CN106349074A - Method for extracting chlorogenic acid in Chinese wolfberry via microwave-assisted ultrasonic - Google Patents
Method for extracting chlorogenic acid in Chinese wolfberry via microwave-assisted ultrasonic Download PDFInfo
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- C07—ORGANIC CHEMISTRY
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- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
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- C07C69/00—Esters of carboxylic acids; Esters of carbonic or haloformic acids
- C07C69/66—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety
- C07C69/73—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety of unsaturated acids
- C07C69/732—Esters of carboxylic acids having esterified carboxylic groups bound to acyclic carbon atoms and having any of the groups OH, O—metal, —CHO, keto, ether, acyloxy, groups, groups, or in the acid moiety of unsaturated acids of unsaturated hydroxy carboxylic acids
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Abstract
A process method for extracting chlorogenic acid in Chinese wolfberry via microwave-assisted ultrasonic comprising the steps of: 1) Raw material pretreatment: the raw material is the skin residues from the fruit juicing and the waste residues from the wolfberry dried fruit, dried to the moisture <=12%, purified, and crushed by a low-temperature mill until the fineness degree reaches >=40 meshes. 2) Extraction: the crushed wolfberry raw materials are subject to the extraction of chlorogenic acid in the extraction pot of the microwave-assisted ultrasonic. The extraction solvent is pure water, the material liquid ratio is 1:5-1: 30 (m/v), pH 4-5, microwave frequency 800-1500MHz, ultrasonic frequency 30-50kHz, microwave extraction time 5-30min, ultrasonic extraction time 60-90min, and temperature 30-50, extraction for once. 3) Aftertreatment: the extracting solution is filtered and concentrated, and frozen in low temperature and vaccum, sublimated and dried, crushed, and packaged to obtain the finished product of the chlorogenic acid in Chinese wolfberry. The invention process has the advantages of low process cost, high production efficiency, stable product quality, and high economic efficiency.
Description
Technical field
The present invention relates to a kind of extraction process of Fructus Lycii Content of Chlorogenic Acid, particularly to a kind of microwave-assisted supersound extraction Fructus Lycii
The method of Content of Chlorogenic Acid, belongs to bioactive substance extractive technique field.
Background technology
Lycium barbarum is China's tradition rare medicinal herbss, has many pharmacology such as enhancing immunity, antioxidation, antitumor
Effect.Zhang Ziping (Ningxia University professor) etc. indicates Ningxia in " research of flavonoids from Lycium barbarum hplc finger printing "
Fructus Lycii chlorogenic acid peak area is higher.This scientific paper was published on " Chinese herbal medicine " the 1st phases of volume 2008 the 39th.Mountain forever triumphant (researcher)
" Study on extraction of Fructus Lycii Content of Chlorogenic Acid " determines in 1000g Fructus Lycii and can mention 7.1g extract Content of Chlorogenic Acid and contain
Measure as 32%.Enterprise, when producing Fructus Lycii processing, can produce substantial amounts of Fructus Lycii defect ware (offal), can using defect ware Fructus Lycii
Extract lycium barbarum polysaccharide, extract the residue after lycium barbarum polysaccharide and also can extract chlorogenic acid.
Chlorogenic acid (chlorogenic acid, hereinafter referred to as ca), is by caffeic acid (caffeic acid) and quinic acid
The depside that (quinic acid, QA) condensation dehydration generates, is plant during aerobic respiration
A kind of phenylpropanoids producing through shikimic acid pathway, molecular formula is c16h18o9, molecular weight 345.30.Chlorogenic acid is anti-
Bacterium, hemostasis, antiinflammatory, function of gallbladder promoting, increase the important source material of leukocyte, antiviral drugs, act on as there is adrenin；Green former
Acid has sensitization to people, inhales after people contains the plant dust of chlorogenic acid, can pant, dermatitis etc., but can be through little after anthropophagy
Intestinal secretion thing acts on, and is changed into no allergenic substance；Chlorogenic acid has blood pressure lowering and antitumor action: the Polyphenols in veterinary antibiotics
As chlorogenic acid, caffeic acid etc. can suppress carcinogen aflatoxin b and the mutagen of benzo [a] pyrene by suppressing activating enzymes
Property；Chlorogenic acid also can reach the effect of anti-cancer, anticancer by reducing carcinogenic utilization rate and its transport in liver；Green
Ortho acid has the kidney invigorating, diuresis, enhancing human body immunity effect.Chlorogenic acid acts on than vitamin e, vitamin to ddph free radical scavenging
C and caffeic acid are eager to excel, and can effectively remove ddph free radical, hydroxyl radical free radical and ultra-oxygen anion free radical.By hydrogen peroxide
In the haemolysis Inhibition test of mice erythrocyte of induction, compare the inhibitory action of several organic Polyphenol Acids, with the suppression of chlorogenic acid
Making is used the strongest.Effective removing to free radical for the chlorogenic acid, can maintain the normal 26S Proteasome Structure and Function of body cell, prevent and delay
The generation of the Pathophysiology phenomenon such as tumor, mutation, aging.
