CN108392540A - A kind of extracting method of Flos Daturae total alkaloids - Google Patents
A kind of extracting method of Flos Daturae total alkaloids Download PDFInfo
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- CN108392540A CN108392540A CN201810336919.6A CN201810336919A CN108392540A CN 108392540 A CN108392540 A CN 108392540A CN 201810336919 A CN201810336919 A CN 201810336919A CN 108392540 A CN108392540 A CN 108392540A
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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)
- A61K36/81—Solanaceae (Potato family), e.g. tobacco, nightshade, tomato, belladonna, capsicum or jimsonweed
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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
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/19—Preparation or pretreatment of starting material involving fermentation using yeast, bacteria or both; enzymatic treatment
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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
- A61K2236/35—Extraction with lipophilic solvents, e.g. Hexane or petrol ether
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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
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
Abstract
The present invention relates to a kind of extracting methods of Flos Daturae total alkaloids comprising following steps：100g datura flowers are crushed, sieving for standby；3 ~ 8g1 butyl, 3 methylimidazole lactate, 2 ~ 6 PEG300 ~ 1000 and 200g deionized waters are mixed, with lactic acid tune pH to 3 ~ 5, obtain acid leaching liquor；Acid leaching liquor is added in datura flower, 0.8 ~ 1.5g acidic cellulases and 0.5 ~ 0.8g acid pectases is added, is uniformly mixed, 1 ~ 4h, filtering, with the aqueous hydrochloric acid solution filter wash slag of pH2 ~ 3, merging filtrate are stirred between maintaining the temperature at 35 ~ 55 DEG C；1% ammonium sulfate and 2%NaCl are added into filtrate, ethyl acetate is added to extract 3 times, remove ethyl acetate phase, alkaloid enrichment phase adjusts pH to 9 ~ 11 with ammonium hydroxide, then it is extracted 3 times with chloroform, chloroform is recovered under reduced pressure, obtains total alkaloid, using the principle that the molten alkali of acid is heavy, the recovery rate of total alkaloid in datura flower is improved.
Description
Technical field
The present invention relates to a kind of extracting methods of Flos Daturae total alkaloids.
Background technology
Datura flower is the dry flower of plant of Solanaceae datura metel, there is the effect of antiasthmatic-antitussive, analgesia, spasmolysis, mainly at
It is divided into tropane type alkaloid, there is very strong physiological activity, also contains liquor-saturated eggplant lactone steroidal and flavonoids master in addition to this
Ingredient is wanted, is detached in extraction difficult.How fully to extract alkaloid active ingredient, increase operation rate, is to improve it into quality
The key of amount.The extraction research of common datura flower alkaloid be concentrated mainly on Soakage extraction, refluxing extraction and Microwave Extraction (in
Patent medicine, the 5th phase of volume 34 in May, 2012), Soakage extraction system according to drifting alkaloids in addition to it can be dissolved in alcohol, also dissolve in chloroform,
The organic solvents such as ether, alkaloid salts especially inorganic acid salt is soluble easily in water, does not dissolve in or be insoluble in common organic solvent；Profit
With the above-mentioned property of alkaloid, alcohol extracting thing is dissolved with sour water, removes insoluble impurities, alkalized with lye, make alkaloid salt
It is transformed into free alkali, then is extracted with organic solvent, merge organic solvent extract liquor, concentrates up to total alkaloid.It sends out under study for action
Existing, recovery rate is unsatisfactory, is not also in recent years very for the research for how improving the recovery rate of alkaloid in datura flower
It is more.
CN201610422547.X discloses a kind of method for extraction and purification of hyoscine in datura flower, obtains foreign gold first
Colored leaching liquor；Leaching liquor recycles ethyl alcohol, obtains mixture by ceramic membrane filter, NF membrane concentration；Mixture dilute hydrochloric acid
Dissolving takes filtrate after filtering；Retain aqueous solution after filtrate extraction；After water phase adjusts pH, then extracts four times and take chloroformic solution；Chloroform
Chloroform is recycled after solution drying, obtains total alkaloid；After total alkaloid is detached with alkali alumina column chromatography, chlorine is recycled
It is imitative, obtain hyoscine.
