CN109248184A - The extracting method of total flavonoids substance in a kind of novel climbing groundsel - Google Patents
The extracting method of total flavonoids substance in a kind of novel climbing groundsel Download PDFInfo
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- CN109248184A CN109248184A CN201811314953.XA CN201811314953A CN109248184A CN 109248184 A CN109248184 A CN 109248184A CN 201811314953 A CN201811314953 A CN 201811314953A CN 109248184 A CN109248184 A CN 109248184A
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Abstract
The invention belongs to organic substance extractive technique field, a kind of extracting method of total flavonoids substance in novel climbing groundsel is disclosed；By fresh climbing groundsel root above section, cleaning, disinfection, drying smash it through 20 meshes and obtain climbing groundsel powder；Climbing groundsel powder is put into immersion 1h ultrasonic extraction 40min under the conditions of 350W80 DEG C in 60% ethanol solution；Solution is taken out after ultrasound, carries out filtering reservation filtrate, is filtered by vacuum after filter residue is impregnated 1h with 70% ethyl alcohol again；After inciting somebody to action filtrate merging twice, centrifuging and taking supernatant carries out concentration, vapors away remaining ethyl alcohol, obtains extracting flavonoids concentrate；Frozen dried is carried out, freeze-dried powder is obtained, total flavonoids substance in climbing groundsel is made.The present invention extracts the total flavonoids substance in climbing groundsel using ultrasonic extraction method, and characterization processes are simple, and recovery rate is higher, and extraction rate is very fast, avoid the problem of long-time refluxing extraction is needed in traditional extraction technique.
Description
Technical field
The invention belongs to total flavonoids substances in organic substance extractive technique field more particularly to a kind of novel climbing groundsel
Extracting method.
Background technique
Currently, the prior art commonly used in the trade is such that
Climbing groundsel is a kind of catananche, be born under hillside, sparse woods, Lin Bian, roadside, in limes marginis thick grass, it is cold in nature,
Bitter has clearing heat and detoxicating, improving eyesight, antipruritic and other effects.It is chiefly used in anemopyretic cold, red eye, swell pain, dysentery, skin eczema sore
Furuncle.Climbing groundsel contains liver poison Pyrrolizidine alkaloid more, and it is huge that acute and chronic poisoning can cause the sinus hepaticus of liver to block syndrome, liver
Microcytosis or liver fibrosis.Contain a large amount of total flavonoids substance in climbing groundsel, flavone compound has free radical resisting, resists
A variety of physiological activity and the pharmacological actions such as oxidation, anticancer, antibacterial, antiviral, anti-inflammatory, antiallergy, anti-diabetic complication, and
With vascular permeability and brittle effect is reduced, have to the treatment and prevention of the diseases such as the tumour of the mankind, aging, angiosis important
Meaning, but comparatively laborious to the extraction process of total flavonoids substance at present, recovery rate is lower.
In conclusion problem of the existing technology is:
(1) comparatively laborious to the extraction process of total flavonoids substance at present, recovery rate is lower.
(2) traditional pulverizer motor easily causes that temperature is excessively high when carrying out the crushing of extreme, and that destroys climbing groundsel has
Imitate ingredient；Furthermore easily cause because temperature is excessively high burn out pulverizer the case where, reduce working efficiency.
Summary of the invention
In view of the problems of the existing technology, the present invention provides total flavonoids substances in a kind of novel climbing groundsel to mention
Take method.
The invention is realized in this way in a kind of novel climbing groundsel total flavonoids substance extracting method are as follows:
Step 1: by fresh climbing groundsel root above section, cleaning, drying, disinfection, with 20 mesh after being crushed using pulverizer
Sieve obtains climbing groundsel powder；
Step 2: climbing groundsel powder being put into 60% ethanol solution and impregnates 1h, and during which each 20min stirring is primary, then
Ultrasonic extraction 40min under the conditions of 350W80 DEG C；
Step 3: taking out solution after ultrasound, be filtered by vacuum, and retains filtrate, filter residue is used to 70% second again
Alcohol is filtered by vacuum after impregnating 1h, obtains filtrate；
Step 4: will twice filtrate merge after, centrifuging and taking supernatant carries out at concentration filtrate using Rotary Evaporators
It manages, remaining ethyl alcohol is vapored away in draught cupboard, obtain extracting flavonoids concentrate；
Step 5: frozen dried is carried out to extracting flavonoids concentrate using freeze dryer, -80 DEG C, 12~16h is lyophilized
Total flavonoids substance in climbing groundsel is made in powder.