Chlorogenic acid is the ester being formed by caffeic acid and quinic acid, has ester bond, unsaturated double-bond and polynary in its molecular structure
3 l fractions of phenol.During plant extract, there is isomerization often through hydrolysis and the migration of intramolecular ester group.
Due to the special construction of chlorogenic acid, determining it can be extracted from plant using ethanol, acetone, methanol polar solvent
Come, but the unstability due to chlorogenic acid itself, it is unable to high temperature, high light and long-time heating during extraction.Mountain is forever triumphant " in Fructus Lycii
The Study on extraction of chlorogenic acid " (food with machinery, 2012-9-18) carried out comprehensively to the technique extracting Fructus Lycii Content of Chlorogenic Acid
Analysis and research, using ultrasonic extraction, with ethanol as solvent, by test, determine volume fraction of ethanol, solid-liquid ratio, carry
Take time, extraction time and ph value, draw chlorogenic acid optimum extraction parameter: volume fraction of ethanol is 74%, solid-liquid ratio is 1: 35
(m: v), extraction time 70min, extraction time are 3 times, ph value is 4.2.Extracting solution through purification by macroporous resin, 1 000g Fructus Lycii
In can mention 7.1g extract, extract Content of Chlorogenic Acid be 32%.Patent application 200910216294.0 discloses " a kind of
The method of extracting chlorogenic acid from Chinese wolfberry " it is characterised in that described method comprises the steps: 1) FRUCTUS LYCII pre-treatment step
Fructus Lycii is put baking oven first and is dried, and puts into standing 24h in hothouse, pulverize in rearmounted common reflux and flow back after taking-up
Defat, leaches solvent, and residue air-dries standby.2) extract lycium barbarum polysaccharide step with ethanol as solvent, using ultrasonic assistant method, carry
Take liquid through concentration, precipitate with ethanol, drying, obtain lycium barbarum polysaccharide coarse powder；Its process conditions is: volume fraction of ethanol is 60%, feed liquid
For 1:30, extraction time is 60min to ratio, and extraction time is 3 times.3) extract residual after Fructus Lycii chlorogenic acid step extraction lycium barbarum polysaccharide
Slag, with ethanol as solvent, ultrasonic assistant method extracts Fructus Lycii Content of Chlorogenic Acid, and it is pure that macroporous resin carries out separation to institute's chlorogenic acid extracting
To change, reversed-phase high-performance liquid chromatography is analyzed to Fructus Lycii Content of Chlorogenic Acid: its process conditions is: volume fraction of ethanol is 55%～
85%, solid-liquid ratio is 1:25～1:40, and the ph value of solution is 3！5, extraction time is 30～110min, and extraction time is 2～4
Secondary.Patent application 201410528464.x discloses " a kind of method extracting separating chlorogenic acid Chinese wolfberry fruit dregs after carrying oil ",
It is characterized in that, it includes following operating procedure: (1) takes the Chinese wolfberry fruit dregs after carrying oil, carries out supercritical with ethanol for entrainer
Carbon dioxide abstraction, extract is standby；(2) by macroporous adsorbent resin on supercritical carbon dioxide extraction extract, preferably use
(in addition macroporous resin d140, hpd100, hpd300 ab-8, dm130, dm130 and ads-17 can also for d101 type macroporous resin
It is suitable for), use water, 10～15% (v/v) ethanol elution successively, collect each alcohol elution respectively, concentrate, be dried, obtain final product green
Ortho acid.
Content of the invention
For Fructus Lycii chlorogenic acid in prior art, in extraction process, complex process, material content are low, extract its lytic activity
It is difficult to retain, extracts the low technical problem of yield, the present invention provides one kind to utilize microwave-assisted ultrasound assisted extraction technique, shortens and extracts
Time, do not use chemical solvent, it is to avoid high temperature leads to the Fructus Lycii chlorogenic acid novel technology for extracting that chlorogenic acid decomposes.This technique is extracted
Fructus Lycii chlorogenic acid has the stable significant advantage of yield height, low cost, product quality.