CN201610756028.7 discloses a kind of method that the Microwave Extraction of datura flower active ingredient is best, using microwave
The parameters such as power, microwave irradiation time, solvent dosage, soaking time, extraction temperature, to datura flower dry cream, total alkaloid, east Liang
Henbane alkali carries take；Using the content of acid-dye colorimetry, high effective liquid chromatography for measuring Flos Daturae total alkaloids, hyoscine,
Dry extract yield is measured with mass method.The optimum process condition of datura flower Microwave Extraction is to be with the volume fraction of 10 times of amounts of medicinal material
75% ethyl alcohol impregnates 2.0h, is 730W in power, temperature is continuous radiation 25min under 65 DEG C of microwave condition.
In view of this, need to invent it is a kind of can from datura flower the method for high-purity extract total alkaloids it is necessary.
Invention content
The purpose of the present invention is to provide a kind of extracting methods easy to operate, the high Flos Daturae total alkaloids of extraction yield.
To achieve the above object, the technical solution used in the present invention is：
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, sieving for standby；
(2) 3 ~ 8g1- butyl -3- methylimidazoles lactate, 2 ~ 6 PEG300 ~ 1000 and 200g deionized waters are mixed, uses lactic acid
PH to 3 ~ 5 is adjusted, acid leaching liquor is obtained；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, 0.8 ~ 1.5g acid is added
Property cellulase and 0.5 ~ 0.8g acid pectases, be uniformly mixed, 1 ~ 4h stirred between maintaining the temperature at 35 ~ 55 DEG C, filter, use
The aqueous hydrochloric acid solution filter wash slag of pH2 ~ 3, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, ethyl acetate is added and extracts 3 times, removes ethyl acetate phase, alkaloid
Enrichment phase adjusts pH to 9 ~ 11 with ammonium hydroxide, is then extracted 3 times with chloroform, chloroform is recovered under reduced pressure, obtains total alkaloid.
As further improvement of the invention, the pH value of the step (2) is 3.5 ~ 4.5.
Improved as of the invention further, 1- butyl -3- methylimidazoles lactate described in the step (2), PEG and
The mass ratio of deionized water is 5.5:4:200.
As further improvement of the invention, the addition of acidic cellulase described in the step (3) is 1.2g, institute
The addition for stating acid pectase is 0.7g.
As further improvement of the invention, pH is 10 in the step (4).
It is improved as of the invention further, the dosage of 3 ethyl acetate and the volume ratio of filtrate are respectively：2~3:
2 ~2.5:1.5~2.5。
It is using advantageous effect caused by above-mentioned technical proposal：
Scheme provided by the present invention improves the recovery rate of total alkaloid in datura flower using the principle that the molten alkali of acid is heavy.Pass through
Broken wall is carried out to datura flower in acid condition, coordinates 1- butyl -3- methylimidazoles lactate and PEG, ensures the activity of enzyme, together
When being fully dissolved out with effective guarantee active constituent, so that broken wall and extraction is carried out at the same time, suitable acidic environment ensure that life
The dissolubility of alkaloids, more conducively extraction and separation.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, invention is carried out with reference to specific embodiment
Clear, complete description.
Embodiment 1
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 5.5g1- butyl -3- methylimidazoles lactate, 4g PEG400 and 200g deionized waters are mixed, extremely with lactic acid tune pH
3.5, obtain acid leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 1.2g is added
The plain enzyme of dimension and 0.7g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 50 DEG C, filter, with the hydrochloric acid of pH2.5
Aqueous solution filter wash slag, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes second
Acetoacetic ester phase, alkaloid enrichment phase adjust pH to 10 with ammonium hydroxide, are then extracted 3 times with 1.5 times of volume chloroforms, chlorine is recovered under reduced pressure
It is imitative, it is dried to obtain total alkaloid dry cream 16.2g, total alkaloid recovery rate is 0.447%.
Embodiment 2
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 3g1- butyl -3- methylimidazoles lactate, 2g PEG800 and 200g deionized waters are mixed, extremely with lactic acid tune pH
3.5, obtain acid leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 1.2g is added
The plain enzyme of dimension and 0.7g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 50 DEG C, filter, with the hydrochloric acid of pH2.5
Aqueous solution filter wash slag, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes second
Acetoacetic ester phase, alkaloid enrichment phase adjust pH to 10 with ammonium hydroxide, are then extracted 3 times with 1.5 times of volume chloroforms, chlorine is recovered under reduced pressure
It is imitative, it is dried to obtain total alkaloid dry cream 15.6g, total alkaloid recovery rate is 0.428%.
