CN106213387A - A kind of method of propolis wax removing - Google Patents
A kind of method of propolis wax removing Download PDFInfo
- Publication number
- CN106213387A CN106213387A CN201610730728.9A CN201610730728A CN106213387A CN 106213387 A CN106213387 A CN 106213387A CN 201610730728 A CN201610730728 A CN 201610730728A CN 106213387 A CN106213387 A CN 106213387A
- Authority
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- China
- Prior art keywords
- propolis
- petroleum ether
- wax removing
- ethanol
- insoluble matter
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 21
- 229940074127 propolis wax Drugs 0.000 title claims abstract description 16
- 241000241413 Propolis Species 0.000 claims abstract description 66
- 229940069949 propolis Drugs 0.000 claims abstract description 66
- 239000003208 petroleum Substances 0.000 claims abstract description 46
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000000605 extraction Methods 0.000 claims abstract description 19
- 239000007766 cera flava Substances 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 17
- 239000000469 ethanolic extract Substances 0.000 claims abstract description 13
- 238000002481 ethanol extraction Methods 0.000 claims abstract description 7
- 239000000284 extract Substances 0.000 claims abstract description 7
- 239000012259 ether extract Substances 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- 238000003805 vibration mixing Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- 229930003935 flavonoid Natural products 0.000 abstract description 6
- 150000002215 flavonoids Chemical class 0.000 abstract description 6
- 235000017173 flavonoids Nutrition 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 230000008092 positive effect Effects 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 25
- 229930003944 flavone Natural products 0.000 description 12
- 235000011949 flavones Nutrition 0.000 description 12
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 9
- 150000002212 flavone derivatives Chemical class 0.000 description 9
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 150000002213 flavones Chemical class 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 239000013543 active substance Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 230000028327 secretion Effects 0.000 description 2
- 206010027439 Metal poisoning Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 210000004907 gland Anatomy 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 208000010501 heavy metal poisoning Diseases 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 235000009048 phenolic acids Nutrition 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Jellies, Jams, And Syrups (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
Abstract
The present invention relates to food processing technology field, a kind of method being specifically related to propolis wax removing, comprise the following steps: (1) Feedstock treating: natural propolis roguing, pulverize；(2) Petroleum ether extraction Cera Flava: propolis mixes in petroleum ether；Sucking filtration, extracts 2 times, and the extract of 2 times volatilizees dry naturally, for Cera Flava extracted amount；(3) ethanol extraction propolis: by the most tolerant the acting in ethanol of (2) 2 extractions of step, generate ethanol extract, then be spin-dried in Rotary Evaporators, obtain propolis weight；The present invention is to carry out at normal pressure and temperature 25 DEG C, it is not necessary to high temperature and high pressure environment, will not have an impact the Flavonoid substances content in propolis, and method is simple to operate, and propolis wax removing rate is high, improves the extraction ratio of Flavonoids in Propolis class material；Propolis is carried out wax removing process there is positive effect.
Description
Technical field
The present invention relates to food processing technology field, a kind of method being specifically related to propolis wax removing.
Background technology
Propolis be Apis herborization leaf bud or bark crack secretion resin and be mixed into mandibular gland secretions and Cera Flava and
The fragrant solids become, is mainly made up of Cera Flava, resin and volatile material；Hair glue is not carried out wax removing meeting
Affect the extraction ratio of Flavonoids in Propolis class material, and containing heavy metal in Cera Flava, be eaten for a long time easy heavy metal poisoning.
Existing propolis wax removing technology has water to carry wax removing, supercritical CO2Wax removing, alcohol extraction merceration wax removing etc.；Water carries wax removing
Wax removing effect is realized by the temperature controlling water and the material ratio of propolis and water；Supercritical CO2Wax removing is under a certain pressure,
CO with certain flow rate2Propolis is carried out extracting wax removing by air-flow；Alcohol extraction merceration wax removing is that ethanol extracts of propolis is carried out merceration process
Carry out wax removing.