In order to solve above-mentioned technical problem, the present invention adopts the following technical scheme that.
A kind of process of microwave-assisted supersound extraction Fructus Lycii Content of Chlorogenic Acid, comprises the steps:
1) pretreatment of raw material: raw material squeeze the juice for medlar fresh fruit after skin slag and dried fruit of lycium barbarum produce in leftover bits and pieces, dry
To moisture≤12%, remove impurity, Lowtemperaturepulverizer is pulverized, and fineness degree reaches >=40 mesh.
2) extract: the Fructus Lycii raw material after pulverizing carries out the extraction of Fructus Lycii chlorogenic acid in microwave-assisted ultrasonic extraction tank,
Extraction solvent is pure water, solid-liquid ratio 1:5-1:30 (m/v), ph 4-5, microwave frequency 800-1500 mhz, ultrasonic frequency
30-50khz, microwave extraction time 5-30min, ultrasonic extraction time 60-90min, temperature 30-50 DEG C, extract 1 time.
3) post processing: extracting solution, through filtering and concentrating, cryogenic vacuum drying bu sublimation, smashes, packaging obtains final product Fructus Lycii green
Ortho acid finished product.
Further, in described raw material at least 80% be dried fruit of lycium barbarum produce in leftover bits and pieces, include FRUCTUS LYCII crushing
Grain, adhesion fruit, fallen fruits, oil fruit etc..
Further, described remove impurity includes: after drying, raw material is removed through electrostatic hair place to go machine, metal detector
Miscellaneous.
Further, the raw material after pulverizing first can soak 1-2h before extracting in pure water, and soaking temperature controls
At 30-50 DEG C.
Further, described filtering and concentrating includes: carry out coarse filtration through plate and frame filter, then dense through molecule membrane filtration
Contracting；Further, described molecular film is preferably the ps ultrafilter membrane of transit dose 200-500 molecular equivalency.
The Fructus Lycii chlorogenic acid finished product that above-mentioned process produces is according to enterprise's production standard labeling after the assay was approved, qualified product
Product items physical and chemical index is as follows.
1st, organoleptic indicator: product sensory index should meet table 1 and require.
Table 1 organoleptic indicator
| Project | Index |
| Color and luster | Canescence |
| Flavour and abnormal smells from the patient | There is the due flavour of Fructus Lycii chlorogenic acid and abnormal smells from the patient, free from extraneous odour |
| Character | Powder |
| Impurity | The exogenous impurity being visible by naked eyes |
2nd, microbiological indicator: product microbiological indicator should meet table 2 and require.
Table 2 microbiological indicator
3rd, product marking composition: chlorogenic acid >=30%.
Extraction process of the present invention produces Fructus Lycii chlorogenic acid product and meets company standard, and product quality is stable, has blood pressure lowering, resists
Tumor, the kidney invigorating, enhancing human body immunity power, defying age, anti-muscle skeleton aging, antibacterial, antiviral, anti-inflammation etc. act on, can
Extensively apply in food, health product, medicine and other fields.
Beneficial effect:
1st, the present invention is applied to the extraction of Fructus Lycii chlorogenic acid, extraction efficiency first using microwave-assisted ultrasonic wave extraction
Height, the extraction yield of Fructus Lycii chlorogenic acid reaches more than 85%；
2nd, Extraction solvent is pure water, solvent-free pollution, economical environment-protective；
3rd, Extracting temperature is low, is effectively retained the biological active substanceies of FRUCTUS LYCII Content of Chlorogenic Acid.
4th, process costs are low, and production efficiency is high, and product quality is stable, high financial profit, formed and produced 1000 kilograms per year
Fructus Lycii chlorogenic acid industrialization production line.
Brief description
Fig. 1: Fructus Lycii chlorogenic acid extraction process flow chart in specific embodiment；
The impact to chlorogenic acid yield for Fig. 2: the solid-liquid ratio；
The impact to chlorogenic acid yield for Fig. 3: the extraction time；
Fig. 4: the ph impact to chlorogenic acid yield.
Specific embodiment
Below by specific embodiment, it is further discussed below the present invention.Unless stated otherwise, do not describe in embodiment
Technological means all can be to be realized with mode known in those skilled in the art.In addition, embodiment be interpreted as illustrative
, and unrestricted the scope of the present invention, the spirit and scope of the invention are limited only by the claims that follow.For art technology
For personnel, on the premise of without departing substantially from spirit and scope of the present invention, to the material component in these embodiments, consumption, chi
Various modifications that very little, shape is carried out, replacement, improve and fall within protection scope of the present invention, and the present invention limited concrete
Parameter should have admissible range of error.
