CN104523767B - A kind of method for extracting Flavonoid substances in cacumen biotae - Google Patents
A kind of method for extracting Flavonoid substances in cacumen biotae Download PDFInfo
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Abstract
The invention provides it is a kind of extract cacumen biotae in Flavonoid substances method, by cacumen biotae clean, drying after crush, obtain cacumen biotae powder, then add water, be uniformly mixed to get mixed liquor；Mixed liquor is freezed 10~24 hours at a temperature of 40~20 DEG C, placed at room temperature until its thawing；Repeat frost room temperature thawing step 2~3 times；Add ethanol fully to mix, carry out ultrasonic wave extraction after 1~3h of immersion, centrifuge, take supernatant, freeze, obtain crude product；Crude product is configured to the solution that concentration is 1~3mg/mL, progress saturation absorption in macroporous resin column is added drop-wise to, removing impurity is eluted with water after absorption, again eluant, eluent is used as with 60~80% ethanol, recycling design and concentration are carried out to eluant, eluent, is finally freezed, that is, obtains Flavonoid substances.This method recovery rate is high, pollution-free, cost is low.
Description
Technical field
The present invention relates to a kind of extracting method of Flavonoid substances, and in particular to one kind extracts flavonoids thing from cacumen biotae
The method of matter.
Background technology
In recent years, due to the progress of free radical life science, make with very strong anti-oxidant and elimination Free Radical
Flavonoid substances are by unprecedented attention.Its antioxidation is stronger than VE 50 times, stronger than VC 20 times, and can pass through blood-brain barrier
Brain is reached, the disease of central nervous system is prevented and treated, especially the maintenance of skin, rejuvenation and blood vessel antiinflammatory action are especially shown
Write.At present, flavone compound report is extracted from ginkgo leaf, perilla leaf, cypress leaf, sophora flower, Chinese toon tender leaf more.But from
Flavonoid substances are extracted in cacumen biotae actually rare.
Cacumen biotae is the dry twig tip and leaf of arbor-vitae, containing a variety of active skull cap components such as flavonoids, tannin, essential oil,
Have effects that Flavonoid substances are them in cooling blood and hemostasis, preventing phlegm from forming and stopping coughing, wind-dispelling wet down, growing and blacking hair, Sweeling-eliminating medicine powder poison, cacumen biotae
One of most important composition.Thus, there be very the extraction of flavone compound for the development of Food Science and medical science in cacumen biotae
Important influence.
The extracting method applied to cacumen biotae Flavonoid substances mainly has at present：It is organic solvent extractionprocess, enzyme extraction method, super
Sound extraction method, microwave loss mechanisms.Wherein, organic solvent extraction is the most commonly used method used both at home and abroad, but this side
Method cycle length, step are more, the residual of organic solvent is had in low yield, and product, have an impact to product quality after extraction；Enzyme is carried
Follow the example of and have to keep optimum temperature, optimal pH, higher is required to the condition control entirely reacted；Ultrasonic wave extraction
Extraction efficiency is greatly improved, extraction time is shortened, saves solvent, and eliminates destruction of the high temperature to extract component,
But efficiency is low during a large amount of extractions；Microwave loss mechanisms, are permitted with quick, solvent load is few, recovery rate is high, cost is low and quality is good etc.
Many advantages, but the composition of its finished product is not highly stable；It is clear that either which kind of extractive technique have itself deficiency and
The characteristics of limitation, and this invention is using freeze thawing and ultrasonic technology combined extracting, freeze-thaw technology is：Cell can form ice
Grain is swelled, crushed, Flavonoid substances is fully discharged, and also protect with while increasing remaining cytosol salinity
Hold activity.The technology is a kind of extracting method efficiently, environmentally friendly.It yet there are no and extract cacumen biotae flavonoids using freeze-thaw technology
The report of material.Experiment proves to use freeze thawing and ultrasonic technology combined extracting efficiently and environmental protection.
The content of the invention
Goal of the invention：For the weak point of the extracting method of above-mentioned Flavonoid substances, the invention provides it is a kind of efficiently,
The extracting method of environmental protection.
Technical scheme：This method is carried out according to the following steps：
(1) cacumen biotae cleaned, dry, crushed, cross 40 mesh sieves, obtain cacumen biotae powder, then add water, uniform mixing；
The water and the mass ratio of cacumen biotae added is about 5：1.
