CN109438460A - The method of tetrandra root A prime and tetrandra root B prime is extracted from tetrandra root - Google Patents
The method of tetrandra root A prime and tetrandra root B prime is extracted from tetrandra root Download PDFInfo
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- CN109438460A CN109438460A CN201811498299.2A CN201811498299A CN109438460A CN 109438460 A CN109438460 A CN 109438460A CN 201811498299 A CN201811498299 A CN 201811498299A CN 109438460 A CN109438460 A CN 109438460A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D491/00—Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00
- C07D491/12—Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00 in which the condensed system contains three hetero rings
- C07D491/18—Bridged systems
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Abstract
The present invention provides a kind of method that tetrandra root A prime and tetrandra root B prime are extracted from tetrandra root, the specific steps of which are as follows: dry tetrandra root root crushes, bacillus subtilis and saccharomycetes to make fermentation is added, alcohol extracting, filtering, is concentrated to give concentrate, salt acid pH, butanol, before immunoassay obtain water phase A and butanol, before immunoassay liquid A；To butanol, before immunoassay liquid A sodium hydroxide and salt acid pH, butanol, before immunoassay is concentrated, sodium carbonate liquor dissolution, filtering, and alcohol crystal obtains tetrandra root A prime；Fetch water phase A, sodium hydroxide to pH value, butanol, before immunoassay, concentration, sodium carbonate liquor dissolution, filtering, and alcohol crystal obtains tetrandra root B prime.The present invention can effectively improve the yield of tetrandra root alkaloid, reduce the difficulty of wastewater treatment, improve the utilization rate of tetrandra root resource.
Description
Technical field
The invention belongs to field of natural product extraction, are related to a kind of side that tetrandra root A prime and tetrandra root B prime are extracted from tetrandra root
Method.
Background technique
Tetrandra root is aristolochiaceae plant, is used as medicine with root, and root is cylindrical, how many to be bent, and traverse furrow, length 6 are got deeply stuck in knee
~15cm, 1.5~3cm of diameter.Crust light brown or light brown yellow, scraping off crust is ecru.Matter is solid, not easily broken, breaks
Face is uneven, and thorn-like, cross section canescence to yellow-white, mealiness, skin zone is thicker, and woody part beam lark is arranged radially.Taste
Hardship, micro-puckery.With block, big, skin depth, rich mealiness person are preferred.Main product Hanzhong Area of Shaanxi.In addition, Hubei, Hunan, Sichuan, Yunnan etc.
Ground.The four seasons can harvest, but preferably section season quarrier.Silt and fibrous root are removed after taking root, scrape off or does not scrape off cork, is shone
Extremely half-dried, diameter is half-and-half rived in 2.5cm or more, is dried.Main ingredient is containing aristolochic acid, cupreol, wood in root
Magnoflorine, allantoin etc..Function is the major functions: wind-dispelling Li Shui, dehumidifying analgesia.For head edema of limbs, waist and knee joints pain etc..
It is more to tetrandra root effective component research at present, such as Xu Yingshu using TLC method separation Stephania tetrandra in hanfangchin A,
B prime can obtain root of fangji A prime and B prime compared with high yield pulp1, but TLC method can not carry out industrialized production.Yellow waterside sun, Zhen Pan etc.
Using the research of hanfangchin A is extracted from Fourstamen Stephania Root axis, leaf, although obtaining the hanfangchin A and B prime of high-purity
Product, but resin and toxic reagent are largely used during the separation process, and the yield for obtaining effective component is low, therefore is producing
It in the process can not scale application.The patent of Publication No. CN102382119A discloses a kind of Tetrandrine and Radix Stephaniae Tetrandrae second
The extracting method of element mixes Radix Stephaniae Tetrandrae powder and calcium lime powder, total alkaloid medicinal extract is obtained using alcohol extracting, after adjusting pH to 2~4
Extraction, stratification；Extract liquor therein is restored through alkalization, and obtained extract acetone solution is filtered, crystallization is concentrated,
It obtains Tetrandrine crude product to recrystallize again, obtains Tetrandrine product；By acidic aqueous solution tune pH9~11 after standing,
The extract acetone solution that will be obtained after extraction, is filtered, crystallization is concentrated, and is obtained Demethyl-tetrandrine crude product and is recrystallized again, obtains
To Demethyl-tetrandrine product.The method is efficiently avoided using toxic reagent and purifying resin, due in raw material disposal process
In, basification directly is carried out using quick lime, dissolution of the starch to its alkaloid in tetrandra root root has been seriously affected, has directly resulted in
The yield of alkaloid is low, while increasing the difficulty of later period wastewater treatment.
