CN109806291A - The method for extraction and purification of effective component in a kind of Yi nationality's medicine tripterygium hypoglaucum hutcs - Google Patents
The method for extraction and purification of effective component in a kind of Yi nationality's medicine tripterygium hypoglaucum hutcs Download PDFInfo
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Abstract
The present invention provides a kind of method for extraction and purification of effective component in Yi nationality's medicine tripterygium hypoglaucum hutcs, the following steps are included: (1) pulverizes and sieves, the mixed enzyme that phosphoric acid-buffer solution of sodium phosphate is added, is made of cellulase and pectase, isothermal reaction at 50 ± 5 DEG C, acetic acid diluted is added, isothermal reaction at 40 ± 5 DEG C, inactivation；(2) ethyl alcohol is added and carries out ultrasonic extraction, be centrifuged, be concentrated under reduced pressure；(3) acetic acid solution dissolution is added in concentrate, and aqueous layer is stayed in organic solvent extraction；(4) lye adjusts aqueous layer pH value, and organic layer is stayed in organic solvent extraction；(5) it is concentrated under reduced pressure, obtains tripterygium hypoglaucum hutcs total alkaloid crude extract；(6) silicagel column is crossed, is eluted using ethyl acetate, eluent is collected after elution, is concentrated and dried.Operation of the present invention is simple, and total alkaloid yield is high in gained effective component tripterygium hypoglaucum hutcs, and impurity content is few, and medical value is high, is suitable for promoting and applying.
Description
Technical field
The present invention relates to technical field of extraction of Chinese traditional medicine, and in particular to the extraction of effective component in a kind of Yi nationality's medicine tripterygium hypoglaucum hutcs
Purification process.
Background technique
Tripterygium hypoglaucum hutcs are Yunnan Yi nationality doctor's common drugs, are Celastraceae tripterygium plant also known as colguhoumia root, six sides
Rattan, glaucousback threewingnut root-bark etc., modern pharmacological research find that it has significant pharmacological action, including dispelling wind and eliminating dampness, promoting blood circulation and hemostasis, and relaxing muscles and tendons connects
The effect of bone, removing toxic substances desinsection.It is usually used in rheumatic arthralgia, hemiplegia, hernia pain, dysmenorrhea, menorrhalgia, postpartum abdominal pain, bleeding
Incessantly, acute infectious hepatitis, chronic nephritis, lupus erythematosus, cancerous swelling, injury and bone fracture, osteomyelitis, bone tuberculosis, epididymis tuberculosis, sore
Poison, psoriasis, neurodermatitis.
The ingredients such as tripterygium hypoglaucum hutcs are containing alkaloids, diterpene, triterpene, sequiterpene, diterpene and alkaloid are tripterygium hypoglaucum hutcs
Main component, while be also main active constituent.Wherein the alkaloid obtained in the tripterygium hypoglaucum hutcs plant is dihydro
Agarofuran type sequiterpene is condensed the pyridine alkaloid structure to be formed from different pyridine acids.It is separated from tripterygium hypoglaucum hutcs at present
Sesquiterpene alkaloids constituents, macrolides and two kinds of non-macrolides can be simply divided into according to its structure.Greatly
Cyclic lactone type sesquiterpene alkaloid is mostly condensed in C-13 and C-13 and different pyridine acids, is also seen to have and is passed through at C-8 and C-15
Oxygen forms a macrocyclic structure.Non- macrolides sesquiterpene alkaloids then mostly connect cyclization by oxygen with C-7 by C-5, and
Ester is condensed at C-6 more than pyridine acid.
In tripterygium hypoglaucum hutcs, total alkaloid content is about 0.3-4%, to treatment of arthritis, tumour, clinical organ transplant
It is significant in efficacy in terms of immunological rejection afterwards, and toxicity is low.Therefore, from tripterygium hypoglaucum hutcs Hydrolysis kinetics high-efficiency low-toxicity alkaloid at
Point, for developing tripterygium hypoglaucum hutcs correlation new drug, there is great research significance.
