CN108101843A - A kind of Sinomenine and its circular centrifugal preparation method - Google Patents
A kind of Sinomenine and its circular centrifugal preparation method Download PDFInfo
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- CN108101843A CN108101843A CN201810113194.4A CN201810113194A CN108101843A CN 108101843 A CN108101843 A CN 108101843A CN 201810113194 A CN201810113194 A CN 201810113194A CN 108101843 A CN108101843 A CN 108101843A
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- stage centrifugal
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- chloroform
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- INYYVPJSBIVGPH-QHRIQVFBSA-N Sinomenine Chemical compound C([C@@H]1N(CC2)C)C3=CC=C(OC)C(O)=C3[C@@]32[C@@H]1C=C(OC)C(=O)C3 INYYVPJSBIVGPH-QHRIQVFBSA-N 0.000 title claims abstract description 30
- INYYVPJSBIVGPH-UHFFFAOYSA-N 14-episinomenine Natural products C1CN(C)C2CC3=CC=C(OC)C(O)=C3C31C2C=C(OC)C(=O)C3 INYYVPJSBIVGPH-UHFFFAOYSA-N 0.000 title claims abstract description 25
- RARWEROUOQPTCJ-RBUKOAKNSA-N cepharamine Natural products C1CC2=CC=C(OC)C(O)=C2[C@@]2(CCN3C)[C@]13C=C(OC)C(=O)C2 RARWEROUOQPTCJ-RBUKOAKNSA-N 0.000 title claims abstract description 25
- 229930002966 sinomenine Natural products 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000000605 extraction Methods 0.000 claims abstract description 113
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 88
- 239000007788 liquid Substances 0.000 claims abstract description 57
- 239000000284 extract Substances 0.000 claims abstract description 36
- 230000008676 import Effects 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000003860 storage Methods 0.000 claims abstract description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 27
- 238000005119 centrifugation Methods 0.000 claims description 8
- INYYVPJSBIVGPH-VLXJIEOASA-N Cucoline Natural products C([C@H]1N(CC2)C)C3=CC=C(OC)C(O)=C3[C@@]32[C@@H]1C=C(OC)C(=O)C3 INYYVPJSBIVGPH-VLXJIEOASA-N 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000005984 hydrogenation reaction Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 description 18
- 238000012546 transfer Methods 0.000 description 16
- 238000002474 experimental method Methods 0.000 description 14
- 230000008569 process Effects 0.000 description 11
- 230000001351 cycling effect Effects 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000012530 fluid Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 239000012467 final product Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000013558 reference substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000005352 clarification Methods 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241001643409 Sinomenium acutum Species 0.000 description 1
- WEVYAHXRMPXWCK-UHFFFAOYSA-N acetonitrile Substances CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000012850 discrimination method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 230000003340 mental effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D221/00—Heterocyclic compounds containing six-membered rings having one nitrogen atom as the only ring hetero atom, not provided for by groups C07D211/00 - C07D219/00
- C07D221/02—Heterocyclic compounds containing six-membered rings having one nitrogen atom as the only ring hetero atom, not provided for by groups C07D211/00 - C07D219/00 condensed with carbocyclic rings or ring systems
- C07D221/22—Bridged ring systems
- C07D221/28—Morphinans
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a kind of Sinomenines and preparation method thereof, this method is to connect two extraction centrifuges, opens centrifugal extractor rotary drum motor, liquid with 10000 ls/h of speed from first-stage centrifugal extracter light phase import is pumped into, passes through two-stage centrifugal extracter；Extractant chloroform with 2500 ls/h of speed from two-stage centrifugal extracter heavy phase import is pumped into, then flows back to chloroform storage tank, is recycled；Extractant chloroform with 5000 ls/h of speed from first-stage centrifugal extracter heavy phase import is pumped into, then flows back to chloroform storage tank, is recycled；Detect the content of Sinomenine in two-stage centrifugal extracter light phase export extraction extraction raffinate, limit peak as；The content of Sinomenine in centrifugal extractor heavy out extract liquor is detected, limits peak, any limit value that reaches of the two stops Xun Huan, collects extract liquor, merge, obtain Sinomenine.Present device is inexpensive, less investment, at low cost.