Embodiment 3
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 8g1- butyl -3- methylimidazoles lactate, 6g PEG1000 and 200g deionized waters are mixed, extremely with lactic acid tune pH
3.5, obtain acid leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 1.2g is added
The plain enzyme of dimension and 0.7g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 40 DEG C, filter, with the hydrochloric acid of pH2.5
Aqueous solution filter wash slag, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes second
Acetoacetic ester phase, alkaloid enrichment phase adjust pH to 10 with ammonium hydroxide, are then extracted 3 times with chloroform, chloroform is recovered under reduced pressure, is dried to obtain
Total alkaloid dry cream 16.4g, total alkaloid recovery rate are 0.449%.
Embodiment 4
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 5.5g1- butyl -3- methylimidazoles lactate, 4g PEG300 and 200g deionized waters are mixed, extremely with lactic acid tune pH
4.5, obtain acid leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 0.8g is added
The plain enzyme of dimension and 0.5g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 55 DEG C, filter, with the hydrochloric acid of pH2.5
Aqueous solution filter wash slag, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes second
Acetoacetic ester phase, alkaloid enrichment phase adjust pH to 11 with ammonium hydroxide, are then extracted 3 times with chloroform, chloroform is recovered under reduced pressure, is dried to obtain
Total alkaloid dry cream 16.0g, total alkaloid recovery rate are 0.439%.
Embodiment 5
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 5.5g1- butyl -3- methylimidazoles lactate, 4g PEG600 and 200g deionized waters are mixed, extremely with lactic acid tune pH
5, obtain acid leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 1.5g is added
The plain enzyme of dimension and 0.8g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 35 DEG C, filter, with the hydrochloric acid of pH2.5
Aqueous solution filter wash slag, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes second
Acetoacetic ester phase, alkaloid enrichment phase adjust pH to 9 with ammonium hydroxide, are then extracted 3 times with chloroform, chloroform is recovered under reduced pressure, is dried to obtain
Total alkaloid dry cream 15.4g, total alkaloid recovery rate are 0.421%.
Embodiment 6
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 8g1- butyl -3- methylimidazoles lactate, 2g PEG400 and 200g deionized waters are mixed, with lactic acid tune pH to 4,
Obtain acid leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 1.2g is added
The plain enzyme of dimension and 0.7g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 35 DEG C, filter, with the hydrochloric acid water of pH3
Solution filter wash slag, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes second
Acetoacetic ester phase, alkaloid enrichment phase adjust pH to 10 with ammonium hydroxide, are then extracted 3 times with 1.5 times of volume chloroforms, chlorine is recovered under reduced pressure
It is imitative, it is dried to obtain total alkaloid dry cream 15.7g, total alkaloid recovery rate is 0.433%.
Comparative example 1
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 200g deionized waters are taken, with lactic acid tune pH to 3.5, obtain acid leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 1.2g is added
The plain enzyme of dimension and 0.7g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 50 DEG C, filter, with the hydrochloric acid of pH2.5
Aqueous solution filter wash slag, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes second
Acetoacetic ester phase, alkaloid enrichment phase adjust pH to 10 with ammonium hydroxide, are then extracted 3 times with 1.5 times of volume chloroforms, chlorine is recovered under reduced pressure
It is imitative, obtain total alkaloid.
Comparative example 2
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 5.5g1- butyl -3- methylimidazoles lactate and 200g deionized waters are mixed, with lactic acid tune pH to 3.5, obtains acid
Property leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 1.2g is added
The plain enzyme of dimension and 0.7g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 50 DEG C, filter, with the hydrochloric acid of pH2.5
Aqueous solution filter wash slag, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes second
Acetoacetic ester phase, alkaloid enrichment phase adjust pH to 10 with ammonium hydroxide, are then extracted 3 times with 1.5 times of volume chloroforms, chlorine is recovered under reduced pressure
It is imitative, obtain total alkaloid.
Comparative example 3
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 4g PEG400 and 200g deionized waters are mixed, with lactic acid tune pH to 3.5, obtains acid leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 1.2g is added
The plain enzyme of dimension and 0.7g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 50 DEG C, filter, with the hydrochloric acid of pH2.5
Aqueous solution filter wash slag, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes second
Acetoacetic ester phase, alkaloid enrichment phase adjust pH to 10 with ammonium hydroxide, are then extracted 3 times with 1.5 times of volume chloroforms, chlorine is recovered under reduced pressure
It is imitative, obtain total alkaloid.