Summary of the invention
The purpose of the present invention is to provide a kind of method for extraction and purification of effective component in Yi nationality's medicine tripterygium hypoglaucum hutcs, operation letters
Single, total alkaloid yield is high in gained tripterygium hypoglaucum hutcs, and impurity content is few, and medical value is high, is suitable for promoting and applying.
In order to achieve the above object, the present invention is achieved by the following technical programs:
The method for extraction and purification of effective component in a kind of Yi nationality's medicine tripterygium hypoglaucum hutcs, comprising the following steps:
(1) root skin of tripterygium hypoglaucum hutcs is smashed it through into 100-150 mesh, being added 3-4 times and measuring pH value is 5.5 ± 0.5
The mixed enzyme of 0.4-0.7% being made of cellulase and pectase, perseverance at 50 ± 5 DEG C is added in phosphoric acid-buffer solution of sodium phosphate
Acetic acid diluted is added in temperature reaction 2-3h, and adjusting pH value is 4-4.5, at 40 ± 5 DEG C after isothermal reaction 1-1.5h, 90-95 DEG C of inactivation 5-
8min；
(2) it is then added 8-11 times and measures the ethyl alcohol progress ultrasonic extraction that mass fraction is 60-80%, carried out after the completion of extracting
Centrifugation, gained filter residue carries out second extraction, merging filtrate, and passes through and concentrate is concentrated under reduced pressure to obtain；
(3) after being dissolved the acetic acid solution that concentrate addition mass fraction is 5-8%, organic solvent extraction is added,
Organic layer is abandoned, aqueous layer is stayed；
(4) pH value of aqueous layer is adjusted to 9.5 ± 0.5 using lye, adds organic solvent and is extracted, abandon water phase
Layer, stays organic layer；
(5) organic layer is carried out being concentrated under reduced pressure into solvent removal completely, obtains tripterygium hypoglaucum hutcs total alkaloid crude extract；
(6) silica gel is subjected to wet method dress post, tripterygium hypoglaucum hutcs total alkaloid crude extract crosses silicon after ethyl acetate dissolution is added
Rubber column gel column is eluted using ethyl acetate, eluent is collected after elution, after concentrate drying to obtain the final product.
Preferably, in the step (1), the mass ratio for tieing up plain enzyme and pectase is 3-6:1.
Preferably, in the step (2), ultrasonic power is 150-200W, and temperature is 50 ± 5 DEG C, extraction time 40-
60min。
Preferably, in the step (2), the relative density of concentrate is 11.2-11.8.
Preferably, in the step (3), the usage amount of acetic acid solution is 14-20 times of concentrate quality；Organic solvent extraction
The number taken is 3-4 times, and every time when extraction, the usage amount of organic solvent is 10-15 times of concentrate quality.
Preferably, in the step (4), the number of organic solvent extraction is 3-4 times, every time when extraction, organic solvent
Usage amount is 10-15 times of concentrate quality.
Preferably, the step (3), in step (4), organic solvent is chloroform, dichloroethanes, one in ethyl acetate
Kind.
Preferably, in the step (4), lye is sodium hydroxide or potassium hydroxide solution, concentration 1-2mol/L.
Preferably, in the step (6), the mesh number of silica gel is 100-200 mesh.
Preferably, in the step (6), silica gel dosage is the 8-13 of tripterygium hypoglaucum hutcs total alkaloid crude extract quality used
Times, the dosage of the ethyl acetate for elution is 80-110 times of tripterygium hypoglaucum hutcs total alkaloid crude extract quality used.
The beneficial effects of the present invention are:
The present invention is in preparing extraction purification tripterygium hypoglaucum hutcs when effective component alkaloid, using cellulase and pectase
It is digested simultaneously, can effectively destroy plant microscopic structure, the resistance to mass tranfer for dissolving out alkaloid from plant cell subtracts
It is low, effective component can Fast Stripping, and during enzymatic hydrolysis is with alcohol extracting, keeping system is acidity, can further promote biology
The dissolution of alkali.