Description
Technical field
The present invention relates to a kind of preparation method of drug, the circular centrifugal preparation side of more particularly to a kind of Sinomenine
Method.
Background technology
Sinomenine production is according to patent technique (application number ZL201110361882.0 or 201410366210.2)
It is produced, containing crude product and refined production.Production technology of crude is：Caulis sinomenii is taken, weight diacolation, percolate are carried out with dilute hydrochloric acid
Alkalization, centrifugation, are then extracted twice with chloroform, are concentrated, crystallization.Wherein, traditional mixing that is embodied as of extraction process is clarified
Liquid and extractant chloroform are stirred by formula --- extraction pot type with being placed in extractor, stand clarification layering, release
The extract liquor of lower floor is extracted twice, combining extraction liquid with this method.
It finds in production, there are the following problems for above-mentioned extraction process：Extracting and emulsifying is serious, and liquid and extractant chloroform mix
Two phase stratification is difficult after conjunction, makes wait separation time very long (tank needs 2~3 days), and has part emulsification that cannot seriously be layered (about
It accounts for 20%) and abandons, cause to extract low production efficiency, yield is low.
The content of the invention
Present invention aims at a kind of Sinomenine and preparation method thereof is provided, the present invention seeks to pass through following technology
What scheme was realized.
Two extraction centrifuges are connected, centrifugal extractor rotary drum motor are opened, by liquid with 10000 ls/h of speed
It is pumped into from first-stage centrifugal extracter light phase import, passes through two-stage centrifugal extracter；By extractant chloroform with 2500 ls/h
Speed be pumped into from two-stage centrifugal extracter heavy phase import, then flow back to chloroform storage tank, recycle；By extractant chloroform with 5000
L/h speed be pumped into from first-stage centrifugal extracter heavy phase import, then flow back to chloroform storage tank, recycle.Detect two level from
The content of Sinomenine, limits peak (such as 0.1mg/ml) in heart extracter light phase export extraction extraction raffinate；Detection centrifugation extraction
The content of Sinomenine in machine heavy out extract liquor is taken, limits peak (such as 100mg/ml), the two is any to reach restriction
Value stops Xun Huan, collects extract liquor, merges.
The Xun Huan two level cross-flow centrifugal extraction equipment can be, including chloroform storage tank (1)；Extraction transfer tank (2),
(4)；Extract relay pump (3), (5)；Liquid storage tank (6)；Liquid delivery pump (7)；First-stage centrifugal extractor (8)；Two-stage centrifugal extracts
Take device (9)；Heavy phase import (15), (17)；Heavy out (16), (18)；Light phase import (19), (21)；Light phase export (20),
(22)；Connecting pipeline (12), (13), (14), (23), (24), (25), (26), (27), (28)；
Wherein, the light phase import (21) of the light phase export (20) of first-stage centrifugal extractor (8) and two-stage centrifugal extractor (9)
It is connected；Chloroform storage tank (1) by connecting pipeline (13), (23) with extraction transfer tank (2) be connected, by connecting pipeline (13),
(26) it is connected with extraction transfer tank (4)；Extraction transfer tank (2) is connected by connecting pipeline (10) with extraction relay pump (3), then
It is connected by connecting pipeline (24) with the heavy phase import (15) of two-stage centrifugal extractor (9)；Extraction transfer tank (4) passes through connecting tube
Line (11) is connected with extraction relay pump (5), then the heavy phase import by connecting pipeline (27) and first-stage centrifugal extractor (8)
(17) it is connected；Liquid storage tank (6) is connected by connecting pipeline (12) with liquid delivery pump (7), then by connecting pipeline (28) with
The light phase import (19) of first-stage centrifugal extractor (8) is connected；The heavy out (18) of first-stage centrifugal extractor (8) passes through connecting tube
Line (14) is connected with extraction transfer tank (4)；The heavy out (16) of two-stage centrifugal extractor (9) passes through connecting pipeline (25) and extraction
Transfer tank (2) is taken to be connected.