Further, it in step 1, cleans and cleans 1~2min for distilled water, effective component is avoided to be lost.
Further, it in step 1, dries in 68~75 DEG C of baking ovens, to be dried to moisture content lower than 8%.
Further, in step 2,1h is impregnated in 60% ethanol solution, during which each 20min stirring is primary, is conducive to effectively
The dissolution of ingredient.
Further, in step 4, centrifuging and taking supernatant, selection supercentrifuge rotating speed is 10000r/min.
Further, in step 5,12~18h of pre-freeze is carried out before freeze-drying in -20 DEG C of refrigerator.
Another object of the present invention is to provide the measuring method of Flavonoid substances, this method are as follows:
Step 1: it is accurate to draw the above Flavonoid substances extracting solution 3mL extracted, the ethyl alcohol that volume fraction is 50% is added
100mL, the sodium nitrite 1mL that mass fraction is 5%, is put into 25mL volumetric flask, shakes up；
Step 2: the aluminum nitrate solution 1mL, concentration 1mol/L that mass fraction is 10% is added into the above volumetric flask again
Sodium hydroxide solution 5mL, shake up；
Step 3: being diluted to groove with 30% ethyl alcohol, absorbance is measured using ultraviolet-uisible spectrophotometer, with same volume
Long-pending pure water replaces extracting solution as blank, obtains the content of Flavonoid substances.
Further, the Detection wavelength for using ultraviolet-uisible spectrophotometer is 510nm.
In conclusion advantages of the present invention and good effect are as follows:
The present invention using ultrasonic extraction method extract climbing groundsel in total flavonoids substance, characterization processes are simple, recovery rate compared with
Height, extraction rate is very fast, avoids the problem of long-time refluxing extraction is needed in traditional extraction technique.
The present invention uses improved thermal model algorithm, and the motivation of the pulverizer uses improved thermal model algorithm, has
Effect protects the effective component of climbing groundsel not destroy because of high temperature, avoids the overload situations of pulverizer, has carried out more to motor
Good protection, improves work efficiency.
Detailed description of the invention
Fig. 1 is the extracting method flow chart of total flavonoids substance in climbing groundsel provided in an embodiment of the present invention.
Fig. 2 is the measuring method flow chart of Flavonoid substances provided in an embodiment of the present invention.
Fig. 3 is that use ultraviolet specrophotometer provided in an embodiment of the present invention measures content detection result schematic diagram.
Fig. 4 is that ultraviolet specrophotometer is respectively adopted after suction filtration provided in an embodiment of the present invention is concentrated to measure content inspection
Survey result schematic diagram.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Application principle of the invention is described in detail with reference to the accompanying drawing.
As shown in Figure 1, in novel climbing groundsel provided in an embodiment of the present invention total flavonoids substance extracting method are as follows:
S101: by fresh climbing groundsel root above section, cleaning, drying, disinfection, with 20 meshes after being crushed using pulverizer
Son sieving, obtains climbing groundsel powder；
S102: climbing groundsel powder being put into 60% ethanol solution and impregnates 1h, and during which each 20min stirring is primary, is then existed
Ultrasonic extraction 40min under the conditions of 350W80 DEG C；
S103: taking out solution after ultrasound, be filtered by vacuum, and retains filtrate, filter residue is used to 70% ethyl alcohol again
It is filtered by vacuum after impregnating 1h, obtains filtrate；
S104: will twice filtrate merge after, centrifuging and taking supernatant, using Rotary Evaporators to filtrate carry out concentration,
Remaining ethyl alcohol is vapored away in draught cupboard, obtains extracting flavonoids concentrate；
S105: carrying out frozen dried to extracting flavonoids concentrate using freeze dryer, -80 DEG C, 12~16h, obtain freeze-dried powder,
Total flavonoids substance in climbing groundsel is made.
