis) is again Lonicera edulis Turcz., black bear fruit, BrachybotryS paridiformis, unfirmly closing Lee
With sheep milk etc., Plant Taxonomy belongs to Caprifoliaceae, Lonicera, Radix Ophiopogonis subgenus, capsule pipe group, blue fruit subgroup, the wildest
Berries machaka, is a kind of emerging Wild fruits, is mainly distributed on Changbai Mountain, Jilin Province of China, Heilongjiang Province
The ground such as Eastern Daxinganling mountain area and the Inner Mongol, North China, northwest and Sichuan.Indigo fruit fruits nutrition enriches, rich in polyphenol, flower
The functional components such as color glycosides, are set to the rare precious wild acinus in the world by the World Food Programme.
The anthocyanin that at present indigo fruit extracts, has antitumor, antioxidation, resisting fatigue, regulation immunity, protection regard
The multiple biological activitys such as power, blood fat reducing, antiinflammatory and promotion hepatic injury reparation, have at aspects such as food, cosmetic even medicine
Huge application potential.
Extraction to Lonicera edulis anthocyanin in recent years has carried out numerous studies, and the extracting method of Lonicera edulis anthocyanin mainly has
Conventional organic solvents extraction, ultrasonic assistant extraction, microwave radiation exaraction, supercritical CO2Extraction, but these methods all exist
Certain defect, conventional organic solvents extracting operation is simple, but yield is low, solvent-oil ratio big, the production cycle is long；Ultrasound wave is auxiliary
Help extraction and microwave radiation exaraction yield to extract higher than conventional organic solvents, but operation is complicated, energy consumption is excessive, and in microwave process
The high temperature produced is likely to cause degraded or the oxidation of anthocyanin, reduces yield；Supercritical CO2Extraction yield is high, but produces into
This is too high.Now, high-pressure pulse electric is widely used in the extraction of bioactive substance, has a significant effect, most researchs
Showing, its main cause is that cell membrane is destroyed and causes cell to crack under highfield effect, beneficially the releasing of active substance
Putting, meanwhile, high-pressure pulse electric has the advantage such as simplicity, reproducible, efficiency is high, parameters easy-regulating.
Based on this, the invention provides the side of a kind of high-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin
Method, utilizes the advantage of high-pressure pulse electric, it is achieved the efficient rapid extraction of Lonicera edulis anthocyanin.
Summary of the invention:The defect existed based on above-mentioned prior art, the present invention proposes a kind of high-pressure pulse electric auxiliary acid
The method changing ethanol extraction Lonicera edulis anthocyanin, the method technique is simple, extraction ratio is high, time-consumingly few, can realize indigo fruit pattern
The efficient rapid extraction of glycosides.
Its technological process and control condition thereof are as follows:
A. pretreatment of raw material: the indigo fruit taking-up being placed on-20 DEG C of refrigerator-freezer freezen protective is put in freezer dryer freezing
Being dried, it is the most standby that dried fruit becomes powder to store after crossing 1mm nylon screen through crusher in crushing.
B. acidic ethanol mixing: take a certain amount of indigo fruit powder, proportionally add 0.1% (v/v) acidic alcohol.
C. high voltage pulse electric field processing: above-mentioned mixed serum is delivered to high-voltage pulse with 7mL/min flow velocity through peristaltic pump
Electric field processing chamber, carries out high voltage pulse electric field processing under the conditions of certain electric field intensity (kV/cm) and umber of pulse (individual).
D. separate: the serosity through high voltage pulse electric field processing is placed in low speed centrifuge centrifugal (4000r/min,
15min), take supernatant, be anthocyanin extracting solution.
E. constant volume: accurately draw 1.25mL anthocyanin extracting solution, adds in 50mL volumetric flask, respectively with the chlorination of pH1.0
The sodium acetate of potassium-hydrochloric acid buffer solution and pH4.5-hac buffer constant volume is standby.
F. light absorption value is measured: take the solution after appropriate constant volume respectively and be placed in test tube, water-bath in 40 DEG C of waters bath with thermostatic control
After 40min, under 510nm and 700nm, measure light absorption value with distilled water for blank respectively, calculate anthocyanin content.
The present invention has the following advantages and effect:
1. the present invention uses high-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin first, at high-voltage pulse electric
Under field action, plant cell wall breaking cracking or perforation, promote the release of indigo fruit intracellular anthocyanin active component, improve pattern
Glycosides yield, shortens extraction time, reduces power consumption, is really achieved high efficiency extraction.
2. to have operating procedure simple, easy for the method for the present invention, and production cost is low, and extraction efficiency is high, good product quality
Deng remarkable advantage.