Embodiment 1
A kind of process of microwave-assisted supersound extraction Fructus Lycii Content of Chlorogenic Acid, comprises the steps:
1) pretreatment of raw material: raw material squeeze the juice for medlar fresh fruit after skin slag and dried fruit of lycium barbarum produce in leftover bits and pieces, dry
To moisture≤12%, remove impurity, Lowtemperaturepulverizer is pulverized, and fineness degree reaches >=40 mesh.
2) extract: the Fructus Lycii raw material after pulverizing carries out the extraction of Fructus Lycii chlorogenic acid in microwave-assisted ultrasonic extraction tank,
Extraction solvent is pure water, solid-liquid ratio 1:5-1:30 (m/v), ph 4-5, microwave frequency 800-1500 mhz, ultrasonic frequency
30-50khz, microwave extraction time 5-30min, ultrasonic extraction time 60-90min, temperature 30-50 DEG C.
3) post processing: extracting solution through carrying out coarse filtration through plate and frame filter, then through molecular film filtering and concentrating, cryogenic vacuum
Drying bu sublimation, smashes, aseptic packaging, obtains final product Fructus Lycii chlorogenic acid finished product.
Further, in described raw material at least 80% be dried fruit of lycium barbarum produce in leftover bits and pieces, include FRUCTUS LYCII crushing
Grain, adhesion fruit, fallen fruits, oil fruit etc..
Further, the raw material after pulverizing first can soak 1-2h before extracting in pure water, and soaking temperature controls
At 30-50 DEG C.
The yield extracting Fructus Lycii chlorogenic acid in present embodiment reaches 85%.In detection finished product, active ingredient chlorogenic acid content reaches
30%.
Embodiment 2
One provided in the present invention preferably in embodiment (with reference to Fig. 1 process chart), a kind of microwave-assisted surpasses
Sound extracts the process of Fructus Lycii Content of Chlorogenic Acid, comprises the steps:
1) pretreatment of raw material: raw material squeeze the juice for medlar fresh fruit after skin slag and dried fruit of lycium barbarum produce in leftover bits and pieces (at least
Account for 80%), dry to moisture≤12%, carry out remove impurity through electrostatic hair place to go machine, metal detector, Lowtemperaturepulverizer is pulverized,
Fineness degree reaches >=40 mesh.
2) extract: the Fructus Lycii raw material after pulverizing first soaks 1h in pure water, soaking temperature controls at 30-50 DEG C；Then
Carry out the extraction of Fructus Lycii chlorogenic acid in microwave-assisted ultrasonic extraction tank, Extraction solvent is pure water, preferred process conditions:
Microwave extraction power is 900 mhz, and ultrasonic extraction power is 40 khz, solid-liquid ratio 1:15 (m/v), 45 DEG C of Extracting temperature, ph
Value 4-5, microwave extraction time 20min, ultrasonic extraction time 90min, extraction time 1 time.
3) post processing: extracting solution through carrying out coarse filtration through plate and frame filter, then through transit dose 200-500 molecular equivalency
Ps ultrafiltration membrance filter concentrates, cryogenic vacuum drying bu sublimation, smashes, aseptic packaging, obtains final product Fructus Lycii chlorogenic acid finished product.
Under present embodiment process conditions, chlorogenic acid extracting yield is 86.3%.In detection finished product, active ingredient chlorogenic acid contains
Measure as 30.2%.
Embodiment 3
The optimization analysis of chlorogenic acid extracting factor.
(1) impact to chlorogenic acid yield for the solid-liquid ratio
As shown in Figure 2, solid-liquid ratio has large effect to chlorogenic acid yield.When solid-liquid ratio is less than 1:20 (m/v), green former
Sour yield is constantly in the trend of rising, and when solid-liquid ratio is more than 1:20 (m/v), yield highest, is in that slow decline becomes afterwards
Gesture.When illustrating that aqueous solvent addition increases, effective ingredient is conducive to dissolution in a solvent, improves yield.When solid-liquid ratio reaches
During 1:20 (m/v), the solvability of possible chlorogenic acid has reached maximum, therefore selects solid-liquid ratio to be 1:15 (m/v), so dense
Contracting, drying are both economical.
