CN109316520A - The extracting method of fructus crataegi pinnatifidae skin total polyphenols - Google Patents
The extracting method of fructus crataegi pinnatifidae skin total polyphenols Download PDFInfo
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Abstract
The invention discloses a kind of extracting methods of fructus crataegi pinnatifidae skin total polyphenols, comprising the following steps: (1) feedstock processing: fructus crataegi pinnatifidae skin is ground into fructus crataegi pinnatifidae skin powder, it is spare；(2) Microwave Extraction: weighing fructus crataegi pinnatifidae skin powder that the step (1) obtains in extraction flask, and the ethyl alcohol that concentration is 30~70% is added, and carries out Microwave Extraction, and microwave power is 210~490W, and extraction time is 8~40min, obtains extracting solution；(3) collect extract: the extracting solution that the step (2) obtains is centrifuged 3~5min under conditions of 3500~4000r/min, obtains fructus crataegi pinnatifidae skin total polyphenols.The present invention uses multistage microwave amplifier fructus crataegi pinnatifidae skin total polyphenols, easy to operate, extraction efficiency is high, has opened up new way for the comprehensive utilization of fructus crataegi pinnatifidae skin.
Description
Technical field
The present invention relates to the extracting methods of phenolic substances in natural plants, more specifically to a kind of fructus crataegi pinnatifidae skin
The extracting method of middle polyphenol.
Background technique
Plant polyphenol is to exist in plant the secondary metabolites with polyhydric phenols structure, it is extensive in various plants
In the presence of, and the plant polyphenol contained in the positions such as skin, root, leaf and fruit in plant is relatively more.Plant polyphenol is in nature
Reserves are especially abundant, its chemical property is active, there is fine physiological activity and pharmacological activity, and it is strong to effectively promote human body
Health, with continuous further investigation, plant polyphenol is widely used in real life, in food industry, medical health care, chemical industry
Daily equal fields play increasingly important role.
Hawthorn is many kinds of in China, and resource reserves are abundant, and there is plantation on the more ground in the whole nation.Fructus crataegi pinnatifidae is the one of fructus crataegi cuneatae
Kind, in the osmanthus west in Guangxi, being distributed Northwest Guangxi Province more.Fructus crataegi pinnatifidae fruit is big, and surface is smooth vivid, rich in a variety of nutrition at
Point.Fructus crataegi pinnatifidae also contains a variety of active ingredients, research shows that fructus crataegi pinnatifidae have promote digestion, decompression, reducing blood lipid, it is anti-oxidant,
It protects liver, improve the effects of immunity of organisms, antibacterial, analgesic.Fructus crataegi pinnatifidae edible value with higher and medical value,
With very big development prospect.
Nowadays, people focus mostly in haw pulp, leaves of Hawthorn, Chinese hawthorn seed, to fructus crataegi pinnatifidae to the research of fructus crataegi pinnatifidae
Utilization be also chiefly used in developing health food, and the product for using fructus crataegi pinnatifidae skin to develop is seldom, most of all as dead meal, because
This, which utilizes fructus crataegi pinnatifidae skin, all has great importance for environmental protection and the utilization of resources.
Currently, the method for extracting polyphenol is mainly organic solvent extraction.But the phenol generalization that organic solvent extraction obtains
Compound production is lower.In addition, ultrasonic wave is also introduced into the extraction of polyphenol, but usually all carry out at high temperature, due to the heat of polyphenol
Stability is bad, is easy to cause polyphenol that oxidational losses occurs, and fractions of active ingredient wrecks.
Summary of the invention
The object of the present invention is to provide a kind of extracting methods of polyphenol in fructus crataegi pinnatifidae skin, do not have to solve existing fructus crataegi pinnatifidae
The problem of being fully utilized carries out Microwave Extraction to the polyphenol in fructus crataegi pinnatifidae skin.This method is easy to operate, extraction efficiency
It is high.
The purpose of the present invention is achieved through the following technical solutions: the extracting method of polyphenol in a kind of fructus crataegi pinnatifidae skin, packet
Include following steps:
(1) feedstock processing: being ground into fructus crataegi pinnatifidae skin powder for fructus crataegi pinnatifidae skin, spare.
(2) Microwave Extraction: weighing fructus crataegi pinnatifidae skin powder that above-mentioned steps (1) obtain in extraction flask, and it is 30 that concentration, which is added,
~70% ethyl alcohol carries out Microwave Extraction, and microwave power is 210~490W, and extraction time is 8~40min, obtains extracting solution.