3. the Lonicera edulis anthocyanin that the present invention obtains, can be applied to food and health care food as a kind of natural additive for foodstuff
Each field such as product.
Accompanying drawing illustrates:
Below in conjunction with the accompanying drawings the detailed description of the invention of the present invention is described in further detail.
Fig. 1 is the concentration of alcohol change affecting laws figure to Lonicera edulis anthocyanin content；
Fig. 2 is the electric field intensity change affecting laws figure to Lonicera edulis anthocyanin content；
Fig. 3 is the umber of pulse change affecting laws figure to Lonicera edulis anthocyanin content；
Fig. 4 is the solid-liquid ratio change affecting laws figure to Lonicera edulis anthocyanin content.
Detailed description of the invention
Embodiment 1, high-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin technique response surface optimization are tested
1, preparation of samples and process of the test
(1) the indigo fruit taking-up being placed on-20 DEG C of refrigerator-freezer freezen protective is put in lyophilization in freezer dryer, after drying
Fruit to become powder to store after crossing 1mm nylon screen through crusher in crushing the most standby.
(2) take a certain amount of indigo fruit powder, proportionally add after 0.1% (v/v) acidic alcohol with 7mL/min flow velocity
Deliver to high-voltage pulse electric field processing chamber through peristaltic pump, carry out under the conditions of certain electric field intensity (kV/cm) and umber of pulse (individual)
High voltage pulse electric field processing.
(3) serosity through high voltage pulse electric field processing is placed in low speed centrifuge centrifugal (4000r/min, 15min), accurate
Really draw 1.25mL supernatant i.e. anthocyanin extracting solution, add in 50mL volumetric flask, delay with the potassium chloride-hydrochloric acid of pH1.0 respectively
The sodium acetate of dissolved liquid and pH4.5-hac buffer constant volume.
(4) solution after taking appropriate constant volume respectively is placed in test tube, in 40 DEG C of waters bath with thermostatic control after water-bath 40min, to steam
Distilled water is that blank measures light absorption value respectively under 510nm and 700nm, calculates anthocyanin content by pH differential method.
(5) anthocyanin content computing formula is:
2, EXPERIMENTAL DESIGN and statistical analysis
(1) single factor experiment
With concentration of alcohol, electric field intensity, umber of pulse and solid-liquid ratio as major influence factors, anthocyanin content is evaluation index
Carrying out single factor experiment, test parallel assay three times, takes its meansigma methods every time.
(2) response phase method optimization design
According to single factor experiment result, choose Lonicera edulis anthocyanin content is rung more significant concentration of alcohol, electric field intensity,
Umber of pulse and these four factors of solid-liquid ratio, according to Box-Behnken design principle design experiment, and utilize design expert
Software carries out data process, sets up the multinomial regression model of secondary, is predicted result of the test analyzing.Design factor water-glass is shown in
Table 1.
Table 1 response surface experiments variable and coding schedule
With concentration of alcohol (X1), electric field intensity (X2), umber of pulse (X3) and solid-liquid ratio (X4) it is independent variable, with indigo fruit flower
Color glycosides content is response value (Y), response surface experiments design and the results are shown in Table 2.
The design of table 2 response surface experiments and result
(3) foundation of model and statistical analysis
Utilize designexpert software that table 2 test data carries out multiple regression analysis, after removing not notable item, obtain
Secondary between response variable (concentration of alcohol, electric field intensity, umber of pulse and solid-liquid ratio) and response value (anthocyanin content) is multinomial
Regression equation:
Y=-76.76933+0.57962X1+1.68863X2+6.30625X3+1.07572X4+3.55000E-003X1X2-
0.015000X1X3+2.27500E-003X1X4+7.00000E-003X2X3-1.85000E-003X2X4-9.5000E-003X3X4-
5.10083E-003X1 2-0.043403X2 2-0.24940X3 2-6.95083E-003X4 2
F inspection can determine that linear relationship significance between each factor and response value, and P value is the least, and explanatory variable is the most notable.By
Analysis of variance table (table 3) understands, the notable (R of linear relationship between its dependent variable and all independent variables2=0.9982), model shows
Work level is less than 0.0001, so this regression variance model is the most notable.
Table 3 quadratic regression model the results of analysis of variance
(4) test result analysis and optimization
Model analysis understands, high-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin optimal processing parameter: second
Determining alcohol 68.12%, electric field intensity 21.31kV/cm, umber of pulse 9.38, solid-liquid ratio 1:79.27g/mL.With this understanding,
To anthocyanin content be 33.1877mg/g indigo fruit powder.
Test 1, high-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin process testing
(1) the indigo fruit taking-up being placed on-20 DEG C of refrigerator-freezer freezen protective is put in lyophilization in freezer dryer, after drying
Fruit to become powder to store after crossing 1mm nylon screen through crusher in crushing the most standby.