Ultrasound is combined later, further tripterygium hypoglaucum hutcs cell wall is crushed, cavitation effect makes solvent to Chinese medicine
Permeability reinforce, and accelerate the solvation degree of ingredient to be extracted, increase the recovery rate of effective component effectively.It
Alkaloid therein is separated and refined using solvent extraction afterwards, and it is further pure to cooperate silica gel column chromatography technology to carry out
Change, the tripterygium hypoglaucum hutcs total alkaloid of purity is high can be obtained.
Operation of the present invention is simple, and total alkaloid yield is high in gained tripterygium hypoglaucum hutcs, and impurity content is few, and medical value is high.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Embodiment 1:
The method for extraction and purification of effective component in a kind of Yi nationality's medicine tripterygium hypoglaucum hutcs, comprising the following steps:
(1) root skin of tripterygium hypoglaucum hutcs is smashed it through into 100 meshes, phosphoric acid-sodium phosphate that 4 times of amount pH value are 5.5 is added
Buffer solution, be added 0.5% be made of cellulase and pectase mixed enzyme (mass ratio for tieing up plain enzyme and pectase is 4:
1) acetic acid diluted is added in, isothermal reaction 3h at 50 DEG C, and adjusting pH value is 95 DEG C of inactivations at 4.5,40 DEG C after isothermal reaction 1.5h
5min。
(2) the ethyl alcohol progress ultrasonic extraction that 11 times of amount mass fractions are 70% is then added, and (ultrasonic power is 200W, temperature
Degree is 50 DEG C, extraction time 60min), it is centrifuged after the completion of extracting, gained filter residue carries out second extraction, and (extraction conditions are same
Preceding primary extraction), merging filtrate, and by the way that concentrate is concentrated under reduced pressure to obtain, the relative density of concentrate is 11.7.
(3) acetic acid solution that 20 times of mass fraction of contracting liquid quality is 6.5% will be added in concentrate obtained by step (3)
After being dissolved, 15 times of concentrate quality are added has ethyl acetate extraction；Organic layer is abandoned when extraction, stays aqueous layer；Extraction
After 3-4 times, merge gained aqueous layer every time.
(4) pH value of aqueous layer is adjusted to 9.5 using the sodium hydroxide solution that concentration is 1mol/L, adds step
(3) ethyl acetate of 12 times of quality of concentrate of gained is extracted, and is abandoned aqueous layer, is stayed organic layer；After extraction 3-4 times, merge every
Secondary gained organic layer.
(5) organic layer is carried out being concentrated under reduced pressure into solvent removal completely, obtains tripterygium hypoglaucum hutcs total alkaloid crude extract.
(6) 100-200 mesh silica gel is adopted, wet method dress post is carried out, ethyl acetate is added in tripterygium hypoglaucum hutcs total alkaloid crude extract
It crosses silicagel column after dissolution, is eluted using ethyl acetate, eluent is collected after elution, after concentrate drying to obtain the final product.Wherein silica gel dosage
For 10 times of tripterygium hypoglaucum hutcs total alkaloid crude extract quality used, the dosage of the ethyl acetate for elution is Kun Mingshan used
100 times of Malus spectabilis total alkaloid crude extract quality.
Comparative example 1:
Unlike the first embodiment: not including step (1)；And in step (2), directly by the root skin powder of tripterygium hypoglaucum hutcs
After sieving with 100 mesh sieve after broken, ultrasonic extraction same as Example 1 is carried out, other steps and embodiment 1 cause.
Comparative example 2: unlike the first embodiment: step (2) is that the ethyl alcohol that 11 times of amount mass fractions are 70% is added to carry out
Refluxing extraction (extraction time 3h) is centrifuged after the completion of extracting, and gained filter residue carries out second extraction, and (extraction conditions are the same as previous
Secondary extraction), other steps and embodiment 1 cause.
In embodiment 1 in tripterygium hypoglaucum hutcs in total alkaloid and comparative example 1, comparative example 2 total alkaloid yield such as 1 institute of table
Show.