Comparative example 4
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 5.5g1- butyl -3- methylimidazoles lactate, 4g PEG400 and 200g deionized waters are mixed, extremely with hydrochloric acid tune pH
3.5, obtain acid leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 1.2g is added
The plain enzyme of dimension and 0.7g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 50 DEG C, filter, with the hydrochloric acid of pH2.5
Aqueous solution filter wash slag, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes second
Acetoacetic ester phase, alkaloid enrichment phase adjust pH to 10 with ammonium hydroxide, are then extracted 3 times with 1.5 times of volume chloroforms, chlorine is recovered under reduced pressure
It is imitative, obtain total alkaloid.
Comparative example 5
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 5.5g1- butyl -3- methylimidazoles lactate, 4g PEG1500 and 200g deionized waters are mixed, with lactic acid tune pH
To 3.5, acid leaching liquor is obtained；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 1.2g is added
The plain enzyme of dimension and 0.7g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 50 DEG C, filter, with the hydrochloric acid of pH2.5
Aqueous solution filter wash slag, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes second
Acetoacetic ester phase, alkaloid enrichment phase adjust pH to 10 with ammonium hydroxide, are then extracted 3 times with 1.5 times of volume chloroforms, chlorine is recovered under reduced pressure
It is imitative, obtain total alkaloid.
Comparative example 6
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 10g1- butyl -3- methylimidazoles lactate, 4g PEG300 and 200g deionized waters are mixed, extremely with lactic acid tune pH
3.5, obtain acid leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 1.2g is added
The plain enzyme of dimension and 0.7g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 50 DEG C, filter, with the hydrochloric acid of pH2.5
Aqueous solution filter wash slag, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes second
Acetoacetic ester phase, alkaloid enrichment phase adjust pH to 10 with ammonium hydroxide, are then extracted 3 times with 1.5 times of volume chloroforms, chlorine is recovered under reduced pressure
It is imitative, obtain total alkaloid.
Comparative example 7
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 5.5g1- butyl -3- methylimidazoles lactate, 8g PEG300 and 200g deionized waters are mixed, extremely with lactic acid tune pH
3.5, obtain acid leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 1.2g is added
The plain enzyme of dimension and 0.7g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 50 DEG C, filter, with the hydrochloric acid of pH2.5
Aqueous solution filter wash slag, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes second
Acetoacetic ester phase, alkaloid enrichment phase adjust pH to 10 with ammonium hydroxide, are then extracted 3 times with 1.5 times of volume chloroforms, chlorine is recovered under reduced pressure
It is imitative, obtain total alkaloid.
Comparative example 8
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 5.5g1- butyl -3- methylimidazoles lactate, 4g PEG400 and 200g deionized waters are mixed, extremely with lactic acid tune pH
3.5, obtain acid leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, be uniformly mixed, keep temperature
Degree stirs 2.5h between 50 DEG C, filters, with the aqueous hydrochloric acid solution filter wash slag of pH2.5, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes second
Acetoacetic ester phase, alkaloid enrichment phase adjust pH to 10 with ammonium hydroxide, are then extracted 3 times with 1.5 times of volume chloroforms, chlorine is recovered under reduced pressure
It is imitative, obtain total alkaloid.
Comparative example 9
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) datura flower is contributed in 200g deionized waters, 1.2g cellulases and 0.7g pectases is added, stirred 2.5 hours,
With hydrochloric acid tune pH to 3.5,5.5g1- butyl -3- methylimidazoles lactate is added and 4g PEG400, agitation and filtration use pH2.5
Aqueous hydrochloric acid solution filter wash slag, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes second
Acetoacetic ester phase, alkaloid enrichment phase adjust pH to 10 with ammonium hydroxide, are then extracted 3 times with 1.5 times of volume chloroforms, chlorine is recovered under reduced pressure
It is imitative, obtain total alkaloid.
Comparative example 10
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 5.5g1- butyl -3- methylimidazoles lactate, 4g PEG400 and 200g deionized waters are mixed, extremely with lactic acid tune pH
3.5, obtain acid leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 1.2g is added
The plain enzyme of dimension and 0.7g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 50 DEG C, filter, with aqueous solution filter wash
Slag, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes second
Acetoacetic ester phase, alkaloid enrichment phase adjust pH to 10 with ammonium hydroxide, are then extracted 3 times with 1.5 times of volume chloroforms, chlorine is recovered under reduced pressure
It is imitative, obtain total alkaloid.
Comparative example 11
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 5.5g1- butyl -3- methylimidazoles lactate, 4g PEG400 and 200g deionized waters are mixed, extremely with lactic acid tune pH
3.5, obtain acid leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 1.2g is added
The plain enzyme of dimension and 0.7g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 50 DEG C, filter, with the hydrochloric acid of pH2.5
Aqueous solution filter wash slag, merging filtrate；
(4) it uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes ethyl acetate phase, alkaloid enrichment phase ammonium hydroxide tune
PH to 10 is saved, is then extracted 3 times with 1.5 times of volume chloroforms, chloroform is recovered under reduced pressure, obtains total alkaloid.