(2) take a certain amount of indigo fruit powder, proportionally add after 0.1% (v/v) acidic alcohol with 7mL/min flow velocity
Deliver to high-voltage pulse electric field processing chamber through peristaltic pump, carry out under the conditions of certain electric field intensity (kV/cm) and umber of pulse (individual)
High voltage pulse electric field processing.
(3) serosity through high voltage pulse electric field processing is placed in low speed centrifuge centrifugal (4000r/min, 15min), accurate
Really draw 1.25mL supernatant i.e. anthocyanin extracting solution, add in 50mL volumetric flask, delay with the potassium chloride-hydrochloric acid of pH1.0 respectively
The sodium acetate of dissolved liquid and pH4.5-hac buffer constant volume.
(4) solution after taking appropriate constant volume respectively is placed in test tube, in 40 DEG C of waters bath with thermostatic control after water-bath 40min, to steam
Distilled water is that blank measures light absorption value respectively under 510nm and 700nm, and calculating anthocyanin content by pH differential method is
32.96mg/g indigo fruit powder.
Test 2, the concentration of alcohol change impact on Lonicera edulis anthocyanin content
Under conditions of electric field intensity 20kV/cm, umber of pulse 8, solid-liquid ratio 1:80, acidic ethanol concentration is set as
40-80% totally 5 changing values；Remaining is with test 1, result such as Fig. 1.
When acidic ethanol concentration is less than 70%, Lonicera edulis anthocyanin content improves with the increase of concentration of alcohol, and this can
Can be owing to along with the increase of concentration of alcohol, the penetrating power of solvent increases the most therewith, beneficially anthocyanin class water-soluble substances
Dissolution；When acidic ethanol concentration is more than 70%, Lonicera edulis anthocyanin content declines, and it is excessive that this is likely due to concentration of alcohol
Time, the too low dissolution being unfavorable for anthocyanin class material on the contrary of polarity, cause anthocyanin content that downward trend occurs.Therefore, most preferably
Acidic ethanol concentration be 70%.
Test 3, the electric field intensity change impact on Lonicera edulis anthocyanin content
Under conditions of acidic ethanol concentration 70%, umber of pulse 8, solid-liquid ratio 1:80, electric field intensity is set as 10-
30kV/cm totally 5 changing values；Remaining is with test 1, result such as Fig. 2.
When electric field intensity is less than 20kV/cm, Lonicera edulis anthocyanin content improves with the increase of electric field intensity, and this may
It is owing to the quantity of electric charge on indigo fruit surface being made under the effect at bigger extra electric field to become many, causing the intracellular dispatch from foreign news agency of indigo fruit
Potential difference increases, and when it is higher than the critical potential of cell membrane, cell membrane will be breakdown, promotes in indigo fruit the materials such as anthocyanin
Dissolution, increase extracted amount；When electric field intensity is more than 20kV/cm, Lonicera edulis anthocyanin content declines, and this was likely due to
High electric field intensity can cause anthocyanin structure to change, and causes anthocyanin to degrade, and makes the extracted amount of anthocyanin reduce, causes
There is downward trend in anthocyanin content.Therefore, optimal electric field intensity is 20kV/cm.
Test 4, the umber of pulse change impact on Lonicera edulis anthocyanin content
Under conditions of acidic ethanol concentration 70%, field intensity 20kV/cm, solid-liquid ratio 1:80, umber of pulse is set as 4-
12 totally 5 changing values；Remaining is with test 1, result such as Fig. 3.
When umber of pulse is less than 10, Lonicera edulis anthocyanin content increases along with umber of pulse and improves, and this is likely due to increase
Big umber of pulse number, adds electric field and the time of indigo fruit effect and frequency, and solvent can quickly ooze under the drive of electric current
Enter cell interior, promote the dissolution of anthocyanin；When umber of pulse more than 10 time, Lonicera edulis anthocyanin content reduce, this be probably by
Destroy cellularity in umber of pulse is excessive, make anthocyanin extracted amount reduce, cause anthocyanin content that downward trend occurs.Cause
This, optimal umber of pulse is 10.
Test 5, the solid-liquid ratio change impact on Lonicera edulis anthocyanin content
Under conditions of acidic ethanol concentration 70%, field intensity 20kV/cm, umber of pulse 10, solid-liquid ratio is set as 1:
Individual totally 5 changing values of 60-1:100；Remaining is with test 1, result such as Fig. 4.