(2) mixed liquor for obtaining step (1) is freezed 10~24 hours at a temperature of -40~-20 DEG C, is placed at room temperature
Until its thawing；Repeat frost-thawing step 2~3 times；In this way, cell can form ice pellets and increase remaining cytosol salinity
While, it is swelled, crushes.Flavonoid substances is fully discharged, and also keep activity.
(3) add ethanol into mixed liquor obtained by step (2) fully to mix, the volume ratio of ethanol and mixed liquor is about 1：1,
Soak after 1~3h, carry out ultrasonic wave extraction, ultrasonic power is 60~100W；Ultrasonic temperature is 40~80 DEG C；Ultrasonic time is 20
~60min；Destruction of the cavitation of ultrasound to cell membrane contributes to the release and dissolution of flavone compound, and ultrasonic wave makes to carry
Take liquid constantly to shake, contribute to solutes accumulation.Therefore, supercritical ultrasonics technology substantially reduces extraction time, improves active ingredient
Extraction rate, the utilization rate of raw material.Ultrasound is centrifuged after terminating, and takes supernatant, freezes, obtains crude product.
(4) crude product is configured to the solution that concentration is 1~3mg/mL, is added drop-wise to progress saturation absorption in macroporous resin column,
Removing impurity is eluted with water after absorption, then recycling design and concentration are carried out to eluant, eluent as eluant, eluent with 60~80% ethanol
Processing, is finally freezed, that is, obtains Flavonoid substances.Described macroreticular resin is D-101, AB-8 or DM-130.It is described molten
The dripping quantity of liquid is 1.5 times of column volume；The consumption of water and ethanol is 5 times of column volume.
Further, it has been found that if after step (2) terminates, gained mixed liquor being freezed again, is subsequently placed in
Melt under ultrasound environments, ultrasonic power is 60~100W；Ultrasonic time is 60~90min, because the fuel factor of ultrasonic wave makes water
Temperature increases, and has water-bath effect to raw material, and temperature is increased to 35~40 DEG C naturally, not only causes mixed liquor fast melt, Er Qieke
To promote the release and dissolution of flavone compound.After melting under ultrasound environments, step (3), (4), the method institute are being carried out
Obtained product recovery rate is greatly improved, and is determined cacumen biotae Flavonoid substances recovery rate and is up to 18.2%.
Beneficial effect：The invention has the characteristics that：Integrated artistic designs advantages of simple, and creative combines a variety of skills
Art, compensate for the deficiency of monotechnics, substantially increase the recovery rate of Flavonoid substances；Due to the particularity of cacumen biotae, this hair
In bright extraction process, relatively low temperature is maintained, the activity of cacumen biotae Flavonoid substances is maintained well so that product
It is highly stable；Solvent load of the present invention is small and is easily recycled, cost-effective；Water is only used in extraction process and two kinds of ethanol is molten
Agent, other solvents such as chloroform, ethyl acetate are not introduced, environmentally safe；These features all largely meet
The requirement of industrialized production.
Embodiment：
Below by way of specific embodiment, the present invention is further described：
Embodiment 1
Fresh cacumen biotae is taken, weighs, clean, is dried in the shade naturally after 60 DEG C of drying in baking oven as raw material；It is crushed to 40
Mesh, obtains cacumen biotae powder；Precise 20g cacumen biotae powder, adds 100mL water, cacumen biotae mixed liquor is made；Cacumen biotae is mixed
Liquid is freezed at -20 DEG C, and room temperature is taken out after 24h and is melted, so repeatedly for three times；Absolute ethyl alcohol 100mL is added, it is fully mixed
It is even, after immersion 2h, carry out ultrasonic wave extraction：Ultrasonic power 60W；Ultrasonic time 20min；40 DEG C of ultrasonic temperature；Centrifuge, take
Supernatant.Supernatant is positioned in freeze dryer and carries out frozen dried, crude product is obtained；It is 1mg/mL by the accurate compound concentration of crude product
Solution, be added drop-wise in AB-8 macroporous resin columns progress saturation absorption, maximum applied sample amount is 1.5 times of column volumes, first with 5 times of cylinders
Long-pending water elution removes impurity, then with 60% ethanol elution of 5 times of column volumes, collects eluent, concentration, freezes, obtain cacumen biotae
Flavonoid substances sample 2.42g.