Comparative example 12
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 5.5g1- butyl -3- methylimidazoles lactate, 4g PEG400 and 200g deionized waters are mixed, extremely with lactic acid tune pH
3.5, obtain acid leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 1.2g is added
The plain enzyme of dimension and 0.7g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 50 DEG C, filter, with the hydrochloric acid of pH2.5
Aqueous solution filter wash slag, merging filtrate；
(4) 3% ammonium sulfate is added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes ethyl acetate
Phase, alkaloid enrichment phase adjust pH to 10 with ammonium hydroxide, are then extracted 3 times with 1.5 times of volume chloroforms, chloroform is recovered under reduced pressure, obtains
To total alkaloid.
Comparative example 13
A kind of extracting method of Flos Daturae total alkaloids comprising following steps：
(1) 100g datura flowers are crushed, crosses 80 mesh sieve, it is spare；
(2) 5.5g1- butyl -3- methylimidazoles lactate, 4g PEG400 and 200g deionized waters are mixed, extremely with lactic acid tune pH
3.5, obtain acid leaching liquor；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, it is acid fine that 1.2g is added
The plain enzyme of dimension and 0.7g acid pectases, are uniformly mixed, 2.5h are stirred between maintaining the temperature at 50 DEG C, filter, with the hydrochloric acid of pH2.5
Aqueous solution filter wash slag, merging filtrate；
(4) 3%NaCl is added into filtrate, uses 2 times of volume ethyl acetate of filtrate to extract respectively 3 times, removes ethyl acetate phase,
Alkaloid enrichment phase adjusts pH to 10 with ammonium hydroxide, is then extracted 3 times with 1.5 times of volume chloroforms, chloroform is recovered under reduced pressure, and obtains total
Alkaloid.
The acid cellulose used in the embodiment of the present invention and comparative example is conventional commercial product, and in the application is stone
Family's village Mei Shida Products, acid pectase are purchased from 101 company of Jining of Shandong Province.
Effect example 1
The assay of total alkaloid, method are as follows：
1. the preparation of atropine sulfate reference substance solution：
Take 102 DEG C of dryings to atropine sulfate 10 mg of constant-quality, it is accurately weighed, it sets in 100 mL measuring bottles, it is fixed to be dissolved in water
Hold scale, shakes up the atropine sulfate reference substance solution to get 0. 1 g/L.
2. 0.5g·mL-1The preparation of acid dyes bromocresol green solution：
Precision weighs bromocresol green 50mg, and Potassium Hydrogen Phthalate 1.021g adds 0.2molL-1Sodium hydroxide solution 6.0m
L makes dissolving, adds water and is diluted to 100mL, shakes up, and is filtered when necessary to get 0.5gmL-1Bromocresol green solution.
3. the preparation of atropine sulfate acid dye spectrophotometer standard curve：
Precision draws 0. 2,0. 4,0. 6,0. 8,1. 0 mL of atropine sulfate reference substance solution, is respectively placed in separatory funnel
In, 0. 500 g/L acid dyes bromocresol greens solution, 3. 0 mL is respectively sequentially added, 10. 0 mL of chloroform is supplemented with water
Equal to volume, shaking extraction 2min stands 5 min, divides and take chloroform layer solution, add 0. 5 g anhydrous sodium sulfates,
Place 20 min.Take another accurate separatory funnel that 10. 0 mL of chloroform is added, precision that 1. 0 mL of water, same method is added
Placebo solution is made, at 420 nm of wavelength measure absorbance, using absorbance as ordinate, acquire regression equation Y=
0.0562X+0.0067, r=0. 999 9 show that atropine sulfate is in good linear relationship in 20 ~ 100 μ g ranges.
4. the assay method of total alkaloid content in extract
Total alkaloid dry cream 0. 2 g is taken, it is accurately weighed, add water 10mL to make dissolving, adjust pH to 2~3, filtration, filtrate is used
Ammonia solution tune pH is extracted 4 times to 9 ~ 10, then with chloroform, and 10 mL, divides and chloroform, merging is taken to be settled to every time
100mL shakes up to get test solution；It is accurate again to draw above-mentioned 1. 0 mL of test solution, by being operated under 3, measures and inhale
Receipts value calculates total alkaloid mass concentration and total alkaloid recovery rate.