(2) impact to chlorogenic acid yield for the extraction time
From the figure 3, it may be seen that chlorogenic acid is when extracting 40-100min, yield is in slow growth trend, but increasing degree is not
Greatly, it is taken as that extraction time is less on the impact of chlorogenic acid yield.The factors such as comprehensive extraction efficiency, Financial cost consider, select
Extraction time is that 90 min are preferable.
(3) impact to chlorogenic acid yield for the ph
As shown in Figure 4, the change of ph value is larger on the extraction impact of chlorogenic acid, and this is with chlorogenic acid originally as a kind of organic acid
Relevant.The advantageous extraction in chlorogenic acid of acid condition, alkalescence condition next part chlorogenic acid, can it may happen that ionizing, hydrolyzing
The yield that chlorogenic acid can be led to declines.When the ph value of solution is about 4～5, chlorogenic acid yield is of a relatively high.
(4) ps, pan, pvdf ultrafiltration effectiveness comparison
Molecular cut off be 10000 ps, pan, pvdf (Vingon) film to 100 kg feed liquid ultrafiltration lh, measure super
Soluble solids content before filter and after ultrafiltration, experiment proves that the decay of ps film is relatively slow, and stain resistance is strong, and the decay of pvdf film is very fast,
Ps film is preferably used in technique.
Claims (8)
1. a kind of process of microwave-assisted supersound extraction Fructus Lycii Content of Chlorogenic Acid is it is characterised in that comprise the steps:
1) pretreatment of raw material: raw material squeeze the juice for medlar fresh fruit after skin slag and dried fruit of lycium barbarum produce in leftover bits and pieces, dry to water
Point≤12%, remove impurity, Lowtemperaturepulverizer is pulverized, and fineness degree reaches >=40 mesh；
2) extract: the Fructus Lycii raw material after pulverizing carries out the extraction of Fructus Lycii chlorogenic acid in microwave-assisted ultrasonic extraction tank, extract
Solvent is pure water, process conditions: solid-liquid ratio 1:5-1:30 (m/v), ph 4-5, microwave frequency 800-1500mhz, ultrasonic wave frequency
Rate 30-50khz, microwave extraction time 5-30min, ultrasonic extraction time 60-90min, temperature 30-50 DEG C, extract 1 time；
3) post processing: extracting solution, through filtering and concentrating, cryogenic vacuum drying bu sublimation, smashes, packaging obtains final product Fructus Lycii chlorogenic acid
Finished product.
2. as claimed in claim 1 a kind of process of microwave-assisted supersound extraction Fructus Lycii Content of Chlorogenic Acid it is characterised in that
In described raw material at least 80% be dried fruit of lycium barbarum produce in leftover bits and pieces, including the broken kernel of FRUCTUS LYCII, adhesion fruit, fallen fruits,
Oil fruit etc..
3. as claimed in claim 1 a kind of process of microwave-assisted supersound extraction Fructus Lycii Content of Chlorogenic Acid it is characterised in that
Described remove impurity includes: after drying, raw material carries out remove impurity through electrostatic hair place to go machine, metal detector.
4. as claimed in claim 1 a kind of process of microwave-assisted supersound extraction Fructus Lycii Content of Chlorogenic Acid it is characterised in that
Raw material after pulverizing first soaked 1-2h before extracting in pure water, and soaking temperature controls at 30-50 DEG C.
5. as claimed in claim 1 a kind of process of microwave-assisted supersound extraction Fructus Lycii Content of Chlorogenic Acid it is characterised in that
The process conditions extracted are: microwave extraction power is 900mhz, and ultrasonic extraction power is 40khz, solid-liquid ratio 1:15 (m/v),
45 DEG C of Extracting temperature, ph value 4-5, microwave extraction time 20min, ultrasonic extraction time 90min, extraction time 1 time.
6. as claimed in claim 1 a kind of process of microwave-assisted supersound extraction Fructus Lycii Content of Chlorogenic Acid it is characterised in that
Described filtering and concentrating includes: carries out coarse filtration through plate and frame filter, then through molecular film filtering and concentrating.
7. as claimed in claim 5 a kind of process of microwave-assisted supersound extraction Fructus Lycii Content of Chlorogenic Acid it is characterised in that
Described molecular film is the ps ultrafilter membrane of transit dose 200-500 molecular equivalency.
8. the Fructus Lycii chlorogenic acid product being obtained by any process of claim 1-7.
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| CN106349074B (en) | 2019-09-24 |
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