Table 1:
| Embodiment 1 | Comparative example 1 | Comparative example 2 | |
| Total alkaloid yield/% | 1.54 | 0.85 | 1.02 |
Embodiment 2:
The method for extraction and purification of effective component in a kind of Yi nationality's medicine tripterygium hypoglaucum hutcs, comprising the following steps:
(1) root skin of tripterygium hypoglaucum hutcs is smashed it through into 120 meshes, it is slow that phosphoric acid-sodium phosphate that 4 times of amount pH value are 5 is added
Rush solution, be added 0.4% be made of cellulase and pectase mixed enzyme (mass ratio for tieing up plain enzyme and pectase is 3:
1) acetic acid diluted is added in, isothermal reaction 3h at 55 DEG C, and adjusting pH value is 95 DEG C of inactivations at 4.5,40 DEG C after isothermal reaction 1.5h
5min；
(2) the ethyl alcohol progress ultrasonic extraction that 10 times of amount mass fractions are 70% is then added, and (ultrasonic power is 150W, temperature
Degree is 45 DEG C, extraction time 60min), it is centrifuged after the completion of extracting, gained filter residue carries out second extraction, and (extraction conditions are same
Preceding primary extraction), merging filtrate, and by the way that concentrate is concentrated under reduced pressure to obtain, the relative density of concentrate is 11.3；
(3) by be added in concentrate obtained by step (3) 14 times of mass fraction of contracting liquid quality for 8% acetic acid solution into
After row dissolution, 15 times of the chloroform that concentrate quality is added is extracted；Organic layer is abandoned when extraction, stays aqueous layer；Extraction 4 times
Afterwards, merge gained aqueous layer every time；
(4) pH value of aqueous layer is adjusted to 10 using the sodium hydroxide solution that concentration is 1-2mol/L, adds step
(3) chloroform of 13 times of quality of concentrate of gained is extracted, and is abandoned aqueous layer, is stayed organic layer；After extraction 4 times, merge gained every time
Organic layer；
(5) organic layer is carried out being concentrated under reduced pressure into solvent removal completely, obtains tripterygium hypoglaucum hutcs total alkaloid crude extract；
(6) 100-200 mesh silica gel is adopted, wet method dress post is carried out, ethyl acetate is added in tripterygium hypoglaucum hutcs total alkaloid crude extract
It crosses silicagel column after dissolution, is eluted using ethyl acetate, eluent is collected after elution, after concentrate drying to obtain the final product.Wherein silica gel dosage
For 13 times of tripterygium hypoglaucum hutcs total alkaloid crude extract quality used, the dosage of the ethyl acetate for elution is Kun Mingshan used
90 times of Malus spectabilis total alkaloid crude extract quality.
Comparative example 3:
Unlike the first embodiment: not including step (1)；And in step (2), directly by the root skin powder of tripterygium hypoglaucum hutcs
After crossing 120 meshes after broken, ultrasonic extraction same as Example 1 is carried out, other steps and embodiment 1 cause.
Comparative example 4: unlike the first embodiment: step (2) is that the ethyl alcohol that 10 times of amount mass fractions are 70% is added to carry out
Refluxing extraction (extraction time 3h) is centrifuged after the completion of extracting, and gained filter residue carries out second extraction, and (extraction conditions are the same as previous
Secondary extraction), other steps and embodiment 2 cause.
In embodiment 2 in tripterygium hypoglaucum hutcs in total alkaloid and comparative example 3, comparative example 4 total alkaloid yield such as 2 institute of table
Show.