(3) it collects extract: the extracting solution that above-mentioned steps (2) obtain is centrifuged 3 under conditions of 3500~4000r/min
~5min obtains fructus crataegi pinnatifidae skin total polyphenols.
Further, in step (2), second is added by the solid-liquid ratio that 20~60mL solvent is added in 1g fructus crataegi pinnatifidae skin powder
Alcohol.
Further, in the step (2), the ethyl alcohol that concentration is 40~60% is added, carries out Microwave Extraction, microwave power
For 210~350W, extraction time is 24~40min.
Further, in the step (2), the solid-liquid ratio of fructus crataegi pinnatifidae skin powder and ethyl alcohol is 1:20~60g/mL.
Further, in step (2), the concentration that ethyl alcohol is added is 50%.
Further, in step (2), the microwave power is 280W.
Further, in step (2), the solid-liquid ratio of the fructus crataegi pinnatifidae skin powder and ethyl alcohol is 1:60g/mL.
Further, in step (2), the extraction time is 40min.
Further, in step (3), the extracting solution is centrifuged 5min under conditions of 3500r/min.
Compared with prior art, the device have the advantages that are as follows:
The present invention obtains fructus crataegi pinnatifidae skin total polyphenols using microwave radiation exaraction, and microwave radiation exaraction can be improved largely
The extracted amount of polyphenol in fructus crataegi pinnatifidae skin, and it is easy to operate simple, the cost of consumption was not only reduced, but also saved the energy, and had been
Effective exploitation utilizes one of the desirable route of fructus crataegi pinnatifidae skin resource, and also new way has been opened up in the comprehensive utilization for fructus crataegi pinnatifidae skin
Diameter.
Detailed description of the invention
Fig. 1 is gallic acid canonical plotting；
Fig. 2 is the curve graph of influence of the concentration of alcohol to fructus crataegi pinnatifidae skin total polyphenols extracted amount；
Fig. 3 is the curve graph of influence of the solid-liquid ratio to fructus crataegi pinnatifidae skin total polyphenols extracted amount；
Fig. 4 is the curve graph of influence of the microwave power to fructus crataegi pinnatifidae skin total polyphenols extracted amount；
Fig. 5 is the curve graph of influence of the extraction time to fructus crataegi pinnatifidae skin total polyphenols extracted amount.
Specific embodiment
With reference to embodiment, technical solution of the present invention is described in further detail, but do not constituted pair
Any restrictions of the invention.
Embodiment 1
(1) feedstock processing: fructus crataegi pinnatifidae skin is crushed with pulverizer, 60 meshes is smashed it through, obtains dry great Guo Shan
Short, bristly hair or beard skin powder, it is spare.
(2) Microwave Extraction: weighing 1g fructus crataegi pinnatifidae skin powder in extraction flask, and it is molten for 30% ethyl alcohol that 30mL, concentration is added
Agent carries out Microwave Extraction, and microwave power 280W, extraction time 8min obtain extracting solution.
(3) it collects extract: extracting solution being centrifuged 5min under conditions of 3500r/min, it is always more to obtain fructus crataegi pinnatifidae Pi
Phenol.
Embodiment 2~5 and the difference of embodiment 1 are that the concentration for the ethyl alcohol being added in the step (2) is respectively
40%, 50%, 60%, 70%.
Embodiment 6
(1) feedstock processing: fructus crataegi pinnatifidae skin is crushed with pulverizer, 60 meshes is smashed it through, obtains dry great Guo Shan
Fructus crataegi pinnatifidae skin powder is set and is put in hermetic bag to storage at the drying of cool place by short, bristly hair or beard skin powder, spare.
(2) Microwave Extraction: weighing 1g fructus crataegi pinnatifidae skin powder in extraction flask, and it is molten for 50% ethyl alcohol that 20mL, concentration is added
Agent carries out Microwave Extraction, and microwave power 280W, extraction time 8min obtain extracting solution.
(3) it collects extract: extracting solution being centrifuged 3min under conditions of 4000r/min, it is always more to obtain fructus crataegi pinnatifidae Pi
Phenol.
Embodiment 7~10 and the difference of embodiment 6 are that in the step (2), the volume of the ethyl alcohol of addition is respectively
30mL、40mL、50mL、60mL。
Embodiment 11
(1) feedstock processing: fructus crataegi pinnatifidae skin is crushed with pulverizer, 60 meshes is smashed it through, obtains dry great Guo Shan
Fructus crataegi pinnatifidae skin powder is set and is put in hermetic bag to storage at the drying of cool place by short, bristly hair or beard skin powder, spare.