Determine：Using ultraviolet spectrophotometry, using rutin as standard reference material, rutin standard curve is drawn, side is determined
The content of CedarLeaves Flavonoid substances.
(1) drafting of standard curve
Rutin standard items 1.0mg accurately is weighed, 25.0mL is settled to for 50% ethanol with concentration.
Accurate rutin standard items (48 μ g/mL) 0.5,1.0,2.0,3.0,4.0, the 5.0mL of drawing divides in 6 colorimetric cylinders
Do not shaken up, be made in the same way of to 5.0mL, 0.1M aluminum trichloride solution 3.0mL and 1M liquor kalii acetici 5.0mL with 50% ethanol
Blank control；40min is placed, question response completely, determines absorbance at 415nm wavelength.It is with rutin standard concentration (C)
Abscissa, absorbance (A) is that ordinate draws standard curve.
(2) measure of cacumen biotae Flavonoid substances recovery rate
Recovery rate Y%=m1/m2× 100%
In formula:m1To obtain the quality (g) of cacumen biotae Flavonoid substances sample；
m2To use the quality (g) of cacumen biotae powder.
(3) in Cacumen Platycladi extract Flavonoid substances content measure
Weigh 5mg extracts to be placed in 25mL volumetric flasks, prepare solution by above-mentioned rutin standard curve method for drafting, and survey
Its absorbance.Flavonoid substances content in extract is calculated by standard curve.
Content P%=CVD × 10-3/ m × 100%
In formula:C is the Flavonoid substances concentration (mg/mL) of the test solution calculated by standard curve；
V is testing sample solution cumulative volume (mL)；
D is the extension rate of test solution；
M is the extract quality (mg) weighed.
According to above-mentioned formula, cacumen biotae Flavonoid substances recovery rate is obtained for 12.1%, and Flavonoid substances contain in extract
Measure as 82.0%；
Tied using general extraction methods (the same without frost-thawing processing, no ultrasonic assistant, other conditions) gained
It is really：Flavonoid substances recovery rate is 3.6%, and Flavonoid substances content is 29.3% in extract；It can be seen that, the present invention is using jelly
Melt and extract cacumen biotae Flavonoid substances with ultrasonic combined technology, high recovery rate, Functionality, quality and appealing design and free of contamination product can be obtained.
Embodiment 2
Precise 20g cacumen biotae powder, adds 100mL water, cacumen biotae mixed liquor is made；By cacumen biotae mixed liquor -40
Freezed at DEG C, room temperature is taken out after 10h and is melted, so repeatedly for three times；Absolute ethyl alcohol 100mL is added, is fully mixed, 2h is soaked
Afterwards, ultrasonic wave extraction is carried out：Ultrasonic power 80W；Ultrasonic time 40min；60 DEG C of ultrasonic temperature；Centrifuge, take supernatant.Will
Supernatant, which is positioned in freeze dryer, carries out frozen dried, obtains crude product；By the solution that the accurate compound concentration of crude product is 2mg/mL, drop
Progress saturation absorption in D-101 macroporous resin columns is added to, maximum applied sample amount is 1.5 times of column volumes, first with the washing of 5 times of column volumes
Decontamination is removed, then with 70% ethanol elution of 5 times of column volumes, collects eluent, concentration, freeze, produce arbor-vitae leaf flavonoid
Material sample 2.74g.
Assay method be the same as Example 1：It is flavonoids thing in 13.7%, extract to determine cacumen biotae Flavonoid substances recovery rate
Matter content is 83.7%.
Tied using general extraction methods (the same without frost-thawing processing, no ultrasonic assistant, other conditions) gained
It is really：Flavonoid substances recovery rate is 3.8%, and Flavonoid substances content is 28.1% in extract；
Embodiment 3
Precise 20g cacumen biotae powder, adds 100mL water, cacumen biotae mixed liquor is made；By cacumen biotae mixed liquor -20
Freezed at DEG C, room temperature is taken out after 24h and is melted, so repeatedly for three times；Absolute ethyl alcohol 100mL is added, is fully mixed, 3h is soaked
Afterwards, ultrasonic wave extraction is carried out：Ultrasonic power 100W；Ultrasonic time 60min；80 DEG C of ultrasonic temperature；Centrifuge, take supernatant.