Summary of the invention
The problems such as generating a large amount of waste water in not high, extraction process for existing tetrandra root recovery rate, the present invention provide it is a kind of from
The method that tetrandra root A prime and tetrandra root B prime are extracted in tetrandra root, can effectively improve the yield of tetrandra root alkaloid, reduce wastewater treatment
Difficulty improves the utilization rate of tetrandra root resource.
The specific steps of which are as follows:
(1) dry tetrandra root root crushes, and water to water content is added and reaches 30%~50%, fermentation of bacillus subtilis 2~3 is added
It, adds saccharomycetes to make fermentation 2~3 days, adds 60~80% ethanol solution refluxing extraction 2 times, each 2h, filtering, merging filtrate,
Filtrate be concentrated under reduced pressure at 55 DEG C~65 DEG C original volume 1/10~/40 concentrate；
(2) 0.1mol/L hydrochloric acid is added to pH2.5~3 to concentrate, is extracted, is obtained with the butanol of two to four times of volumes
Water phase A and butanol, before immunoassay liquid A；
(3) 0.01mol/L sodium hydroxide solution is added to pH9~10 to butanol, before immunoassay liquid A, stratification obtains solution C (no
Containing butanol), it with 0.1mol/L hydrochloric acid to pH2.5~3, is extracted with the butanol of two to four times of volumes, obtains butanol, before immunoassay liquid B；
(4) butanol, before immunoassay liquid B is concentrated to dryness at 50~65 DEG C, obtains dried object A, then 1mol/L is added thereto
Sodium carbonate liquor is dissolved, filtering, and ethyl alcohol is added to final concentration of 60~70%, carries out crystallizing to obtain tetrandra root A prime；
(5) fetch water phase A, 0.01mol/L sodium hydroxide solution is added to pH9~10, the butanol of two to four times of volumes of use into
Row extraction, obtains butanol, before immunoassay liquid D,
(6) butanol, before immunoassay liquid D is concentrated to dryness at 50~65 DEG C, obtains dried object B, then thereto be added 0.5~
1mol/L sodium carbonate liquor is dissolved, filtering, and ethyl alcohol is added to final concentration of 50~60%, carries out crystallizing to obtain tetrandra root B prime.
Described to be filtered into ceramic membrane filter 1 time, fenestra pore size is 0.22 μm.
The bacillus subtilis and barms can be made by oneself according to a conventional method, can also directly buy from market,
Such as Angel Yeast.
The amount of bacillus subtilis is added in the step (1), is 5~15:100 by volume L/ feed with paper-mulberry leaf weight kg ratio；
The amount of saccharomycete, is 5~15:100 by volume L/ feed with paper-mulberry leaf weight kg ratio, and fermented and cultured temperature is 28~30 DEG C.
In a specific embodiment, step (1) the amount L and tetrandra root weight kg that 60~80% ethanol solutions are added
Than for 0.5~4:1.
In a specific embodiment, step (4) amount that sodium carbonate liquor is added, by volume L and dried object A weight
Amount kg ratio is 2~5:1.
In a specific embodiment, step (6) amount that sodium carbonate liquor is added, by volume L and dried object B weight
Amount kg ratio is 2~5:1.
Technical effect
1, using bacillus subtilis and saccharomycete mixed fermentation, consumption of starch is fallen completely, effectively prevents tetrandra root root
The influence to the dissolution of its alkaloid in the high temperature process of middle starch.
2, by multi-strain fermentation, be conducive to the conversion of alkaloid in tetrandra root root, improve tetrandra root A prime and tetrandra root B prime
Yield, reduce production cost, section medicine tetrandra root medicine resource.
Specific embodiment
Embodiment 1
It takes the dry tetrandra root root of 100kg to crush, water to water content is added and reaches 35%, 10L fermentation of bacillus subtilis 2 is added
It, adds 12L saccharomycetes to make fermentation 3 days, adds 75% ethanol solution 200L refluxing extraction 2h, filtering, then is added into filter residue
75% ethanol solution 200L refluxing extraction 2h, filtering, filtrate, filtrate are concentrated under reduced pressure into 20L at 55 DEG C and obtain concentrate twice for merging；
0.1mol/L hydrochloric acid is added to pH2.5 to concentrate, is extracted with 60L butanol, obtains water phase A and butanol, before immunoassay liquid A；To butanol
0.001mol/L sodium hydroxide solution is added to pH9 in extract liquor A, and stratification obtains 5L solution C (without butanol), uses 0.1mol/L
Hydrochloric acid is extracted with 20L butanol to pH2.5, obtains butanol, before immunoassay liquid B；Butanol, before immunoassay liquid B is concentrated under reduced pressure at 55 DEG C
It is dry, 2.48kg dried object A is obtained, then 0.5mol/L sodium carbonate liquor 8L is added thereto and is dissolved, filters, ethyl alcohol is added to end
Concentration is 65%, carries out crystallizing to obtain 1.83kg tetrandra root A prime.