(2) Microwave Extraction: weighing 1g fructus crataegi pinnatifidae skin powder in extraction flask, and it is molten for 50% ethyl alcohol that 60mL, concentration is added
Agent carries out Microwave Extraction, and microwave power 210W, extraction time 8min obtain extracting solution.
(3) it collects extract: extracting solution being centrifuged 5min under conditions of 3500r/min, it is always more to obtain fructus crataegi pinnatifidae Pi
Phenol.
Embodiment 12~15 and the difference of embodiment 11 are, in the step (2), microwave power be respectively 280W,
350W、420W、490W。
Embodiment 16
(1) feedstock processing: fructus crataegi pinnatifidae skin is crushed with pulverizer, 60 meshes is smashed it through, obtains dry great Guo Shan
Fructus crataegi pinnatifidae skin powder is set and is put in hermetic bag to storage at the drying of cool place by short, bristly hair or beard skin powder, spare.
(2) Microwave Extraction: weighing 1g fructus crataegi pinnatifidae skin powder in extraction flask, and it is molten for 50% ethyl alcohol that 50mL, concentration is added
Agent carries out Microwave Extraction, and microwave power 350W, extraction time 8min obtain extracting solution.
(3) it collects extract: extracting solution being centrifuged 5min under conditions of 3500r/min, it is always more to obtain fructus crataegi pinnatifidae Pi
Phenol.
Embodiment 17~20 and the difference of embodiment 16 are, in the step (2), extraction time be respectively 16min,
24min、32min、40min。
Experimental example
1. pretreatment of raw material
Fructus crataegi pinnatifidae skin is crushed with high speed Universal pulverizer, smashes it through 60 meshes, obtains dry fructus crataegi pinnatifidae skin
Fructus crataegi pinnatifidae skin powder is set and is put in hermetic bag to storage at the drying of cool place by powder, spare.
2. the drafting of gallic acid standard curve
Gallic acid 0.0250g is accurately weighed with distilled water dissolution and constant volume is into 1000mL brown volumetric flask, obtains matter
Measure the gallic acid titer that concentration is 0.025mg/mL.No food of 0,0.5,1.0,1.5,2.0,2.5,3.0mL is pipetted respectively
Sub- standard acid solution is placed in 7 25mL volumetric flasks, then is separately added into 1.0mL forint phenol reagent, and oscillation shakes up, in 0.5-8min
4.0mL 10%Na is added2CO3Solution, uses distilled water constant volume after sufficiently shaking up, room temperature is protected from light 1h, makees blank with distilled water
Control, measures its light absorption value at 760nm.Using light absorption value as ordinate, gallic acid mass concentration is that abscissa draws standard
Curve obtains equation of linear regression y=0.1108x+0.0037, coefficient R2=0.9991.Gallic acid standard curve is such as
Shown in Fig. 1.
3. the measurement of fructus crataegi pinnatifidae skin total polyphenols
Fructus crataegi pinnatifidae skin total polyphenols are obtained according to the method for Examples 1 to 20,1.0mL extract is then accurately pipetted and is placed in
In 25mL volumetric flask, 1.0mL forint phenol reagent is added, oscillation shakes up, and 4.0mL 10%Na is added in 0.5-8min2CO3It is molten
Liquid uses distilled water constant volume after mixing, room temperature is protected from light 1h, makees blank control with distilled water, its extinction is measured at 760nm
Value.
The calculation method of polyphenol content is as follows:
The light absorption value determined in extracting solution is substituted into calibration curve equation, polyphenol in fructus crataegi pinnatifidae skin sample liquid is obtained
Concentration, substitute into following formula in fructus crataegi pinnatifidae skin total polyphenols extracted amount can be obtained.
C in formula --- the concentration (μ g/mL) of polyphenol in fructus crataegi pinnatifidae skin sample liquid；
The total volume (mL) of V --- extracting solution；
N --- extension rate；
M --- the quality (g) of weighed fructus crataegi pinnatifidae skin powder.
4. influence of the single factor test to fructus crataegi pinnatifidae skin total polyphenols extracted amount
By Examples 1 to 20 according to Examples 1 to 5,6~10,11~15 and 16~20 points be four groups, study ethyl alcohol respectively
The influence of concentration, solid-liquid ratio, microwave power and extraction time to fructus crataegi pinnatifidae skin total polyphenols extracted amount.