In step S101, cleans and clean 1~2min for distilled water, effective component is avoided to be lost.
In step S101, dry in 68~75 DEG C of baking ovens, to be dried to moisture content lower than 8%.
In step S102,1h is impregnated in 60% ethanol solution, during which each 20min stirring is primary, is conducive to effective component
Dissolution.
In step S104, centrifuging and taking supernatant, selection supercentrifuge rotating speed is 10000r/min.
In step S105,12~18h of pre-freeze is carried out before freeze-drying in -20 DEG C of refrigerator.
As shown in Fig. 2, the measuring method of Flavonoid substances provided in an embodiment of the present invention are as follows:
S201: it is accurate to draw the above Flavonoid substances extracting solution 3mL extracted, the ethyl alcohol that volume fraction is 50% is added
100mL, the sodium nitrite 1mL that mass fraction is 5%, is put into 25mL volumetric flask, shakes up；
S202: being added the aluminum nitrate solution 1mL that mass fraction is 10% into the above volumetric flask again, and concentration is 1mol/L's
Sodium hydroxide solution 5mL, shakes up；
S203: being diluted to groove with 30% ethyl alcohol, absorbance is measured using ultraviolet-uisible spectrophotometer, with same volume
Pure water replace extracting solution as blank, obtain the content of Flavonoid substances.
The Detection wavelength provided in an embodiment of the present invention for using ultraviolet-uisible spectrophotometer is 510nm.
The motivation of pulverizer provided in an embodiment of the present invention uses improved thermal model algorithm, specifically:
Single order motor thermal models equation are as follows:
In formula: T ' (t) is the temperature rise of motor；I ' (t) is the electric current of motor；C is the heat capacity coefficient of motor；H
For the coefficient of heat transfer of motor；R is the stator resistance of motor；
By its discretization, and set Tiny increment dt Δ T, Δ t, be meant that within the extremely short Δ t time, the temperature of motor by
T rises to T+ Δ T:
When electromotor overload,Then temperature T slowly increases；When motor no longer overloads,T value slowly reduces, to the heat dissipation of motor and its similar.
The invention will be further described combined with specific embodiments below.
Embodiment 1
Influence of the concentration of alcohol to recovery rate
Climbing groundsel powder is equally divided into 5 parts, it is molten to be respectively put into the ethyl alcohol that concentration is 50%, 60%, 70%, 80%, 90%
It is impregnated in liquid, later ultrasonic extraction 40min under the conditions of 350W90 DEG C, uv-spectrophotometric is respectively adopted after filtering concentration
Meter measures content, testing result as shown in figure 3, the concentration of alcohol that uses of the present invention for optimum extraction concentration.
Embodiment 2
Influence of the temperature to recovery rate
Climbing groundsel powder is equally divided into 5 parts, be put into 60% ethanol solution impregnate 1h after, respectively 350W40 DEG C, 50 DEG C,
Ultrasonic extraction 40min under the conditions of 60 DEG C, 70 DEG C, 80 DEG C, suction filtration is respectively adopted ultraviolet specrophotometer and measures after being concentrated to be contained
Amount, as shown in figure 4, as the temperature rises, the recovery rate of flavone compound gradually rises, 80 DEG C of whens, reach most testing result
High level, therefore, the Extracting temperature that the present invention selects are optimum extraction temperature, when the temperature is excessively high, a large amount of alcohol dissolubility impurity dissolutions
Speed is dramatically speeded up, and interferes the extraction of Flavonoid substances, leads to the decline for changing similar recovery rate.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (8)
1. the extracting method of total flavonoids substance in a kind of novel climbing groundsel, which is characterized in that in the novel climbing groundsel
The extracting method of total flavonoids substance are as follows:
Step 1: by fresh climbing groundsel root above section, cleaning, disinfection, drying, with 20 mesh sieve after being crushed using pulverizer
Sieving, obtains climbing groundsel powder；
Step 2: climbing groundsel powder being put into 60% ethanol solution and impregnates 1h, and during which each 20min stirring is primary, is then existed
Ultrasonic extraction 40min under the conditions of 350W80 DEG C；
Step 3: taking out solution after ultrasound, be filtered by vacuum, and retains filtrate, filter residue is used again 70% ethyl alcohol soak
It is filtered by vacuum after bubble 1h, obtains filtrate；
Step 4: will twice filtrate merge after, centrifuging and taking supernatant, using Rotary Evaporators to filtrate carry out concentration, lead to
Remaining ethyl alcohol is vapored away in wind cupboard, obtains extracting flavonoids concentrate；
Step 5: frozen dried is carried out to extracting flavonoids concentrate using freeze dryer, -80 DEG C, 12~16h, obtains freeze-dried powder, system
Obtain total flavonoids substance in climbing groundsel.
