CN110151810A - A method of safflower extract is prepared using eutectic solvent - Google Patents
A method of safflower extract is prepared using eutectic solvent Download PDFInfo
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- CN110151810A CN110151810A CN201910408398.5A CN201910408398A CN110151810A CN 110151810 A CN110151810 A CN 110151810A CN 201910408398 A CN201910408398 A CN 201910408398A CN 110151810 A CN110151810 A CN 110151810A
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- eutectic solvent
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
- A61K36/286—Carthamus (distaff thistle)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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Abstract
The invention discloses a kind of methods for preparing safflower extract using eutectic solvent, the method are as follows: saffron powder is added in eutectic solvent aqueous solution, the ultrasonic extraction 15-60min under 25-75 DEG C, 50-200W, centrifugation, take supernatant, as safflower extract;The present invention provides a kind of method for preparing safflower extract using eutectic solvent efficiently, green, this method can main component in high efficiency extraction safflower simultaneously, the content for being wherein dehydrated carthamin yellow carthamus B is high compared with water extract by 45.9%, this method solvent usage is low (200mg flos carthami/1mL Extraction solvent), the disadvantages of extraction time needed for effectively preventing other solvents is long, extract is perishable is a kind of Novel extraction method suitable for Chinese medicine and other natural drugs.
Description
(1) technical field
The present invention relates to a kind of methods for preparing safflower extract using eutectic solvent.
(2) background technique
Safflower is the dry flower of composite family safflower plant safflower (Carthamus tinctorius L), is that China is answered extensively
Traditional Chinese medicine.One is all had to cardiovascular and cerebrovascular, nervous system, immune system through the safflower of clinical and pharmacological research discovery for many years
Fixed effect, there is the effect of blood circulation, removing blood stasis and acesodyne, is commonly used to treatment dysmenorrhea, amenorrhea due to stagnation of blood, postpartum stasis abdominal pain, bruise
Damage and arthralgia, the diseases such as coronary heart diseases and angina pectoris, common Chinese patent drug such as DANHONG ZHUSHEYE, guhong injection etc. with
Flavour of a drug are wanted based on safflower.
The main active of safflower is general flavone and carthamin yellow class compound.The chemical component structure of safflower includes
Flavones, alkaloid, sequiterpene, organic acid, carbene etc..Wherein hydroxyl radical carthamin yellow carthamus A and kaempferia galanga cellulose content are higher, in " China
Pharmacopeia " (2015 editions) be quality mark object.Wherein " Chinese Pharmacopoeia " (2015 editions) regulation hydroxyl safflower red pigment A (C27H32O16)
It must not be less than 1.0% (dry product), Kaempferide must not be less than 0.050% (dry product).
Chinese drugs have many characteristics, such as composition diversity, complexity.Wherein extracting separation is Chinese Traditional Medicine
Key link, is directly related to the quality and quantity of extract component, to influence stability and validity of product etc..With
The continuous propulsion of China's modernization of Chinese medicine process, traditional extraction process efficiency is lower, repeatability is poor, and polarity section is relatively narrow etc.
Problem increasingly draws attention.Specifically for safflower extracts preparation, then show as that water extract extraction efficiency is low, quality is difficult
Control, perishable etc..
(3) summary of the invention
It is an object of the present invention to provide a kind of green, the side of safflower extract is efficiently prepared using natural eutectic solvent
Method, this method can efficiently prepare safflower extract, wherein the content of dehydration safflower yellow B is high compared with water extract by 45.9%.This method
Chinese medicine is extracted by introducing natural eutectic solvent (Natural Deep Eutectic Solvent, NADES),
Short the time required to method, low energy consumption, and NADES itself is environmentally protective, is a kind of new medicine and other natural drug extracting methods.
The technical solution adopted by the present invention is that:
The present invention provides a kind of method for preparing safflower extract using eutectic solvent, the method are as follows: by safflower powder
End is added in eutectic solvent aqueous solution, the ultrasonic extraction 15-60min under 25-75 DEG C, 50-200W, centrifugation (preferably 16200 ×
10min under g), take supernatant, as safflower extract;Eutectic solvent is by hydrogen bond donor in the eutectic solvent aqueous solution
(Hydrogen Bond Donor, HBD) and hydrogen bond receptor (Hydrogen Bond Acceptor, HBA) and/or deionized water
Mix (i.e. eutectic solvent is prepared by hydrogen bond donor and hydrogen bond receptor Hybrid Heating, or by hydrogen bond donor, hydrogen bond by
Body and deionized water Hybrid Heating are prepared), the hydrogen bond donor include: sucrose (Suc), glycerol (Gly), lactic acid (Lac),
Urea (Ur), methylurea (Mu), dimethyl urea (Du), acetamide (Am), the hydrogen bond receptor include: choline chloride (ChCl),
Glycine betaine (Bet), L-PROLINE (L-Pro), D-PROLINE (D-Pro).