Fetch water phase A, and 0.01mol/L sodium hydroxide solution is added to pH9, is extracted with 50L butanol, obtains butanol, before immunoassay liquid
Butanol, before immunoassay liquid D is concentrated to dryness at 55 DEG C, obtains 1.96kg dried object B by D, then 0.5mol/L carbonic acid is added thereto
Sodium solution 10L is dissolved, filtering, and ethyl alcohol is added to final concentration of 55%, carries out crystallizing to obtain 1.57kg tetrandra root B prime.Through HPLC
Method detects, in obtained product, the content 98.72% of tetrandra root A prime, and the content 98.87% of tetrandra root B prime.
Comparative examples 1
It takes the dry tetrandra root root of 100kg to crush, adds 75% ethanol solution 200L refluxing extraction 2h, filter, then be added into filter residue
75% ethanol solution 200L refluxing extraction 2h, filtering, filtrate, filtrate are concentrated under reduced pressure into 20L at 55 DEG C and obtain concentrate twice for merging；
0.1mol/L hydrochloric acid is added to pH2.5 to concentrate, is extracted with 60L butanol, obtains water phase A and butanol, before immunoassay liquid A；To butanol
0.001mol/L sodium hydroxide solution is added to pH9 in extract liquor A, and stratification obtains 4L solution C (without butanol), uses 0.1mol/L
Hydrochloric acid is extracted with 20L butanol to pH2.5, obtains butanol, before immunoassay liquid B；Butanol, before immunoassay liquid B is concentrated under reduced pressure at 55 DEG C
It is dry, 1.25kg dried object A is obtained, then 0.5mol/L sodium carbonate liquor 4L is added thereto and is dissolved, filters, ethyl alcohol is added to end
Concentration is 65%, carries out crystallizing to obtain 0.95kg tetrandra root A prime.
Fetch water phase A, and 0.01mol/L sodium hydroxide solution is added to pH9, is extracted with 50L butanol, obtains butanol, before immunoassay liquid
Butanol, before immunoassay liquid D is concentrated to dryness at 55 DEG C, obtains 1.05kg dried object B by D, then 0.5mol/L carbonic acid is added thereto
Sodium solution 10L is dissolved, filtering, and ethyl alcohol is added to final concentration of 55%, carries out crystallizing to obtain 0.48kg tetrandra root B prime.Through HPLC
Method detects, in obtained product, the content 98.65% of tetrandra root A prime, and the content 98.81% of tetrandra root B prime.
Embodiment 2
It takes the dry tetrandra root root of 200kg to crush, water to water content is added and reaches 40%, 20L fermentation of bacillus subtilis 2 is added
It, adds 22L saccharomycetes to make fermentation 3 days, adds 75% ethanol solution 500L refluxing extraction 2h, filtering, then is added into filter residue
75% ethanol solution 300L refluxing extraction 2h, filtering, filtrate, filtrate are concentrated under reduced pressure into 40L at 55 DEG C and obtain concentrate twice for merging；
0.1mol/L hydrochloric acid is added to pH2.5 to concentrate, is extracted with 120L butanol, obtains water phase A and butanol, before immunoassay liquid A；Xiang Ding
0.001mol/L sodium hydroxide solution is added to pH9 in alcohol extract liquor A, and stratification obtains 8L solution C (without butanol), uses
0.1mol/L hydrochloric acid is extracted with 30L butanol to pH2.5, obtains butanol, before immunoassay liquid B；By butanol, before immunoassay liquid B at 50~65 DEG C
It is concentrated to dryness, obtains 5.05kg dried object A, then 1mol/L sodium carbonate liquor 15L is added thereto and is dissolved, filter, add
Enter ethyl alcohol to final concentration of 60~70%, carries out crystallizing to obtain 4.12kg tetrandra root A prime.