When solid-liquid ratio is less than 1:80, Lonicera edulis anthocyanin content increases along with solid-liquid ratio and improves, and this is likely due to
The increase of Extraction solvent volume, expands the concentration difference inside and outside histiocyte, promotes that Lonicera edulis anthocyanin expands in Extraction solvent
Dissipate, beneficially anthocyanin dissolution；When solid-liquid ratio is more than 1:80, Lonicera edulis anthocyanin content reduces, and this is likely due to solvent
Too much have impact on electric current and the intercellular effect of indigo fruit, have impact on the dissolution of anthocyanin, make anthocyanin extracted amount reduce, cause
There is downward trend in anthocyanin content.Therefore, optimal solid-liquid ratio is 1:80.
Claims (6)
1. a high-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin technique, it is characterised in that be with indigo fruit
Raw material, utilizes high-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin and by response surface optimization extraction process, its
Technological process and operating procedure are as follows:
High-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin technological process: pretreatment of raw material → acidic ethanol mixing
→ high voltage pulse electric field processing → separation → constant volume → mensuration light absorption value；
High-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin operating procedure is as follows with main points:
(1) pretreatment of raw material: the indigo fruit taking-up being placed on-20 DEG C of refrigerator-freezer freezen protective is put in freezer dryer freezing dry
Dry, it is the most standby that dried fruit becomes powder to store after crossing 1mm nylon screen through crusher in crushing；
(2) acidic ethanol mixing: take a certain amount of indigo fruit powder, proportionally add 0.1% (v/v) acidic alcohol；
(3) high voltage pulse electric field processing: above-mentioned mixed serum is delivered to high-pressure pulse electric with 7mL/min flow velocity through peristaltic pump
Process chamber, carries out high voltage pulse electric field processing under the conditions of certain electric field intensity (kV/cm) and umber of pulse (individual)；
(4) separate: the serosity through high voltage pulse electric field processing is placed in low speed centrifuge centrifugal (4000r/min, 15min),
Take supernatant, be anthocyanin extracting solution；
(5) constant volume: accurately draw 1.25mL anthocyanin extracting solution, adds in 50mL volumetric flask, respectively with the potassium chloride of pH1.0-
The sodium acetate of hydrochloric acid buffer solution and pH4.5-hac buffer constant volume is standby；
(6) light absorption value is measured: take the solution after appropriate constant volume respectively and be placed in test tube, water-bath 40min in 40 DEG C of waters bath with thermostatic control
After, under 510nm and 700nm, measure light absorption value with distilled water for blank respectively, calculate anthocyanin content.
2. high-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin technique as claimed in claim 1, its feature
Being, during described addition acidic ethanol, acidic ethanol concentration is 40%-80%, indigo fruit powder and acidic ethanol feed liquid
Ratio is 1:60-1:100g/mL.
3. high-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin technique as claimed in claim 1, its feature
Being, described high voltage pulse electric field processing condition: electric field intensity is 10-30kV/cm, umber of pulse is 4-12.
4. high-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin technique as claimed in claim 1, its feature
It is, the potassium chloride-hydrochloric acid buffer solution of described pH1.0 and the sodium acetate of pH4.5-hac buffer compound method: (1)
Potassium chloride-the hydrochloric acid buffer solution of pH1.0: according to the ratio of 25:67 by Klorvess Liquid that concentration is 0.2mol/L and
The hydrochloric acid solution of 0.2mol/L uniformly mixes, and pH meter corrects；(2) sodium acetate-hac buffer of pH4.5: according to the ratio of 1:1
The sodium acetate solution of acetum that concentration is 0.2mol/L and 0.2mol/L is uniformly mixed by example, and pH meter corrects.
5. high-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin technique as claimed in claim 1, its feature
Being, described anthocyanin content computational methods are pH differential method, and formula is as follows:
In formula: A (A510-A700nm) pH1.0-(A510-A700nm)pH4.5；
The molal weight of Mw C-3-G, 449.2g/mol；
The cms of b light path, 1cm；
The molar extinction coefficient of ε C-3-G, 26,900L cm1·mol1；
The extension rate that n sample is total；
The cumulative volume of V extracting solution, mL；
V0Sample volume, mL.
6. high-pressure pulse electric auxiliary acidization ethanol extraction Lonicera edulis anthocyanin technique as claimed in claim 1, its feature
Being, described indigo fruit powder mixed serum arranges 4 variablees (concentration of alcohol, electric fields through high-pressure pulse electric assisted extraction
Intensity, umber of pulse and solid-liquid ratio), utilize designexpert software to carry out data process according to Box-Behnken design principle
And process optimization.
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| CN107652337A (en) * | 2017-09-26 | 2018-02-02 | 齐鲁工业大学 | The anthocyanin such as a kind of black rice, black soya bean, purple potato, rose, tree peony extract preparation method |
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