Description of the drawings
Fig. 1 cycles two level cross-flow Centrifugical extraction schematic diagram
1 is chloroform storage tank；2nd, 4 be extraction transfer tank；3rd, 5 be extraction relay pump；6 be liquid storage tank；7 is defeated for liquid
Send pump；8 be first-stage centrifugal extractor；9 be two-stage centrifugal extractor；15th, 17 be heavy phase import；16th, 18 be that heavy phase goes out
Mouthful；19th, 21 be light phase import；20th, 22 be light phase export；12nd, 13,14,23,24,25,26,27,28 be connecting tube
Line
Fig. 2 cucolines " Xun Huan two level cross-flow Centrifugical extraction " experimental channel connection figure
Experimental example 1：Circular centrifugal extraction process (Xun Huan two level cross-flow Centrifugical extraction)
Circular centrifugal extraction on the basis of one-stage centrifugal extracts extraction or multistage centrifugal extraction, sets an extractant
Transfer tank, extractant is recycled.This technique is illustrated exemplified by cycling two level cross-flow Centrifugical extraction.
Process
Two extraction centrifuges are connected by schematic diagram, open centrifugal extractor rotary drum motor, liquid is extracted from first-stage centrifugal
Machine light phase import is taken to be pumped into, passes through two-stage centrifugal extracter；By extractant chloroform with 1/4 times of liquid speed amount speed from
Two-stage centrifugal extracter heavy phase import is pumped into, then flows back to chloroform storage tank, is recycled；By extractant chloroform with the 1/ of liquid speed
2 times of amount speed are pumped into from first-stage centrifugal extracter heavy phase import, then flow back to chloroform storage tank, are recycled.Detect two-stage centrifugal extraction
The content of Sinomenine in machine light phase export extraction extraction raffinate is taken, limits peak (such as 0.1mg/ml)；Detect centrifugal extractor
The content of Sinomenine in heavy out extract liquor limits peak (such as 100mg/ml), and the two is any to reach limit value i.e.
Stop Xun Huan, collect extract liquor, merge.
Production efficiency
Production capacity (handles gauge) with liquid：It is 12 that now selected centrifugal extractor maximum, which can be fabricated to mixing flux,
Ten thousand ls/h, can continuous production, extraction production efficiency be：【120000/(1+1/2)】/ 1000=80m3/h.
Extract output of fluid：Complete in similary extraction, extraction output of fluid is about the 5%~14% of liquid volume.
Technique problems and advantages
Inferior position：1st, equipment is not with using the single-stage of Xun Huan or multistage centrifugal extraction phase ratio, increasing expense.But compared with extractor
It compares, input is more.
Advantage：1st, technique and material adaptability are good, in extracter complete mixing, extraction, separated overall process, using from
Mental and physical efforts separate, and extracting and demixing, emulsion layer demulsification are quick, and production is smooth.
2nd, it is easy to operate, and can continuous production.
3rd, production capacity is huge, is 128 times (80/0.625) for mixing clarification formula.
4th, extraction process does not lose, and (extraction yield=receive must extract liquid measure/chloroform inventory to extraction high income, about
100%).
5th, extracting output of fluid, small (cycle two level cross-flow centrifugal extracting process is about the 5%~14% of liquid volume, and is not used
The two level cross-flow centrifugal extracting process of circulation technology is about the 75% of liquid volume), while extracting complete, extract liquor quantity
Few, lower process needs the also few of concentration, and lower process production efficiency improves, and production cost declines, and productivity effect improves.
6th, above advantage, it is comprehensive to cause production efficiency height, production cost low.
Experimental example 2：Experimental study data
First, experiment purpose
Previous experiments have determined that extraction process is Centrifugical extraction, it is contemplated that extraction output of fluid is larger, to subsequent concentration process
Pressure is very big.On the premise of extraction yield is met, output of fluid is extracted to reduce, while reduces the consumption of chloroform, through analyzing hydrochloric acid
The solubility property of cucoline and chloroform and extraction principle are intended intending using " cycling extraction " technique on the basis of centrifugal extraction.For
Confirm the feasibility of technique, carry out this extraction experiments.
2nd, experimental method
(1) design of two level cross-flow centrifugal extracting process is cycled
Utilization according to material characteristic and to Centrifugical extraction principle, devises cycling extraction technique, and band expects equipment manufacturer
It is tested.On the basis of two level cross-flow Centrifugical extraction, chloroform is recycled by taking two level cross-flow Centrifugical extraction as an example for experiment.