Table 2:
| Embodiment 2 | Comparative example 3 | Comparative example 4 | |
| Total alkaloid yield/% | 1.43 | 0.78 | 0.98 |
Embodiment 3:
The method for extraction and purification of effective component in a kind of Yi nationality's medicine tripterygium hypoglaucum hutcs, comprising the following steps:
(1) root skin of tripterygium hypoglaucum hutcs is smashed it through into 150 meshes, phosphoric acid-sodium phosphate that 4 times of amount pH value are 5.5 is added
Buffer solution, be added 0.7% be made of cellulase and pectase mixed enzyme (mass ratio for tieing up plain enzyme and pectase is 5:
1) acetic acid diluted is added in, isothermal reaction 2h at 55 DEG C, and adjusting pH value is 90 DEG C of inactivations at 4.5,45 DEG C after isothermal reaction 1.5h
8min。
(2) the ethyl alcohol progress ultrasonic extraction that 11 times of amount mass fractions are 80% is then added, and (ultrasonic power is 200W, temperature
Degree is 50 DEG C, extraction time 50min), it is centrifuged after the completion of extracting, gained filter residue carries out second extraction, and (extraction conditions are same
Preceding primary extraction), merging filtrate, and by the way that concentrate is concentrated under reduced pressure to obtain, the relative density of concentrate is 11.5.
(3) by be added in concentrate obtained by step (3) 18 times of mass fraction of contracting liquid quality for 8% acetic acid solution into
After row dissolution, 10 times of the dichloroethanes extraction of concentrate quality is added；Organic layer is abandoned when extraction, stays aqueous layer；Extraction 4 times
Afterwards, merge gained aqueous layer every time.
(4) pH value of aqueous layer is adjusted to 9.5 using the sodium hydroxide solution that concentration is 2mol/L, adds step
(3) ethyl acetate of 10 times of quality of concentrate of gained is extracted, and is abandoned aqueous layer, is stayed organic layer；After extraction 3 times, merge each
Gained organic layer.
(5) organic layer is carried out being concentrated under reduced pressure into solvent removal completely, obtains tripterygium hypoglaucum hutcs total alkaloid crude extract.
(6) 100-200 mesh silica gel is adopted, wet method dress post is carried out, ethyl acetate is added in tripterygium hypoglaucum hutcs total alkaloid crude extract
It crosses silicagel column after dissolution, is eluted using ethyl acetate, eluent is collected after elution, after concentrate drying to obtain the final product.Wherein silica gel dosage
For 13 times of tripterygium hypoglaucum hutcs total alkaloid crude extract quality used, the dosage of the ethyl acetate for elution is Kun Mingshan used
80 times of Malus spectabilis total alkaloid crude extract quality.
Apply example 4:
The method for extraction and purification of effective component in a kind of Yi nationality's medicine tripterygium hypoglaucum hutcs, comprising the following steps:
(1) root skin of tripterygium hypoglaucum hutcs is smashed it through into 100 meshes, it is slow that phosphoric acid-sodium phosphate that 3 times of amount pH value are 6 is added
Rush solution, be added 0.4% be made of cellulase and pectase mixed enzyme (mass ratio for tieing up plain enzyme and pectase is 6:
1) acetic acid diluted is added in, isothermal reaction 2.5h at 50 DEG C, and adjusting pH value is 95 DEG C of inactivation 5min at 4,45 DEG C after isothermal reaction 1h.
(2) the ethyl alcohol progress ultrasonic extraction that 8 times of amount mass fractions are 60% is then added, and (ultrasonic power is 150W, temperature
Degree is 55 DEG C, extraction time 40min), it is centrifuged after the completion of extracting, gained filter residue carries out second extraction, and (extraction conditions are same
Preceding primary extraction), merging filtrate, and by the way that concentrate is concentrated under reduced pressure to obtain, the relative density of concentrate is 11.2.
(3) by be added in concentrate obtained by step (3) 14 times of mass fraction of contracting liquid quality for 5% acetic acid solution into
After row dissolution, 12 times of the chloroform extraction of concentrate quality is added；Organic layer is abandoned when extraction, stays aqueous layer；After extraction 3 times, close
And each gained aqueous layer.
(4) pH value of aqueous layer is adjusted to 10 using the potassium hydroxide solution that concentration is 1mol/L, adds step (3)
The ethyl acetate of 15 times of gained concentrate quality is extracted, and is abandoned aqueous layer, is stayed organic layer；After extraction 4 times, merge gained every time
Organic layer.