Further, the eutectic solvent is to be mixed by hydrogen bond donor with hydrogen bond receptor with the ratio between the amount of substance 1:1-2.5
Heating is prepared.
Further, the eutectic solvent is by hydrogen bond donor, hydrogen bond receptor and deionized water with the ratio between amount of substance 1:
0.25-1:1-5 Hybrid Heating is prepared.
Further, preferably eutectic solvent is prepared as follows: by hydrogen bond donor and hydrogen bond receptor and/or deionized water
After mixing, at 80-100 DEG C heating stirring 0.5-2 hours (preferably 80 DEG C, 1h), is formed and clarify uniform eutectic solvent.
Further, eutectic solvent volumetric concentration is 25-100% (preferably 75%) in the eutectic solvent aqueous solution,
The saffron powder weight is calculated as 25-200mg/mL (preferably 200mg/mL) with eutectic solvent aqueous solution volumetric usage.
Further, extraction conditions are preferred are as follows: ultrasonic extraction 30 minutes at 50 DEG C, 200W.
Further, the eutectic solvent is preferred are as follows: L-PROLINE (L-Pro) and acetamide (Am) and deionized water are with object
After the ratio between amount of matter 1:1:2 mixing, it is made in 80 DEG C of heating 1h, is denoted as DES-17 (L-Pro-Am).
Compared with prior art, beneficial effect of the present invention is mainly reflected in: the present invention provides a kind of utilization efficiently, green
The method that eutectic solvent prepares safflower extract, this method can main component in high efficiency extraction safflower simultaneously, wherein being dehydrated red
The content of anthoxanthin B is high compared with water extract by 45.9%, and this method solvent usage is low (200mg flos carthami/1mL Extraction solvent),
The disadvantages of extraction time needed for effectively preventing other solvents is long, extract is perishable is a kind of suitable for Chinese medicine and other days
The Novel extraction method of right drug.
(4) Detailed description of the invention
The high-efficient liquid phase chromatogram of Fig. 1 embodiment 1.
The high-efficient liquid phase chromatogram of Fig. 2 embodiment 2.
The high-efficient liquid phase chromatogram of Fig. 3 embodiment 3.
The high-efficient liquid phase chromatogram of Fig. 4 comparative example 1.
(5) specific embodiment
The present invention is described further combined with specific embodiments below, but protection scope of the present invention is not limited in
This:
With reference to embodiments to safflower effective ingredients hydroxyl radical carthamin yellow carthamus A of the present invention, dehydration safflower yellow
The extracting method of plain B is further illustrated, to help those skilled in the art to have inventive concept of the invention, technical solution
More complete, accurate and deep understanding.
Safflower used in the embodiment of the present invention is acquired according to " Chinese Pharmacopoeia " (2015) and is prepared.
Embodiment 1.DES-17 is solvent
L-PROLINE (1.15g), acetamide (0.59g), deionized water (36 μ L) is mixed with the ratio of molar ratio 1:1:2
Close, in 80 DEG C heating stirring 1 hour, formed and clarify uniform eutectic solvent, be denoted as DES-17.By the DES-17 of 750 μ L with
250 μ L water are uniformly mixed, and are added in 1.5mL centrifuge tube, then accurately weigh 200.0mg saffron powder and be added thereto, at 50 DEG C
Ultrasonic extraction 30min, ultrasonic power 200W.After ultrasonic extraction, it is centrifuged 10min under 13300r/min, takes supernatant, as
Safflower extract.Supernatant carries out high performance liquid chromatography detection (Fig. 1) after diluting 10 times with 50% methanol aqueous solution of volumetric concentration,
According to compound (hydroxyl radical carthamin yellow carthamus A and hydroxyl radical carthamin yellow carthamus A) standard curve, contained chemical combination in safflower extract is obtained
Species and content calculate recovery rate (mg/g) with compounds content in recovery rate=extract/safflower weight, measure extract
In contain: hydroxyl radical carthamin yellow carthamus A, 31.5mg/g;It is dehydrated carthamin yellow carthamus B, 14.5mg/g.
High performance liquid chromatography (HPLC), specific testing conditions: Agilent Extend C-18 (250mm*4.6mm, 6um);
Mobile phase is 0.1% formic acid water (A)-acetonitrile (B), elution program: 0-12min, 10-22%B, 12-20min, 26%B, 20-
30min, 26-90%B;Detection wavelength 0-7min, 270nm, 7-20min, 403nm, 20-80min, 270min;25 DEG C of column temperature;Stream
Fast 0.8mL/min, 20 microlitres of sample volume.