Existing propolis wax removing technology has cost high, and technique is loaded down with trivial details, and high to temperature requirement, wax removing efficiency is low, elapsed time
The shortcomings such as length；Although it is the lowest that water puies forward wax removing wax removing rate, but propolis is understood some phenolic acids active component and is dissolved in water and loses
Go, and need under 70 DEG C of hot environments, can in propolis main active substances flavones content exist impact；Supercritical
CO2Wax removing is to need high-temperature heating environment and cost is high, technique is loaded down with trivial details, and same high temperature and high pressure environment, general pressure is
30MPa, temperature is 60 DEG C, the impact that can there is the main active substances flavones content in propolis, can affect Flavonoids in Propolis
Extraction ratio；Alcohol extraction merceration wax removing need not high pressure-temperature heat treated, but wax removing efficiency is the lowest, it is impossible to meets wanting of wax removing
Ask.
Summary of the invention
For solving the problem that above-mentioned propolis wax removing exists, a kind of method that the invention provides propolis wax removing, including following
Step:
(1) Feedstock treating: by natural propolis roguing, is placed in pulverizer, grinds；
(2) Petroleum ether extraction Cera Flava:
The most respectively propolis powder, petroleum ether are proportionally added in tool plug conical flask；Under the conditions of room temperature 25 DEG C, ultrasonic vibration stirs
Mix so that it is mixing；Sucking filtration, separates insoluble matter A and petroleum ether extract A；
B. the most tolerant A sucking filtration in upper step a obtained and a certain amount of petroleum ether add in tool plug conical flask；Room temperature 25 DEG C
Under the conditions of, ultrasonic vibration stirs so that it is mixing；Sucking filtration, isolates insoluble matter B and petroleum ether extract B；
C. volatilized dry take out petroleum ether extract A caught on a filter and petroleum ether extract B, weigh, be the Cera Flava of extraction naturally
Weight；
D. repeat above a, b, step c n time, obtain the gravimetric value of n part Cera Flava, calculate average yield, wax removing rate can be obtained；
(3) ethanol extraction propolis:
E. the insoluble matter B that will obtain in step (2), adds insoluble matter B, 75% ethanol in tool plug conical flask the most respectively；?
Under the conditions of room temperature 25 DEG C, ultrasonic vibration stirs so that it is mixing；Separate insoluble matter C and ethanol extract, ethanol extract is revolved
Turn evaporimeter to be spin-dried for；
F. the extract after being spin-dried for is weighed, be propolis weight；
G. repeat above e, f step n time, obtain n part propolis gravimetric value, calculate average yield, propolis yield can be obtained.
In described step (2) a, b, propolis powder, the weight ratio of petroleum ether are 1:4 ~ 1:6, described supersonic frequency is 35 ~
45KHz, ultrasonic vibration mixing time is 40 ~ 50min.
As preferably, in described step (2) a, b, propolis powder, the weight ratio of petroleum ether are 1:5, and described supersonic frequency is
40KHz, ultrasonic vibration mixing time is 45min.
In described step (3) e, insoluble matter B:75% ethanol weight ratio is 1:9 ~ 1:11；Described supersonic frequency is 35 ~ 45KHz,
Ultrasonic vibration mixing time is 40 ~ 50min, described in be spin-dried for condition and be: temperature is 50 DEG C, pressure is 0.09 ~ 0.10MPa, rotating speed
It is 55 ~ 65rpm.
As preferably, in described step (3) e, insoluble matter B:75% ethanol weight ratio is 1:10；Described supersonic frequency is
40KHz, ultrasonic vibration mixing time is 45min, described in be spin-dried for condition and be: temperature is 50 DEG C, pressure is 0.09MPa, rotating speed is
60rpm。
Beneficial effects of the present invention:
The present invention is to carry out at normal pressure and temperature 25 DEG C, it is not necessary to high temperature and high pressure environment, will not be to the Flavonoid substances in propolis
Content has an impact, and method is simple to operate, and propolis wax removing rate is high, improves the extraction ratio of Flavonoids in Propolis class material；The present invention
Propolis wax removing rate, up to 38.5%, carries the 37.6% of wax removing higher than water, supercritical CO222.5% and alcohol extraction merceration wax removing of wax removing
15.3%；And need not the experiment links such as High Temperature High Pressure, liposoluble ingredient does not lose, and will not contain total flavones in propolis
Amount plays impact；Propolis to non-wax removing and the propolis by this method wax removing carry out general flavone content detection, and result shows, removes
After wax, in propolis, general flavone content is 2.46 times of the general flavone content of non-wax removing propolis, propolis carries out wax removing process and has long-pending
Pole meaning.