(5) organic layer is carried out being concentrated under reduced pressure into solvent removal completely, obtains tripterygium hypoglaucum hutcs total alkaloid crude extract.
(6) 100-200 mesh silica gel is adopted, wet method dress post is carried out, ethyl acetate is added in tripterygium hypoglaucum hutcs total alkaloid crude extract
It crosses silicagel column after dissolution, is eluted using ethyl acetate, eluent is collected after elution, after concentrate drying to obtain the final product.Wherein silica gel dosage
For 9 times of tripterygium hypoglaucum hutcs total alkaloid crude extract quality used, the dosage of the ethyl acetate for elution is Kun Mingshan used
110 times of Malus spectabilis total alkaloid crude extract quality.
Apply example 5:
The method for extraction and purification of effective component in a kind of Yi nationality's medicine tripterygium hypoglaucum hutcs, comprising the following steps:
(1) root skin of tripterygium hypoglaucum hutcs is smashed it through into 120 meshes, it is slow that phosphoric acid-sodium phosphate that 4 times of amount pH value are 5 is added
Rush solution, be added 0.6% be made of cellulase and pectase mixed enzyme (mass ratio for tieing up plain enzyme and pectase is 3:
1) acetic acid diluted is added in, isothermal reaction 3h at 55 DEG C, and adjusting pH value is 95 DEG C of inactivations at 4.5,35 DEG C after isothermal reaction 1.5h
8min。
(2) the ethyl alcohol progress ultrasonic extraction that 10 times of amount mass fractions are 70% is then added, and (ultrasonic power is 180W, temperature
Degree is 45 DEG C, extraction time 60min), it is centrifuged after the completion of extracting, gained filter residue carries out second extraction, and (extraction conditions are same
Preceding primary extraction),
Merging filtrate, and by the way that concentrate is concentrated under reduced pressure to obtain, the relative density of concentrate is 11.8.
(3) by be added in concentrate obtained by step (3) 20 times of mass fraction of contracting liquid quality for 7% acetic acid solution into
After row dissolution, 15 times of the ethyl acetate extraction of concentrate quality is added；Organic layer is abandoned when extraction, stays aqueous layer；Extraction 4 times
Afterwards, merge gained aqueous layer every time.
(4) pH value of aqueous layer is adjusted to 9 using the sodium hydroxide solution that concentration is 1mol/L, adds step (3)
The chloroform of 12 times of gained concentrate quality is extracted, and is abandoned aqueous layer, is stayed organic layer；After extraction 3 times, it is organic to merge gained every time
Layer.
(5) organic layer is carried out being concentrated under reduced pressure into solvent removal completely, obtains tripterygium hypoglaucum hutcs total alkaloid crude extract.
(6) 100-200 mesh silica gel is adopted, wet method dress post is carried out, ethyl acetate is added in tripterygium hypoglaucum hutcs total alkaloid crude extract
It crosses silicagel column after dissolution, is eluted using ethyl acetate, eluent is collected after elution, after concentrate drying to obtain the final product.Wherein silica gel dosage
For 13 times of tripterygium hypoglaucum hutcs total alkaloid crude extract quality used, the dosage of the ethyl acetate for elution is Kun Mingshan used
90 times of Malus spectabilis total alkaloid crude extract quality.
The yield of total alkaloid is as shown in table 3 in tripterygium hypoglaucum hutcs in embodiment 3-5.