Embodiment 2DES-21 is solvent
Choline chloride (1.40g), acetamide (0.59g), deionized water (18 μ L) is mixed with the ratio of molar ratio 1:1:1
Close, in 80 DEG C heating stirring 1 hour, formed and clarify uniform eutectic solvent, be denoted as DES-21.By the DES-21 of 750 μ L with
250 μ L water are uniformly mixed, and are added in 1.5mL centrifuge tube, then accurately weigh 200.0mg saffron powder and be added thereto, at 50 DEG C
Ultrasonic extraction 30min, ultrasonic power 200W.After ultrasonic extraction, it is centrifuged 10min under 13300r/min, takes supernatant, as
Safflower extract.The high performance liquid chromatography described in embodiment 1 after supernatant dilutes 10 times with 50% methanol aqueous solution of volumetric concentration
It detects (Fig. 2), measures in extract and contain: hydroxyl radical carthamin yellow carthamus A, 29.6mg/g;It is dehydrated carthamin yellow carthamus B, 13.7mg/g.
Embodiment 3.DES-10 is solvent
L-PROLINE (1.15g) is mixed with lactic acid (1.80g) with the ratio of molar ratio 1:1, it is small in 80 DEG C of heating stirrings 1
When, it is formed and clarifies uniform eutectic solvent, be denoted as DES-10.The DES-10 of 750 μ L is uniformly mixed with 250 μ L water, is added
In 1.5mL centrifuge tube, then accurately weighs 200.0mg saffron powder and be added thereto, the ultrasonic extraction 30min at 50 DEG C, ultrasonic function
Rate is 200W.After ultrasonic extraction, it is centrifuged 10min under 13300r/min, takes supernatant, as safflower extract.Supernatant is used
The high performance liquid chromatography detection (Fig. 3) described in embodiment 1 after 50% methanol aqueous solution of volumetric concentration dilutes 10 times, measures extract
In contain: hydroxyl radical carthamin yellow carthamus A, 30.3mg/g;It is dehydrated carthamin yellow carthamus B, 13.5mg/g.
1 water of comparative example is solvent
It accurately weighs 200.0mg saffron powder to be added in 1.5mL centrifuge tube, 1mL deionized water is added, it is ultrasonic at 50 DEG C
Extract 30min, ultrasonic power 200W.After ultrasonic extraction, it is centrifuged 10min under 13300r/min, takes supernatant, as safflower
Water extract.The high performance liquid chromatography detection described in embodiment 1 after supernatant dilutes 10 times with 50% methanol aqueous solution of volumetric concentration
(Fig. 4), measures in extract and contains: hydroxyl radical carthamin yellow carthamus A, 28.9mg/g;It is dehydrated carthamin yellow carthamus B, 10.0mg/g.
Influence of the 4 eutectic solvent type of embodiment to extraction effect
DES-17 in embodiment 1 is replaced with into other eutectic solvents in table 1, molar ratio is as shown in table 1, other operations are same
Embodiment 1.Hydroxyl radical carthamin yellow carthamus A in obtained safflower extract, the content for being dehydrated carthamin yellow carthamus B are shown in Table 1.As a result it shows
Show, the comprehensive performance of extracting of DES-17 is best, followed by DES-10 and DES-21.
Influence of the 1. eutectic solvent type of table to recovery rate
Influence of the eutectic solvent volumetric concentration to recovery rate in 5 eutectic solvent aqueous solution of embodiment
DES-17 volumetric concentration in embodiment 1 is changed to shown in table 2, other operations are extracted with embodiment 1, obtained safflower
Hydroxyl radical carthamin yellow carthamus A in object, the content for being dehydrated carthamin yellow carthamus B are shown in Table 2.The results show that 75%DES extraction effect is best.
Influence of the 2. eutectic solvent concentration of table to extraction effect
Embodiment 6 extracts influence of the solid-to-liquid ratio to recovery rate
The quality (mg) of safflower in embodiment 1 and DES-17 aqueous solution total volume (ml) ratio are changed to shown in table 3, other behaviour
Make with embodiment 1, hydroxyl radical carthamin yellow carthamus A in obtained safflower extract, the content for being dehydrated carthamin yellow carthamus B are shown in Table 3.As a result
It has been shown that, 200mg/mL are optimum extraction solid-to-liquid ratio.