2. the extracting method of total flavonoids substance in novel climbing groundsel as described in claim 1, which is characterized in that the step
In rapid one, cleans and clean 1~2min for distilled water.
3. the extracting method of total flavonoids substance in novel climbing groundsel as described in claim 1, which is characterized in that the step
In rapid one, dry in 68~75 DEG C of baking ovens, to be dried to moisture content lower than 8%.
4. the extracting method of total flavonoids substance in novel climbing groundsel as described in claim 1, which is characterized in that the step
In rapid two, 1h is impregnated in 60% ethanol solution, during which each 20min stirring is primary, is conducive to the dissolution of effective component.
5. the extracting method of total flavonoids substance in novel climbing groundsel as described in claim 1, which is characterized in that the step
In rapid four, centrifuging and taking supernatant, selection supercentrifuge rotating speed is 10000r/min.
6. the extracting method of total flavonoids substance in novel climbing groundsel as described in claim 1, which is characterized in that the step
In rapid five, 12~18h of pre-freeze is carried out before freeze-drying in -20 DEG C of refrigerator.
7. the extracting method of total flavonoids substance in novel climbing groundsel as described in claim 1, which is characterized in that the flavones
The measuring method of substance are as follows:
Step 1: drawing the above Flavonoid substances extracting solution 3mL extracted, and the ethyl alcohol 100mL that volume fraction is 50%, matter is added
The sodium nitrite 1mL that score is 5% is measured, is put into 25mL volumetric flask, shakes up；
Step 2: being added the aluminum nitrate solution 1mL that mass fraction is 10% into the above volumetric flask again, and concentration is the hydrogen of 1mol/L
Sodium hydroxide solution 5mL, shakes up；
Step 3: being diluted to groove with 30% ethyl alcohol, absorbance is measured using ultraviolet-uisible spectrophotometer, with same volume
Pure water replaces extracting solution as blank, obtains the content of Flavonoid substances.
8. the extracting method of total flavonoids substance in novel climbing groundsel as described in claim 1, which is characterized in that the use
The Detection wavelength of ultraviolet-uisible spectrophotometer is 510nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112716991A (en) * | 2021-01-29 | 2021-04-30 | 西藏天虹科技股份有限责任公司 | Method for extracting and purifying total flavonoids of senecio dianthus |
| CN113512017A (en) * | 2021-09-13 | 2021-10-19 | 江西中医药大学 | Compound in radish leaf groundsel and preparation method and application thereof |
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| CN106038644A (en) * | 2016-05-11 | 2016-10-26 | 南京泽朗医药科技有限公司 | A method of preparing senecio dianthus franch total flavonoids and applications of the total flavonoids |
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- 2018-11-06 CN CN201811314953.XA patent/CN109248184A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106038644A (en) * | 2016-05-11 | 2016-10-26 | 南京泽朗医药科技有限公司 | A method of preparing senecio dianthus franch total flavonoids and applications of the total flavonoids |
Non-Patent Citations (2)
| Title |
|---|
| 李筱玲等: "千里光总黄酮提取方法研究", 《陕西农业科学》 * |
| 李筱玲等: "响应面法优化千里光总黄酮提取工艺研究", 《陕西农业科学》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112716991A (en) * | 2021-01-29 | 2021-04-30 | 西藏天虹科技股份有限责任公司 | Method for extracting and purifying total flavonoids of senecio dianthus |
| CN113512017A (en) * | 2021-09-13 | 2021-10-19 | 江西中医药大学 | Compound in radish leaf groundsel and preparation method and application thereof |
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Application publication date: 20190122 |