Fig. 2 is shown in equipment pipe connection, connects two extraction centrifuges by schematic diagram, opens centrifugal extractor rotary drum motor,
Liquid from first-stage centrifugal extracter light phase import is pumped into, passes through two-stage centrifugal extracter；By extractant chloroform respectively with phase
When 1/2 l/h of speed of liquid is pumped into from first-stage centrifugal extracter heavy phase import, then level-one chloroform tank is flowed back to, recycled；
It is pumped into the speed of suitable 1/4 l/h of liquid from two-stage centrifugal extracter heavy phase import, then flows back to two chloroform tanks, cycling makes
With.The content of Sinomenine in two-stage centrifugal extracter light phase export extraction extraction raffinate is detected, limits peak (such as 0.1mg/
ml)；The content of Sinomenine in detection centrifugal extractor heavy out extract liquor, restriction peak (such as 100mg/ml), two
Any limit value that reaches of person stops Xun Huan, collects extract liquor, merges.
Extract liquor and extraction extraction raffinate sample is taken to do sinomenium acutum alkali content measure during experiment.
Investigate whether technique is applicable in, main inspection target：Whether can extract completely, calculate extraction yield, >=95% is extraction
Completely.
(2) sample cucoline Content Test method (liquid chromatography) is extracted
Chromatographic condition：【According to cucoline discrimination method result of study early period】：C18 chromatographic columns, 0.78% phosphoric acid of mobile phase
Dihydro sodium solution-acetonitrile (85:15), Detection wavelength 265nm.
1st, prepared by reference substance
Take cucoline reference substance appropriate, it is accurately weighed, add 0.01mol/L hydrochloric acid solutions be made every milliliter containing 100 micrograms it is molten
Liquid shakes up to obtain the final product.
2nd, sample treatment
(1), " liquid before extraction " sample treatment
Take this product appropriate, filter paper filtering, precision measures 2ml into 100ml measuring bottles, and 0.01mol/L hydrochloric acid is added to be shaken to scale
It is even to obtain the final product.
(2), " extraction extraction raffinate ", " extract liquor " sample treatment
Take this product appropriate, filter paper filtering, precision measures 2ml and volatilized to water-bath, adds 0.01mol/L hydrochloric acid molten three times in right amount
Solution, is fully transferred in 100ml measuring bottles, 0.01mol/L hydrochloric acid is added to be shaken up to scale to obtain the final product.
3rd, assay method
It is accurate respectively to draw reference substance solution and each 20 microlitres of test solution, liquid chromatograph is injected, is measured, is calculated,
To obtain the final product.
4th, result judgement
When extracting complete, extraction extraction raffinate content is less than 0.1mg/ml.
3rd, experiment equipment
Solution S 20160501, about 300kg after the basified centrifugation of caulis sinomenii diacolation extract Workshop Production, mailing to experiment
Ground；
Chloroform 1 barrel (300kg), 6mol/L hydrochloric acid is appropriate, sample plot purchase；
Sampling bottle 40, precision test paper, it is several；
150 type of centrifugal extractor and flow pump, storage tank, totally two sets, Zhengzhou day one extracts company
50 type of centrifugal extractor and flow pump, storage tank, totally two sets, Zhengzhou day one extracts company
4th, experimentation
Test the date:On July 28th, 2016
Place：Zhengzhou day one extracts company's laboratory weather：It is cloudy, 28 DEG C
(1) liquid pre-treatment
PH=8.5 is adjusted with hydrochloric acid before liquid experiment, is sampled 1 (liquid before extraction).
(2) experimental program
1st, after experiment is started by Xun Huan two level cross-flow centrifugal extracting process, flow set and sampling according to the form below carry out, and change
Flow set and sampling are not shut down.Medicinal liquid flow is fixed as 120L/h, and the experimental propulsion of chloroform flow is adjusted accordingly
It is whole, investigate influence of the flow velocity change to extraction.
Sampling：Extract liquor, extraction extraction raffinate
2nd, further to investigate influence of the flow velocity to extraction, separately plus the experiment of 50 machines has been done, each flow velocity is only in experiment
Vertical experiment.
5th, experimental result and analysis
(1), 150 type press proof product examine measured data such as following table
Analysis
1st, the extract liquor of two samples leaks in transit, fails to detect, but end-point analysis is not caused to determine
Property influence.