Detailed description of the invention
One, petroleum ether wax removing experiment
Embodiment 1:
(1) weigh natural propolis 10g, be placed in mortar, grind；
(2) Petroleum ether extraction Cera Flava:
A. according to propolis powder: petroleum ether weight ratio is 1:5, respectively propolis powder, petroleum ether are added in tool plug conical flask；In room temperature
Under the conditions of 25 DEG C, supersonic frequency is 40KHz, ultrasonic vibration stirring 45min so that it is mixing；Sucking filtration, separates insoluble matter A1 and oil
Ether extracting solution A1；
B. the most tolerant A1 sucking filtration in upper step a obtained, by insoluble matter A1: petroleum ether weight ratio is 1:5, respectively by insoluble matter
A1, petroleum ether add in tool plug conical flask；Under the conditions of room temperature 25 DEG C, supersonic frequency is 40KHz, ultrasonic vibration stirring 45min,
Make it mix；Sucking filtration, separates, obtains insoluble matter B1 and petroleum ether extract B1；
C. volatilized dry take out petroleum ether extract A1 caught on a filter and petroleum ether extract B1, weigh, for 3.94g, be naturally
The weight of the Cera Flava extracted；
(3) ethanol extraction propolis:
E. the insoluble matter B1 that will obtain in step (2), by insoluble matter B1:75% ethanol weight ratio 1:10, respectively by insoluble matter B1,
75% ethanol adds in tool plug conical flask；Under the conditions of room temperature 25 DEG C, supersonic frequency are 40KHz, ultrasonic vibration 45min so that it is mixed
Even；Separate insoluble matter C1 and ethanol extract, obtain final insoluble matter C1, be weighed as 1.39g；Ethanol extract rotary evaporation
Instrument is spin-dried for；Rotary Evaporators is to be 0.09MPa at temperature 50 C, pressure, under the conditions of rotating speed is 60rpm, be spin-dried for；
F. the extract after being spin-dried for is weighed, for 4.52g, be propolis weight.
Embodiment 2:
(1) weigh natural propolis 10g, be placed in mortar and grind；
(2) Petroleum ether extraction Cera Flava:
A. according to propolis powder: petroleum ether weight ratio is 1:5, respectively propolis powder, petroleum ether are added in tool plug conical flask；In room temperature
Under the conditions of 25 DEG C, supersonic frequency is 40KHz, ultrasonic vibration stirring 45min so that it is mixing；Sucking filtration, separates insoluble matter A2 and oil
Ether extracting solution A2；
B. the most tolerant A2 sucking filtration in upper step a obtained, by insoluble matter A2: petroleum ether weight ratio is 1:5, respectively by insoluble matter
A2, petroleum ether add in tool plug conical flask；Under the conditions of room temperature 25 DEG C, supersonic frequency is 40KHz, ultrasonic vibration stirring 45min,
Make it mix；Sucking filtration, separates, obtains insoluble matter B2 and petroleum ether extract B2；
C. volatilized dry take out petroleum ether extract A2 caught on a filter and petroleum ether extract B2, weigh, for 3.83g, be naturally
The weight of the Cera Flava extracted；
(3) ethanol extraction propolis:
E. the insoluble matter B2 that will obtain in step (2), by non-miscible compound B2:75% ethanol weight ratio 1:10, respectively by insoluble matter
B2,75% ethanol add in tool plug conical flask；Under the conditions of room temperature 25 DEG C, supersonic frequency are 40KHz, ultrasonic vibration 45min, make
Its mixing；Separate insoluble matter C2 and ethanol extract, obtain final insoluble matter C2, weigh, for 1.35g；Ethanol extract is revolved
Turn evaporimeter to be spin-dried for；Rotary Evaporators is to be 0.09MPa at temperature 50 C, pressure, under the conditions of rotating speed is 60rpm, be spin-dried for；