By the concentration of alcohol in Examples 1 to 5 be abscissa, polyphenol extracted amount is ordinate, obtains Fig. 2.It can from Fig. 2
To find out, concentration of alcohol is affected to polyphenol extraction effect, whole in downward trend after first rising, and is in concentration of alcohol
When 30%~50%, the fructus crataegi pinnatifidae skin total polyphenols extracted amount rate of climb is very fast, and when concentration of alcohol is 50%, extracted amount reaches
Maximum value.Concentration of alcohol is more than after 50%, and fructus crataegi pinnatifidae skin total polyphenols extracted amount starts to be decreased obviously, this may be because of ethyl alcohol
When concentration is smaller, the polarity of solvent and the polarity of polyphenol are kept off, and the polyphenol in solution is difficult to be leached out, as ethyl alcohol is dense
The increase of degree, the two polarity is close, and polyphenol extraction amount reaches ultimate attainment, peak value occurs, however high concentration ethanol is denaturalized cell membrane,
Cause some polyphenol that cannot be dissolved out well, meanwhile, high concentration ethanol dissolves out more other substances, in the solution with it is more
Phenol forms competitive relation, and polyphenol content is caused to reduce.
By the solid-liquid ratio in embodiment 6~10 be abscissa, polyphenol extracted amount is ordinate, obtains Fig. 3.It can from Fig. 3
To find out, with the raising of solid-liquid ratio, fructus crataegi pinnatifidae skin total polyphenols extracted amount reaches 1:50 in trend is gradually increasing, in solid-liquid ratio
(g/mL) occurs peak value when, however as continuing growing for solid-liquid ratio, polyphenol extracted amount slowly declines instead.This may be because
Solid-liquid ratio is continuously increased, and infiltrates fructus crataegi pinnatifidae skin completely, and the microwave energy that fructus crataegi pinnatifidae skin absorbs is more, cell
Broken degree is preferable, and the polyphenol amount of dissolution is more, and when solid-liquid ratio is 1:50 (g/mL), polyphenol extracted amount reaches highest.This
Afterwards, with the increase of solid-liquid ratio, polyphenol extracted amount decline, this is because higher solid-liquid ratio needs microwave under certain energy
More solution are heated, required time extends, and the energy that fructus crataegi pinnatifidae skin absorbs is also less, and the degree of clasmatosis is reduced,
With regard to less, extracted amount declines the polyphenol amount of dissolution instead.
By the microwave power in embodiment 11~15 be abscissa, polyphenol extracted amount is ordinate, obtains Fig. 4.Such as Fig. 4 institute
Show, when microwave power is promoted to 280W from 210W, fructus crataegi pinnatifidae skin total polyphenols extracted amount is gradually increased, and reaches maximum in 280W
Value；When microwave power continues to increase, polyphenol extracted amount constantly declines.This is possible as microwave power increase, and microwave energy turns
Turning to thermal energy makes system heat up, and promotes cell rupture, polyphenol substance overflows, diffusion velocity is accelerated, and polyphenol extracted amount increases.Micro-
After wave power is more than 280W, microwave power is excessively high, and the microwave that system absorbs increases, and rate of rise in temperature is accelerated, and leads to polyphenol quilt
Oxidation is decomposed, so the extracted amount of fructus crataegi pinnatifidae skin total polyphenols shows the trend being gradually reduced.
By the extraction time in embodiment 16~20 be abscissa, polyphenol extracted amount is ordinate, obtains Fig. 5.It can by Fig. 5
To find out, with being continuously increased for microwave extraction time, the trend of rising is integrally presented in fructus crataegi pinnatifidae skin total polyphenols extracted amount,
When extraction time 8min increases to 32min, the fructus crataegi pinnatifidae skin total polyphenols extracted amount rate of climb is very fast, when extraction time is 32min,
Fructus crataegi pinnatifidae skin total polyphenols extracted amount reaches peak value, and after 32min, extracted amount slowly declines.This may be because when extracting
Between increase the time of contact of solute and solvent, adequately contact overflow polyphenol from cell, on fructus crataegi pinnatifidae skin extracted amount
It rises, until reaching maximum value, but microwave extraction time is too long, a small amount of polyphenol is decomposed under the strong effect of microwave, to mention
Taken amount decline.