Fetch water phase A, and 0.01mol/L sodium hydroxide solution is added to pH9, is extracted with 120L butanol, obtains butanol, before immunoassay
Butanol, before immunoassay liquid D is concentrated to dryness at 50~65 DEG C, obtains 4.28kg dried object B, then 1mol/L is added thereto by liquid D
Sodium carbonate liquor is dissolved, filtering, and ethyl alcohol is added to final concentration of 50~60%, carries out crystallizing to obtain 3.26kg tetrandra root B prime.
It is detected through HPLC method, in obtained product, the content 98.81% of tetrandra root A prime, the content 98.93% of tetrandra root B prime.
Claims (6)
1. a kind of method that tetrandra root A prime and tetrandra root B prime are extracted from tetrandra root, the specific steps of which are as follows:
(1) dry tetrandra root root crushes, and water to water content is added and reaches 30%~50%, is added fermentation of bacillus subtilis 2~3 days,
It adds saccharomycetes to make fermentation 2~3 days, adds 60~80% ethanol solution refluxing extraction 2 times, each 2h, filter, merging filtrate, filter
Liquid be concentrated under reduced pressure at 55 DEG C~65 DEG C original volume 1/10~/40 concentrate；
(2) 0.1mol/L hydrochloric acid is added to pH2.5~3 to concentrate, is extracted with the butanol of two to four times of volumes, obtains water phase
A and butanol, before immunoassay liquid A；
(3) 0.01mol/L sodium hydroxide solution is added to pH9~10 to butanol, before immunoassay liquid A, stratification obtains solution C (without fourth
Alcohol), it with 0.1mol/L hydrochloric acid to pH2.5~3, is extracted with the butanol of two to four times of volumes, obtains butanol, before immunoassay liquid B；
(4) butanol, before immunoassay liquid B is concentrated to dryness at 50~65 DEG C, obtains dried object A, then 1mol/L carbonic acid is added thereto
Sodium solution is dissolved, filtering, and ethyl alcohol is added to final concentration of 60~70%, carries out crystallizing to obtain tetrandra root A prime；
(5) fetch water phase A, and 0.01mol/L sodium hydroxide solution is added to pH9~10, is extracted with the butanol of two to four times of volumes
It takes, obtains butanol, before immunoassay liquid D,
(6) butanol, before immunoassay liquid D is concentrated to dryness at 50~65 DEG C, obtains dried object B, then 0.5~1mol/ is added thereto
L sodium carbonate liquor is dissolved, filtering, and ethyl alcohol is added to final concentration of 50~60%, carries out crystallizing to obtain tetrandra root B prime.
2. the method according to claim 1, described to be filtered into ceramic membrane filter 1 time, fenestra pore size is 0.22 μm.
3. the method according to claim 1, the middle amount that bacillus subtilis is added of the step (1), by volume L/ feed with paper-mulberry leaf weight
Amount kg ratio is 5~15:100；The amount of saccharomycete, is 5~15:100 by volume L/ feed with paper-mulberry leaf weight kg ratio, and fermented and cultured temperature is
28~30 DEG C.
4. the method according to claim 1, step (1) amount L and tetrandra root weight the kg ratio that 60~80% ethanol solutions are added
For 0.5~4:1.
5. the method according to claim 1, step (4) amount that sodium carbonate liquor is added, by volume L and dried object A weight
Kg ratio is 2~5:1.
6. the method according to claim 1, step (6) amount that sodium carbonate liquor is added, by volume L and dried object B weight
Kg ratio is 2~5:1.
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| CN201811498299.2A CN109438460A (en) | 2018-12-08 | 2018-12-08 | The method of tetrandra root A prime and tetrandra root B prime is extracted from tetrandra root |
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| CN201811498299.2A CN109438460A (en) | 2018-12-08 | 2018-12-08 | The method of tetrandra root A prime and tetrandra root B prime is extracted from tetrandra root |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112608328A (en) * | 2020-12-24 | 2021-04-06 | 重庆医药高等专科学校 | Crystal form of 5-bromotetrandrine ethyl formate and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112608328A (en) * | 2020-12-24 | 2021-04-06 | 重庆医药高等专科学校 | Crystal form of 5-bromotetrandrine ethyl formate and preparation method thereof |
| CN112608328B (en) * | 2020-12-24 | 2021-09-28 | 重庆医药高等专科学校 | Crystal form of 5-bromotetrandrine ethyl formate and preparation method thereof |
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Application publication date: 20190308 |