Supernatant is positioned in freeze dryer and carries out frozen dried, crude product is obtained；By the solution that the accurate compound concentration of crude product is 3mg/mL,
Progress saturation absorption in D-130 macroporous resin columns is added drop-wise to, maximum applied sample amount is 1.5 times of column volumes, first with the water of 5 times of column volumes
Elution removes impurity, then with 80% ethanol elution of 5 times of column volumes, collects eluent, concentration, freezes, produce cacumen biotae flavones
Class material sample 2.88g.
Assay method be the same as Example 1：It is flavonoids thing in 14.4%, extract to determine cacumen biotae Flavonoid substances recovery rate
Matter content is 80.5%；
Tied using general extraction methods (the same without frost-thawing processing, no ultrasonic assistant, other conditions) gained
It is really：Flavonoid substances recovery rate is 3.9%, and Flavonoid substances content is 26.5% in extract.
Embodiment 4
Precise 20g cacumen biotae powder, adds 100mL water, cacumen biotae mixed liquor is made；By cacumen biotae mixed liquor -20
Freezed at DEG C, room temperature is taken out after 24h and is melted, so repeatedly for three times；Absolute ethyl alcohol 100mL is added, is fully mixed, 2h is soaked
Afterwards, ultrasonic wave extraction is carried out：Ultrasonic power 100W；Ultrasonic time 40min；70 DEG C of ultrasonic temperature；Centrifuge, take supernatant.
Supernatant is positioned in freeze dryer and carries out frozen dried, crude product is obtained；By the solution that the accurate compound concentration of crude product is 3mg/mL,
Progress saturation absorption in D-101 macroporous resin columns is added drop-wise to, maximum applied sample amount is 1.5 times of column volumes, first with the water of 5 times of column volumes
Elution removes impurity, then with 80% ethanol elution of 5 times of column volumes, collects eluent, concentration, freezes, produce cacumen biotae flavones
Class material sample 2.96g.
Assay method be the same as Example 1：It is flavonoids thing in 14.8%, extract to determine cacumen biotae Flavonoid substances recovery rate
Matter content is 84.7%；
Tied using general extraction methods (the same without frost-thawing processing, no ultrasonic assistant, other conditions) gained
It is really：Flavonoid substances recovery rate is 4.1%, and Flavonoid substances content is 30.2% in extract；
Flavonoid substances in cacumen biotae, which are extracted, using method of the present invention compared with general extraction methods, tests knot
Fruit see the table below：
Table 1
As can be seen from Table 1 flavonoids thing is extracted this invention takes the technology of frost-thawing and ultrasonic assistant
Flavonoid substances content is far longer than general extraction methods in matter, gained cacumen biotae Flavonoid substances recovery rate and extract.
Recovery rate 14% or so, and product is stable, Flavonoid substances content is more than 80% in extract.
Further, we have studied the application of ultrasonic wave in frost-melting process.Specific embodiment is as follows：
Embodiment 5
Precise 20g cacumen biotae powder, adds 100mL water, cacumen biotae mixed liquor is made；By cacumen biotae mixed liquor -20
Freezed at DEG C, room temperature is taken out after 24h and is melted, so repeatedly for three times；Aqueous, which is positioned in freeze dryer, carries out frozen dried, obtains
To crude product；By the solution that the accurate compound concentration of crude product is 3mg/mL, progress saturation absorption in D-101 macroporous resin columns is added drop-wise to,
Maximum applied sample amount is 1.5 times of column volumes, first with the water elution removing impurity of 5 times of column volumes, then with 80% ethanol of 5 times of column volumes
Elution, collects eluent, concentration, freezes, produce cacumen biotae Flavonoid substances sample 1.16g.
Assay method be the same as Example 1：Flavonoid substances content in cacumen biotae Flavonoid substances recovery rate 5.8%, extract
For 83.9%；
Embodiment 5-1
Precise 20g cacumen biotae powder, adds 100mL water, cacumen biotae mixed liquor is made；By cacumen biotae mixed liquor -20
Freezed at DEG C, room temperature is taken out after 24h and is melted, it is so repeatedly secondary；Then freezed, taken after 24h at -20 DEG C again
Go out and melted under ultrasound environments, due to the fuel factor of ultrasound, temperature is increased to 35 DEG C, after about 80min melts, aqueous naturally
It is positioned in freeze dryer and carries out frozen dried, obtains crude product；By the solution that the accurate compound concentration of crude product is 3mg/mL, D- is added drop-wise to
Saturation absorption is carried out in 101 macroporous resin columns, maximum applied sample amount is 1.5 times of column volumes, is first removed with the water elution of 5 times of column volumes
Impurity, then with 80% ethanol elution of 5 times of column volumes, collect eluent, concentration, freeze, produce cacumen biotae Flavonoid substances sample
Product 2.38g.