F. the extract after being spin-dried for is weighed, for 4.49g, be propolis weight.
Embodiment 3:
(1) weigh natural propolis 10g, be placed in mortar and grind；
(2) Petroleum ether extraction Cera Flava:
A. according to propolis powder: petroleum ether weight ratio is 1:5, respectively propolis powder, petroleum ether are added in tool plug conical flask；In room temperature
Under the conditions of 25 DEG C, supersonic frequency is 40KHz, ultrasonic vibration stirring 45min so that it is mixing；Sucking filtration, separates insoluble matter A3 and oil
Ether extracting solution A3；
B. the most tolerant A3 sucking filtration in upper step a obtained, by insoluble matter A3: petroleum ether weight ratio is 1:5, respectively by insoluble matter
A3, petroleum ether add in tool plug conical flask；Under the conditions of room temperature 25 DEG C, supersonic frequency is 40KHz, ultrasonic vibration stirring 45min,
Make it mix；Sucking filtration, separates, obtains insoluble matter B3 and petroleum ether extract B3；
C. volatilized dry take out petroleum ether extract A3 caught on a filter and petroleum ether extract B3, weigh, for 3.78g, be naturally
The weight of the Cera Flava extracted；
(3) ethanol extraction propolis:
E. the insoluble matter B3 that will obtain in step (2), is 1:10 by non-miscible compound B3:75% ethanol weight ratio, respectively by insoluble
Thing B3,75% ethanol add in tool plug conical flask；Under the conditions of room temperature 25 DEG C, supersonic frequency are 40KHz, ultrasonic vibration 45min,
Make it mix；Separate insoluble matter C3 and ethanol extract, obtain final insoluble matter C3, weigh, for 1.47g；Ethanol extract is used
Rotary Evaporators is spin-dried for；Rotary Evaporators is to be 0.09MPa at temperature 50 C, pressure, under the conditions of rotating speed is 60rpm, revolve
Dry；
F. the extract after being spin-dried for is weighed, for 4.57g, be propolis weight.
Embodiment 1,2,3 interpretation of result is as follows:
| Embodiment | 1 | 2 | 3 |
| Natural propolis (g) | 10 | 10 | 10 |
| Petroleum ether extraction Cera Flava amount (g) | 3.94 | 3.83 | 3.78 |
| Ethanol extraction propolis amount (g) | 4.52 | 4.49 | 4.57 |
| Final insoluble matter (g) | 1.39 | 1.35 | 1.47 |
Can calculate the meansigma methods of 3 embodiments from upper table, the average wax removing rate of propolis is 38.5%, and the average of propolis obtains
Rate is 45.2%.
Two, total flavone content in propolis test experience
1, propolis and above-described embodiment 1,2,3 of weighing non-wax removing obtain each 3g of wax removing propolis；
2, it is separately added into 75% ethanol 60ml, merceration 1h, supersound extraction twice, each 45min, is cooled to room temperature；
3, filtering ethanol extract, constant volume is in 100ml volumetric flask, standby；
4, general flavone content is detected by GBT 24283-2009 national standard method.
Result is as follows:
| Embodiment | 1 | 2 | 3 |
| Wax removing total flavone content in propolis (mg/g) | 298.92 | 298.43 | 297.35 |
| Non-wax removing total flavone content in propolis (mg/g) | 120.34 | 121.28 | 121.72 |
Upper table result shows, in wax removing propolis, general flavone content is averagely 2.46 times of the general flavone content of non-wax removing propolis, logical
Cross this method propolis is carried out wax removing process there is positive effect.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope that the invention discloses, the change that can readily occur in or replacement,
All should contain within protection scope of the present invention.