2nd, the extraction extraction raffinate content of each period is very low, and far below 0.2mg/ml, and extraction yield is very high, shows sample
Product extract completely, can also further carry out cycling extraction.In 140min, extraction liquid measure is liquid volume：(20+20)/
(120*140/60) * 100%=14.3%.
3rd, with the extension of extraction process, content is in be gradually increasing trend for level-one, two level extraction liquid hold-up；According to trend point
Analysis, when extraction liquid hold-up increases to a certain degree, because the increase of Dissolve things inside, extract liquor proportion can raise, and viscosity can increase,
Motor load can aggravate.When reaching a certain content (such as 100mg/ml), motor is more than live load, must stop cycle, change
New chloroform carries out cycling extraction.Or when extracting a specified time, extraction extraction raffinate content goes beyond the limit (0.2mg/ml), must also stop
Xun Huan renews chloroform and carries out cycling extraction.Because pilot scale liquid volume is limited, the content of extract liquor is only being given birth to greatly during stop in cycling
It is measured in production.It when reaching stop in Xun Huan, is counted using extracting liquid hold-up as 100mg/ml, according to above-mentioned data trend, level-one extraction
Take 18 times that liquid hold-up is about two level extraction liquid hold-up, then estimation extraction liquid measure is liquid volume：(20+20)/ {(20*100
+ 20*100/18) */2.69 }=5%.
(2), 50 type press proof product examine measured data such as following table
Analysis
1st, partial extraction liquid sample leaks in transit, fails to detect, but end-point analysis is not caused decisive
It influences.
2nd, each flow velocity proportioning test of the experimental result of comprehensive 150 type machines and 50 type machines, liquid and extractant, 1:3、1:
2、1:1、1:0.75、1:0.5、1:0.25, extraction is complete.
6th, experiment conclusion
Circular centrifugal extraction process confirms feasible.The outstanding advantage of the technique, exemplified by cycling two-stage centrifugal extraction process,
On the basis of similary extraction is complete, extraction liquid measure is about the 5%~14% of liquid volume, and does not use the two level of circulation technology wrong
It is about the 75% of liquid volume to flow centrifugal extracting process.Extract liquor quantity is few, and lower process needs the also few of concentration, chloroform consumption
Also reduce, production efficiency improves, and production cost declines, and productivity effect improves.
Embodiment 1
Two level cross-flow centrifugal extraction equipment is cycled, including chloroform storage tank (1)；Extract transfer tank (2), (4)；Extract relay pump
(3)、(5)；Liquid storage tank (6)；Liquid delivery pump (7)；First-stage centrifugal extractor (8)；Two-stage centrifugal extractor (9)；Heavy phase into
Mouth (15), (17)；Heavy out (16), (18)；Light phase import (19), (21)；Light phase export (20), (22)；Connecting pipeline
(12)、(13)、(14)、(23)、(24)、 (25)、(26)、(27)、(28)；
Wherein, the light phase import (21) of the light phase export (20) of first-stage centrifugal extractor (8) and two-stage centrifugal extractor (9)
It is connected；Chloroform storage tank (1) by connecting pipeline (13), (23) with extraction transfer tank (2) be connected, by connecting pipeline (13),
(26) it is connected with extraction transfer tank (4)；Extraction transfer tank (2) is connected by connecting pipeline (10) with extraction relay pump (3), then is led to
Connecting pipeline (24) is crossed with the heavy phase import (15) of two-stage centrifugal extractor (9) to be connected；Extraction transfer tank (4) passes through connecting tube
Line (11) is connected with extraction relay pump (5), then the heavy phase import by connecting pipeline (27) and first-stage centrifugal extractor (8)
(17) it is connected；Liquid storage tank (6) is connected by connecting pipeline (12) with liquid delivery pump (7), then by connecting pipeline (28) with
The light phase import (19) of first-stage centrifugal extractor (8) is connected；The heavy out (18) of first-stage centrifugal extractor (8) passes through connecting tube
Line (14) is connected with extraction transfer tank (4)；The heavy out (16) of two-stage centrifugal extractor (9) passes through connecting pipeline (25) and extraction
Transfer tank (2) is taken to be connected.