Assay method be the same as Example 1：Flavonoid substances content in cacumen biotae Flavonoid substances recovery rate 11.9%, extract
For 84.1%；
Embodiment 4-1
Precise 20g cacumen biotae powder, adds 100mL water, cacumen biotae mixed liquor is made；By cacumen biotae mixed liquor -20
Freezed at DEG C, room temperature is taken out after 24h and is melted, it is so repeatedly secondary；Then freezed, taken after 24h at -20 DEG C again
Go out and melted under ultrasound environments, due to the fuel factor of ultrasound, temperature is increased to 36 DEG C, after about 80min melts naturally, adds
Absolute ethyl alcohol 100mL, is fully mixed, and after immersion 2h, carries out ultrasonic wave extraction：Ultrasonic power 100W；Ultrasonic time 40min；It is super
Sound temperature 70 C；Centrifuge, take supernatant.Residue is carried out to processing 1 time as stated above, merges supernatant；By supernatant
It is positioned in freeze dryer and carries out frozen dried, obtains crude product；By the solution that the accurate compound concentration of crude product is 3mg/mL, D- is added drop-wise to
Saturation absorption is carried out in 101 macroporous resin columns, maximum applied sample amount is 1.5 times of column volumes, is first removed with the water elution of 5 times of column volumes
Impurity, then with 80% ethanol elution of 5 times of column volumes, collect eluent, concentration, freeze, produce cacumen biotae Flavonoid substances sample
Product 3.64g.
Assay method be the same as Example 1：It is flavonoids thing in 18.2%, extract to determine cacumen biotae Flavonoid substances recovery rate
Matter content is 84.3%.
Result of the test see the table below：
Table 2
As seen from Table 2 in freezing-melting process, melted under ultrasound environments, can effectively improve arbor-vitae
The recovery rate of leaf flavonoid material.Because melting under the environment of ultrasound, because the fuel factor of ultrasonic wave makes water temperature basic
Maintain 35~40 DEG C so that mixed liquor fast melt, at the same its cavitation can promote the release of flavone compound with
Dissolution, improves the recovery rate of cacumen biotae Flavonoid substances.
Claims (8)
1. a kind of method for extracting Flavonoid substances in cacumen biotae, it is characterised in that carry out according to the following steps：
(1) by cacumen biotae clean, drying after crush, obtain cacumen biotae powder, then add water, be uniformly mixed to get mixed liquor；
(2) mixed liquor is freezed 10~24 hours at a temperature of -40~-20 DEG C, placed at room temperature until its thawing；Repeat ice
Jelly-room temperature thawing step 2~3 times；
(3) ethanol is added into mixed liquor obtained by step (2) fully to mix, after 1~3h of immersion, carry out ultrasonic wave extraction, centrifugation
Separation, takes supernatant, freezes, obtains crude product；Ultrasonic power is 60~100W；Ultrasonic time is 20~60min；Ultrasonic temperature is
40~80 DEG C；
(4) crude product is configured to the solution that concentration is 1~3mg/mL, is added drop-wise to progress saturation absorption in macroporous resin column, absorption
After be eluted with water removing impurity, then recycling design and concentration are carried out to eluant, eluent as eluant, eluent with 60~80% ethanol,
Finally freezed, that is, obtain Flavonoid substances.
2. the method as described in claim 1, it is characterised in that water and the mass ratio of cacumen biotae are 5：1.
3. the method as described in claim 1, it is characterised in that the volume ratio 1 of ethanol and mixed liquor：1.
4. the method as described in claim 1, it is characterised in that described macroreticular resin is D-101, AB-8 or DM-130.
5. the method as described in claim 1, it is characterised in that the dripping quantity of the solution is 1.5 times of column volume；Water and second
The consumption of alcohol is 5 times of column volume.