5. orthogonal experiment is analyzed
In order to which the interaction between the different factors of various analyses is to microwave radiation exaraction fructus crataegi pinnatifidae skin total polyphenols
It influences, orthogonal arrage L is selected according to the result that single factor experiment obtains9(34) extraction process of polyphenol in fructus crataegi pinnatifidae skin is carried out
Optimizing research, the design of orthogonal test factor level are shown in Table 2.
The design of 1 orthogonal test factor level of table
The each test example of orthogonal experiment is extracted according to the measurement and calculation method of fructus crataegi pinnatifidae skin total polyphenols in 2
Amount, the results are shown in Table 2 for experiment.
The analysis of 2 orthogonal experiments of table
By comparing very poor R value, it can be deduced that in microwave radiation exaraction fructus crataegi pinnatifidae skin during polyphenol, to polyphenol
Maximum extracted amount influence is solid-liquid ratio, followed by extraction time, is microwave power to it is the smallest to extract influence, i.e.,
The size of influence factor puts in order and is: B (solid-liquid ratio) > D (extraction time) > A (concentration of alcohol) > C (microwave power).
The present invention obtains fructus crataegi pinnatifidae skin total polyphenols using microwave radiation exaraction, extracted amount 23.00~43.80mg/g it
Between.In concentration of alcohol 50%, solid-liquid ratio 1:60g/mL, microwave power 280W, the polyphenol extracted under conditions of extraction time 40min
Amount is 43.80mg/g.Test result shows that the microwave auxiliary extracting method that the present invention uses can largely improve fructus crataegi pinnatifidae
The extracted amount of skin total polyphenols, and it is easy to operate simple, the cost of consumption was not only reduced, but also saved the energy, and had been effective exploitation
Utilize one of the desirable route of fructus crataegi pinnatifidae skin resource.The present invention for fructus crataegi pinnatifidae skin extract polyphenol theoretical foundation is provided, also for
New way has been opened up in the comprehensive utilization of fructus crataegi pinnatifidae skin.
Claims (9)
1. a kind of extracting method of fructus crataegi pinnatifidae skin total polyphenols, which comprises the following steps:
(1) feedstock processing: being ground into fructus crataegi pinnatifidae skin powder for fructus crataegi pinnatifidae skin, spare；
(2) Microwave Extraction: weighing fructus crataegi pinnatifidae skin powder that the step (1) obtains in extraction flask, be added concentration be 30~
70% ethyl alcohol carries out Microwave Extraction, and microwave power is 210~490W, and extraction time is 8~40min, obtains extracting solution；
(3) extract is collected: the extracting solution that the step (2) obtains is centrifuged 3 under conditions of 3500~4000r/min~
5min obtains fructus crataegi pinnatifidae skin total polyphenols.
2. the extracting method of fructus crataegi pinnatifidae skin total polyphenols according to claim 1, it is characterised in that: in step (2), by 1g
The solid-liquid ratio that 20~60mL solvent is added in fructus crataegi pinnatifidae skin powder adds ethyl alcohol.
3. the extracting method of fructus crataegi pinnatifidae skin total polyphenols according to claim 1 or 2, it is characterised in that: the step (2)
In, be added concentration be 40~60% ethyl alcohol, carry out Microwave Extraction, microwave power be 210~350W, extraction time be 24~
40min。
4. the extracting method of fructus crataegi pinnatifidae skin total polyphenols according to claim 1 or 2, it is characterised in that: the step (2)
In, the solid-liquid ratio of fructus crataegi pinnatifidae skin powder and ethyl alcohol is 1:20~60g/mL.
5. the extracting method of fructus crataegi pinnatifidae skin total polyphenols according to claim 4, it is characterised in that: described in step (2)
The concentration of ethyl alcohol is 50%.
6. the extracting method of fructus crataegi pinnatifidae skin total polyphenols described according to claim 1 or 2 or 5, it is characterised in that: step (2)
In, the microwave power is 280W.
7. the extracting method of polyphenol in fructus crataegi pinnatifidae skin according to claim 6, it is characterised in that: described in step (2)
The solid-liquid ratio of fructus crataegi pinnatifidae skin powder and ethyl alcohol is 1:60g/mL.
8. the extracting method of fructus crataegi pinnatifidae skin total polyphenols described according to claim 1 or 2 or 5 or 7, it is characterised in that: step
(2) in, the extraction time is 40min.
9. the extracting method of fructus crataegi pinnatifidae skin total polyphenols according to claim 1, it is characterised in that: described in step (3)
Extracting solution is centrifuged 5min under conditions of 3500r/min.
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