Table 3. extracts influence of the solid-to-liquid ratio to extraction effect
Influence of 7 Extracting temperature of embodiment to extraction effect
Temperature in embodiment 1 is changed to shown in table 4, other operations are with embodiment 1, and hydroxyl is red in obtained safflower extract
Anthoxanthin A, the content for being dehydrated carthamin yellow carthamus B are shown in Table 4.The results show that 50 DEG C are optimum extraction temperature.
Influence of 4. Extracting temperature of table to extraction effect
Embodiment 8 extracts influence of the power to extraction effect
Power in embodiment 1 is changed to shown in table 5, other operations are with embodiment 1, and hydroxyl is red in obtained safflower extract
Anthoxanthin A, the content for being dehydrated carthamin yellow carthamus B are shown in Table 5.The results show that 200W is optimum extraction power.
Influence of 5. power of table to extraction effect
Influence of 9 extraction time of embodiment to extraction effect
Extraction time in embodiment 1 is changed to shown in table 6, other operations are with embodiment 1, hydroxyl in obtained safflower extract
Base carthamus tinctorius yellow colour A, the content for being dehydrated carthamin yellow carthamus B are shown in Table 6.The result shows that 30min is the optimum extraction time.
Influence of 6. extraction time of table to extraction effect
Claims (7)
1. a kind of method for preparing safflower extract using eutectic solvent, it is characterised in that the method are as follows: by saffron powder
It is added in eutectic solvent aqueous solution, the ultrasonic extraction 15-60min under 25-75 DEG C, 50-200W, centrifugation takes supernatant, as
Safflower extract;Eutectic solvent is by hydrogen bond donor and hydrogen bond receptor and/or deionized water in the eutectic solvent aqueous solution
It mixes, the hydrogen bond donor includes: sucrose, glycerol, lactic acid, urea, methylurea, dimethyl urea, acetamide, the hydrogen bond
Receptor includes: choline chloride, glycine betaine, L-PROLINE, D-PROLINE.
2. the method as described in claim 1, it is characterised in that the eutectic solvent be by hydrogen bond donor and hydrogen bond receptor with
The ratio between amount of substance 1:1-2.5 Hybrid Heating is prepared.
3. the method as described in claim 1, it is characterised in that the eutectic solvent is by hydrogen bond donor, hydrogen bond receptor and to go
Ionized water is prepared with the ratio between amount of substance 1:0.25-1:1-5 Hybrid Heating.
4. the method as described in claim 1, it is characterised in that the eutectic solvent is prepared as follows: by hydrogen bond donor
After being mixed with hydrogen bond receptor and/or deionized water, 80-100 DEG C heating stirring 0.5-2 hours, formed clarify it is uniform low total
Molten solvent.
5. the method as described in claim 1, it is characterised in that eutectic solvent volume is dense in the eutectic solvent aqueous solution
Degree is 25-100%, and the saffron powder weight is calculated as 25-200mg/mL with eutectic solvent aqueous solution volumetric usage.
6. the method as described in claim 1, it is characterised in that extraction conditions are as follows: ultrasonic extraction 30 minutes at 50 DEG C, 200W.
7. the method as described in claim 1, it is characterised in that the eutectic solvent are as follows: L-PROLINE and acetamide and go from
After sub- water is mixed with the ratio between the amount of substance 1:1:2, it is made in 80 DEG C of heating 1h.
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Cited By (3)
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CN113768871A (en) * | 2021-09-23 | 2021-12-10 | 陕西中医药大学 | Traditional Chinese medicine preparation of hydroxyl carthamin yellow A |
CN115286680A (en) * | 2022-07-08 | 2022-11-04 | 南昌大学 | Method for extracting tea saponin from tea seed meal |
CN115844766A (en) * | 2022-11-30 | 2023-03-28 | 上海致臻志臣科技有限公司 | Oil and fat composition for cosmetics, plant extract, and preparation method and application thereof |
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CN108497497A (en) * | 2018-04-23 | 2018-09-07 | 广东省农业科学院蚕业与农产品加工研究所 | The extraction of mulberry leaf active material and store method |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113768871A (en) * | 2021-09-23 | 2021-12-10 | 陕西中医药大学 | Traditional Chinese medicine preparation of hydroxyl carthamin yellow A |
CN115286680A (en) * | 2022-07-08 | 2022-11-04 | 南昌大学 | Method for extracting tea saponin from tea seed meal |
CN115286680B (en) * | 2022-07-08 | 2024-03-29 | 南昌大学 | Method for extracting tea saponin from tea seed meal |
CN115844766A (en) * | 2022-11-30 | 2023-03-28 | 上海致臻志臣科技有限公司 | Oil and fat composition for cosmetics, plant extract, and preparation method and application thereof |
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