6. a kind of method for extracting Flavonoid substances in cacumen biotae, it is characterised in that carry out according to the following steps：
(1) by cacumen biotae clean, drying after crush, obtain cacumen biotae powder, then add water, be uniformly mixed to get mixed liquor；
(2) mixed liquor is freezed 10~24 hours at a temperature of -40~-20 DEG C, placed at room temperature until its thawing；Repeat ice
Jelly-room temperature thawing step 2~3 times；The mixed liquor of gained after frost 10~24 hours, is placed at a temperature of -40~-20 DEG C
Melt in ultrasonic wave；
(3) ethanol is added into mixed liquor obtained by step (2) fully to mix, after 1~3h of immersion, carry out ultrasonic wave extraction, centrifugation
Separation, takes supernatant, freezes, obtains crude product；Ultrasonic power is 60~100W；Ultrasonic time is 20~60min；Ultrasonic temperature is
40~80 DEG C；
(4) crude product is configured to the solution that concentration is 1~3mg/mL, is added drop-wise to progress saturation absorption in macroporous resin column, absorption
After be eluted with water removing impurity, then recycling design and concentration are carried out to eluant, eluent as eluant, eluent with 60~80% ethanol,
Finally freezed, that is, obtain Flavonoid substances.
7. method as claimed in claim 6, it is characterised in that in ultrasonic melting process, ultrasonic power is 60~100W；Ultrasound
Time is 69~90min.
8. a kind of method for extracting Flavonoid substances in cacumen biotae, it is characterised in that carry out according to the following steps：
By cacumen biotae clean, drying after crush, obtain cacumen biotae powder, then add water, be uniformly mixed to get mixed liquor；Will mixing
Liquid is freezed 10~24 hours at a temperature of -40~-20 DEG C, is placed at room temperature until its thawing；Repeat frost-room temperature and melt step
It is rapid secondary；Freeze again, be placed in ultrasonic wave and melt, after thawing, freeze, obtain crude product；By crude product be configured to concentration for 1~
3mg/mL solution, is added drop-wise in macroporous resin column progress saturation absorption, is eluted with water removing impurity after absorption, then with 60~
80% ethanol carries out recycling design and concentration to eluant, eluent, is finally freezed, that is, obtain flavonoids thing as eluant, eluent
Matter.
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| CN105581943A (en) * | 2016-01-05 | 2016-05-18 | 南京科技职业学院 | Application of Chinese Arborvitae twig extract in shampoo |
| CN105640827A (en) * | 2016-01-05 | 2016-06-08 | 南京科技职业学院 | Method for preparing shampoo by adopting simple physical means |
| CN107595900A (en) * | 2017-08-18 | 2018-01-19 | 合肥丰洁生物科技有限公司 | A kind of extracting method of Thuja extract |
| CN110680776A (en) * | 2018-07-05 | 2020-01-14 | 伽蓝（集团）股份有限公司 | Application of arborvitae |
| CN114470012A (en) * | 2022-02-08 | 2022-05-13 | 上海章华保健化妆品有限公司 | Extraction method and application of cacumen biotae extract |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942991A (en) * | 2012-12-04 | 2013-02-27 | 深圳国能环保节能科技有限公司 | Microalgae oil extraction method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3224719B2 (en) * | 1994-08-20 | 2001-11-05 | 省三 小山 | Non-irritating, non-corrosive, aromatic neutral resin oil-based wound healing agent and epithelial formation promoting agent extracted from evergreen shrubs of the genus Hinoki or Asunaro |
-
2014
- 2014-12-16 CN CN201410785394.6A patent/CN104523767B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942991A (en) * | 2012-12-04 | 2013-02-27 | 深圳国能环保节能科技有限公司 | Microalgae oil extraction method |
Non-Patent Citations (3)
| Title |
|---|
| 大孔吸附树脂纯化侧柏叶总黄酮的工艺研究;黄月纯等;《中药新药与临床药理》;20100131;第21卷(第1期);第75-80页 * |
| 超声波法和冻结-融解法相结合提取紫薯中花色甙;顾红梅等;《食品科学》;20041231;第25卷(第7期);第104-108页 * |
| 超声波法提取侧柏叶片中黄酮类化合物的研究;赵永光等;《河北农业大学学报》;20050331;第28卷(第2期);第54-56页 * |
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