Table 3:
| Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Total alkaloid yield/% | 1.45 | 1.39 | 1.51 |
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (10)
1. the method for extraction and purification of effective component in a kind of Yi nationality's medicine tripterygium hypoglaucum hutcs, which comprises the following steps:
(1) root skin of tripterygium hypoglaucum hutcs is smashed it through into 100-150 mesh, is added 3-4 times and measures the phosphoric acid-that pH value is 5.5 ± 0.5
The mixed enzyme of 0.4-0.7% being made of cellulase and pectase is added in buffer solution of sodium phosphate, and constant temperature is anti-at 50 ± 5 DEG C
2-3h to be answered, acetic acid diluted is added, adjusting pH value is 4-4.5, at 40 ± 5 DEG C after isothermal reaction 1-1.5h, 90-95 DEG C of inactivation 5-
8min；
(2) then be added 8-11 times measure mass fraction be 60-80% ethyl alcohol carry out ultrasonic extraction, extract after the completion of carry out from
The heart, gained filter residue carries out second extraction, merging filtrate, and passes through and concentrate is concentrated under reduced pressure to obtain；
(3) after being dissolved the acetic acid solution that concentrate addition mass fraction is 5-8%, organic solvent extraction is added, abandoning has
Machine layer, stays aqueous layer；
(4) pH value of aqueous layer is adjusted to 9.5 ± 0.5 using lye, adds organic solvent and is extracted, abandon aqueous layer,
Stay organic layer；
(5) organic layer is carried out being concentrated under reduced pressure into solvent removal completely, obtains tripterygium hypoglaucum hutcs total alkaloid crude extract；
(6) silica gel being subjected to wet method dress post, tripterygium hypoglaucum hutcs total alkaloid crude extract crosses silicagel column after ethyl acetate dissolution is added,
It is eluted using ethyl acetate, eluent is collected after elution, after concentrate drying to obtain the final product.
2. the method for extraction and purification of effective component in Yi nationality's medicine tripterygium hypoglaucum hutcs according to claim 1, which is characterized in that institute
It states in step (1), the mass ratio for tieing up plain enzyme and pectase is 3-6:1.
3. the method for extraction and purification of effective component in Yi nationality's medicine tripterygium hypoglaucum hutcs according to claim 1, which is characterized in that institute
It states in step (2), ultrasonic power is 150-200W, and temperature is 50 ± 5 DEG C, extraction time 40-60min.
4. the method for extraction and purification of effective component in Yi nationality's medicine tripterygium hypoglaucum hutcs according to claim 1, which is characterized in that institute
It states in step (2), the relative density of concentrate is 11.2-11.8.
5. the method for extraction and purification of effective component in Yi nationality's medicine tripterygium hypoglaucum hutcs according to claim 1, which is characterized in that institute
It states in step (3), the usage amount of acetic acid solution is 14-20 times of concentrate quality；The number of organic solvent extraction is 3-4 times,
Every time when extraction, the usage amount of organic solvent is 10-15 times of concentrate quality.
6. the method for extraction and purification of effective component in Yi nationality's medicine tripterygium hypoglaucum hutcs according to claim 1, which is characterized in that institute
It states in step (4), the number of organic solvent extraction is 3-4 times, and every time when extraction, the usage amount of organic solvent is concentrate quality
10-15 times.
7. the method for extraction and purification of effective component in Yi nationality's medicine tripterygium hypoglaucum hutcs according to claim 1, which is characterized in that institute
State step (3), in step (4), organic solvent is one of chloroform, dichloroethanes, ethyl acetate.
8. the method for extraction and purification of effective component in Yi nationality's medicine tripterygium hypoglaucum hutcs according to claim 1, which is characterized in that institute
It states in step (4), lye is sodium hydroxide or potassium hydroxide solution, concentration 1-2mol/L.
9. the method for extraction and purification of effective component in Yi nationality's medicine tripterygium hypoglaucum hutcs according to claim 1, which is characterized in that institute
It states in step (6), the mesh number of silica gel is 100-200 mesh.
10. the method for extraction and purification of effective component in Yi nationality's medicine tripterygium hypoglaucum hutcs according to claim 1, which is characterized in that
In the step (6), silica gel dosage is 8-13 times of tripterygium hypoglaucum hutcs total alkaloid crude extract quality used, the second for elution
The dosage of acetoacetic ester is 80-110 times of tripterygium hypoglaucum hutcs total alkaloid crude extract quality used.
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