Claims (5)
1. the method for a propolis wax removing, it is characterised in that comprise the following steps:
(1) Feedstock treating: by natural propolis roguing, is placed in pulverizer, grinds；
(2) Petroleum ether extraction Cera Flava:
The most respectively propolis powder, petroleum ether are proportionally added in tool plug conical flask；Under the conditions of room temperature 25 DEG C, ultrasonic vibration stirs
Mix so that it is mixing；Sucking filtration, separates insoluble matter A and petroleum ether extract A；
B. the most tolerant A sucking filtration in upper step a obtained and a certain amount of petroleum ether add in tool plug conical flask；Room temperature 25 DEG C
Under the conditions of, ultrasonic vibration stirs so that it is mixing；Sucking filtration, isolates insoluble matter B and petroleum ether extract B；
C. volatilized dry take out petroleum ether extract A caught on a filter and petroleum ether extract B, weigh, be the Cera Flava of extraction naturally
Weight；
D. repeat above a, b, step c n time, obtain the gravimetric value of n part Cera Flava, calculate average yield, wax removing rate can be obtained；
(3) ethanol extraction propolis:
E. the insoluble matter B that will obtain in step (2), adds insoluble matter B, 75% ethanol in tool plug conical flask the most respectively；?
Under the conditions of room temperature 25 DEG C, ultrasonic vibration stirs so that it is mixing；Separate insoluble matter C and ethanol extract, ethanol extract is revolved
Turn evaporimeter to be spin-dried for；
F. the extract after being spin-dried for is weighed, be propolis weight；
G. repeat above e, f step n time, obtain n part propolis gravimetric value, calculate average yield, propolis yield can be obtained.
The method of a kind of propolis wax removing the most according to claim 1, it is characterised in that propolis in described step (2) a, b
Powder, the weight ratio of petroleum ether are 1:4 ~ 1:6, and described supersonic frequency is 35 ~ 45KHz, and ultrasonic vibration mixing time is 40 ~ 50min.
The method of a kind of propolis wax removing the most according to claim 2, it is characterised in that propolis in described step (2) a, b
Powder, the weight ratio of petroleum ether are 1:5, and described supersonic frequency is 40KHz, and ultrasonic vibration mixing time is 45min.
The method of a kind of propolis wax removing the most according to claim 1, it is characterised in that insoluble matter B in described step (3) e:
75% ethanol weight ratio is 1:9 ~ 1:11；Described supersonic frequency is 35 ~ 45KHz, and ultrasonic vibration mixing time is 40 ~ 50min, institute
Stating the condition of being spin-dried for is: temperature is 50 DEG C, pressure is 0.09 ~ 10MPa, rotating speed is 55 ~ 65rpm.
The method of a kind of propolis wax removing the most according to claim 4, it is characterised in that insoluble matter B in described step (3) e:
75% ethanol weight ratio is 1:10；Described supersonic frequency is 40KHz, and ultrasonic vibration mixing time is 45min, described in be spin-dried for condition
For: temperature be 50 DEG C, pressure be 0.09MPa, rotating speed be 60rpm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610730728.9A CN106213387A (en) | 2016-08-26 | 2016-08-26 | A kind of method of propolis wax removing |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610730728.9A CN106213387A (en) | 2016-08-26 | 2016-08-26 | A kind of method of propolis wax removing |
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| CN106213387A true CN106213387A (en) | 2016-12-14 |
Family
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| CN201610730728.9A Pending CN106213387A (en) | 2016-08-26 | 2016-08-26 | A kind of method of propolis wax removing |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106805177A (en) * | 2017-01-06 | 2017-06-09 | 重庆师范大学 | A kind of extracting method of propolis |
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| CN1839890A (en) * | 2006-01-27 | 2006-10-04 | 兰州大学 | Method for preparing water-soluble bee glue product and use thereof |
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2016
- 2016-08-26 CN CN201610730728.9A patent/CN106213387A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1839890A (en) * | 2006-01-27 | 2006-10-04 | 兰州大学 | Method for preparing water-soluble bee glue product and use thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106805177A (en) * | 2017-01-06 | 2017-06-09 | 重庆师范大学 | A kind of extracting method of propolis |
| CN106805177B (en) * | 2017-01-06 | 2020-04-07 | 重庆师范大学 | Propolis extraction method |
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Application publication date: 20161214 |