Total alkaloid recovery rate (%)=［ (total alkaloid mass concentration × 100 × dry cream amount in test sample)/dry cream takes
Sample amount ］ × 100/medicinal material amount
Shown in upper table, it is added without 1- butyl -3- methylimidazoles lactate and PEG300 extraction effects is not considerable, be individually added into
1- butyl -3- methylimidazoles lactate or PEG300, total alkaloid recovery rate, which is relatively added without, to increase, but still pays no attention to
Think.1- butyl -3- methylimidazoles lactate and PEG300 are added before broken wall, can promote total biology during effectively in broken wall
The recovery rate of alkali.The addition of 1- butyl -3- methylimidazoles lactate and PEG300 are not The more the better, can be with from comparative example 6 and 7
Find out, recovery rate is substantially reduced.PEG molecular weight, on recovery rate, there is also influences, after PEG1500 is added, the result is that making us losing
It hopes.It is more preferable compared with hydrochloric acid effect with newborn acid for adjusting pH, thus it is speculated that probably due to hydrochloric acid can influence the activity of enzyme.Ammonium sulfate and NaCl mono-
With using, meeting recovery rate has facilitation.Method provided by the present invention so that the recovery rate of total alkaloid, which has, obviously to be carried
It is high.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, it will be understood by those of ordinary skill in the art that：It still may be used
To modify to the technical solution recorded in previous embodiment or equivalent replacement of some of the technical features；And
These modifications or replacements, the spirit and model of technical solution of the embodiment of the present invention that it does not separate the essence of the corresponding technical solution
It encloses.
Claims (6)
1. a kind of extracting method of Flos Daturae total alkaloids, which is characterized in that it includes the following steps：
(1) 100g datura flowers are crushed, sieving for standby；
(2) 3 ~ 8g1- butyl -3- methylimidazoles lactate, 2 ~ 6 PEG300 ~ 1000 and 200g deionized waters are mixed, uses lactic acid
PH to 3 ~ 5 is adjusted, acid leaching liquor is obtained；
(3) the acid leaching liquor that step (2) obtains is added to step (1) treated in datura flower, 0.8 ~ 1.5g acid is added
Property cellulase and 0.5 ~ 0.8g acid pectases, be uniformly mixed, 1 ~ 4h stirred between maintaining the temperature at 35 ~ 55 DEG C, filter, use
The aqueous hydrochloric acid solution filter wash slag of pH2 ~ 3, merging filtrate；
(4) 1% ammonium sulfate and 2%NaCl are added into filtrate, ethyl acetate is added and extracts 3 times, removes ethyl acetate phase, alkaloid
Enrichment phase adjusts pH to 9 ~ 11 with ammonium hydroxide, is then extracted 3 times with chloroform, chloroform is recovered under reduced pressure, obtains total alkaloid.
2. a kind of extracting method of Flos Daturae total alkaloids according to claim 1, which is characterized in that the step (2)
PH value be 3.5 ~ 4.5.
3. a kind of extracting method of Flos Daturae total alkaloids according to claim 3, which is characterized in that the step (2)
Described in 1- butyl -3- methylimidazoles lactate, PEG and deionized water mass ratio be 5.5:4:200.
4. a kind of extracting method of Flos Daturae total alkaloids according to claim 1, which is characterized in that the step (3)
Described in the addition of acidic cellulase be 1.2g, the addition of the acid pectase is 0.7g.
5. a kind of extracting method of Flos Daturae total alkaloids according to claim 1, which is characterized in that the step (4)
Middle pH is 10.
6. a kind of extracting method of Flos Daturae total alkaloids according to claim 1, which is characterized in that 3 acetic acid
The dosage of ethyl ester and the volume ratio of filtrate are respectively：2 ~3:2 ~2.5:1.5~2.5.
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Cited By (2)
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| CN114344221A (en) * | 2022-02-10 | 2022-04-15 | 河北医科大学 | Pure natural emulsion type lipstick or lip glaze and preparation method thereof |
| CN115317547A (en) * | 2022-10-13 | 2022-11-11 | 广东心宝药业科技有限公司 | Flos Daturae Metelis extract, and its preparation method and application in preparing medicine for treating heart failure |
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| CN115317547A (en) * | 2022-10-13 | 2022-11-11 | 广东心宝药业科技有限公司 | Flos Daturae Metelis extract, and its preparation method and application in preparing medicine for treating heart failure |
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