Embodiment 2：Sinomenine is prepared using 1 cycling extraction equipment of embodiment
Two extraction centrifuges are connected, centrifugal extractor rotary drum motor are opened, by liquid with 10000 ls/h of speed
It is pumped into from first-stage centrifugal extracter light phase import, passes through two-stage centrifugal extracter；By extractant chloroform with 2500 ls/h
Speed be pumped into from two-stage centrifugal extracter heavy phase import, then flow back to chloroform storage tank, recycle；By extractant chloroform with 5000
L/h speed be pumped into from first-stage centrifugal extracter heavy phase import, then flow back to chloroform storage tank, recycle；Detect two level from
The content of Sinomenine, limits peak (such as 0.1mg/ml) in heart extracter light phase export extraction extraction raffinate；Detection centrifugation extraction
The content of Sinomenine in machine heavy out extract liquor is taken, limits peak (such as 100mg/ml), the two is any to reach restriction
Value stops Xun Huan, collects extract liquor, merges.
Liquid of the present invention is prepared by the following method：Caulis sinomenii is taken, by the use of 0.3mol/L hydrochloric acid solutions as solvent, is moistened
Wet, dipping, diacolation, percolate hydrogenation calcium oxide adjust pH value to 11~12, and centrifugation, filtration collect filtrate, with 6mol/L hydrochloric acid
It is 8~9 that solution, which adjusts pH value, obtains liquid.
Claims (2)
1. a kind of Sinomenine, it is characterised in that the Sinomenine is made by the following method, connects two extraction centrifuges,
Centrifugal extractor rotary drum motor is opened, by liquid with 10000 ls/h of speed from first-stage centrifugal extracter light phase import pump
Enter, pass through two-stage centrifugal extracter；By extractant chloroform with 2500 ls/h of speed from two-stage centrifugal extracter heavy phase into
Mouth is pumped into, then flows back to chloroform storage tank, is recycled；Extractant chloroform is extracted with 5000 ls/h of speed from first-stage centrifugal
Machine heavy phase import is pumped into, then flows back to chloroform storage tank, is recycled；Detect salt in two-stage centrifugal extracter light phase export extraction extraction raffinate
The content of sour cucoline, limit peak as；Detect the content of Sinomenine in centrifugal extractor heavy out extract liquor, limit
Determine peak, any limit value that reaches of the two stops Xun Huan, collects extract liquor, merge, obtain Sinomenine；
The liquid is prepared by the following method：Caulis sinomenii is taken, by the use of 0.3mol/L hydrochloric acid solutions as solvent, soaks, impregnate, ooze
It filters, percolate hydrogenation calcium oxide adjusts pH value to 11~12, and filtrate is collected in centrifugation, filtration, and pH is adjusted with 6mol/L hydrochloric acid solutions
It is worth for 8~9, obtains liquid.
2. a kind of preparation method of Sinomenine, it is characterised in that this method is to connect two extraction centrifuges, opens centrifugation
Liquid with 10000 ls/h of speed from first-stage centrifugal extracter light phase import is pumped into, passed through by extracter rotary drum motor
Two-stage centrifugal extracter；Extractant chloroform is pumped into 2500 ls/h of speed from two-stage centrifugal extracter heavy phase import, then
Chloroform storage tank is flowed back to, is recycled；By extractant chloroform with 5000 ls/h of speed from first-stage centrifugal extracter heavy phase import
It is pumped into, then flows back to chloroform storage tank, recycle；Detect Sinomenine in two-stage centrifugal extracter light phase export extraction extraction raffinate
Content limits peak；The content of Sinomenine in detection centrifugal extractor heavy out extract liquor, restriction peak, two
Any limit value that reaches of person stops Xun Huan, collects extract liquor, merges, obtain Sinomenine；
The liquid is prepared by the following method：Caulis sinomenii is taken, by the use of 0.3mol/L hydrochloric acid solutions as solvent, soaks, impregnate, ooze
It filters, percolate hydrogenation calcium oxide adjusts pH value to 11~12, and filtrate is collected in centrifugation, filtration, and pH is adjusted with 6mol/L hydrochloric acid solutions
It is worth for 8~9, obtains liquid.
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| CN113797583A (en) * | 2021-08-25 | 2021-12-17 | 合肥通用机械研究院有限公司 | A kind of extraction pilot-scale method based on crude drug centrifugal solvent extraction system |
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