CN109503571A - A kind of method of dehydrocorydaline in D101 macroporous resin purification rhizoma corydalis - Google Patents
A kind of method of dehydrocorydaline in D101 macroporous resin purification rhizoma corydalis Download PDFInfo
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Abstract
The invention belongs to chemical analysis technology field, a kind of method of dehydrocorydaline in D101 macroporous resin purification rhizoma corydalis is disclosed；Dehydrocorydaline in rhizoma corydalis is extracted using flash method, and 0.12g medicinal material/mL is made as load solution in extracting solution；140mL sample solution is taken, D101 macroporous resin column, coutroi velocity 2mL/min, loading absorption are passed through；It first uses the distillation water elution of 3BV after having adsorbed, then uses 70mL, 70% ethanol solution of concentration is eluant, eluent, and with the elution of the rate of 3mL/min, eluent is concentrated to dryness to obtain the final product.The method of rhizoma corydalis extracting solution D101 macroporous resin purification provided by the invention, simple process, the rapid and effective method that can rationally become purifying dehydrocorydaline.Using purification process provided by the invention, the content of dehydrocorydaline is increased to 4.65% from 0.33%.
Description
Technical field
It is purple that the invention belongs to dehydrogenations in chemical analysis technology field more particularly to a kind of D101 macroporous resin purification rhizoma corydalis
The method of violet alkali.
Background technique
Rhizoma corydalis also known as corydalis tuber are the dry tubers of opium poppy section Genus Corydalis, are one of famous " eight Zhe's ", and
Clinically common Chinese medicine.Rhizoma corydalis ingredient is complicated, and effective component is mainly alkaloid.Tetrahydropalmatine is that its is main
Analgesia, calm ingredient.And the effective component dehydrocorydaline of rhizoma corydalis single medicinal material preparation " Kedaling " has expansion coronal dynamic
The effects of arteries and veins is the main active for treating coronary heart diseases and angina pectoris.Dehydrocorydaline (Dehydrocorydaline, referred to as
DHC) belong to isoquinilone derivatives Alkaloid.Total alkali and tetrahydropalmatine side are concentrated mainly on about the research of rhizoma corydalis at present
Face, and the research of the extraction separation method of dehydrocorydaline is reported fewer.
Currently, in the industry dehydrocorydaline extraction separation the prior art be such that medicinal powder add alcohol reflux extract,
Ultrasonic extraction or medicinal powder use chloroform refluxing extraction after being moistened with 10% ammonium hydroxide again.Extracting solution recycling design obtains total medicinal extract,
Add dilute hydrochloric acid to pinch molten, filter off insoluble matter, acid liquid is extracted with chloroform again, is recycled chloroform, is obtained solid content.Solid content uses silica gel again
Column chromatography for separation, preparative high performance liquid chromatography or high speed adverse current chromatogram further isolate and purify.
In conclusion problem of the existing technology is:
(1) ethyl alcohol and chloroform equal solvent dosage are big in the extraction process of dehydrocorydaline, and extraction time is long, at high cost.Chlorine
It imitates easily to make malicious class harmful influence, buys and cumbersome using formality, and be more toxic, the contact of unsuitable large dosage for a long time.
(2) the solid content dehydrogenation purple alkali content obtained after chloroform extraction is lower, also contains a large amount of lipophilic contaminant, directly
Silica gel column chromatography separation needs repeated multiple times column chromatography, and experimental period is long, and solvent consumption is big, and in addition column chromatography can then be made repeatedly
At the absorption of dehydrocorydaline on silica gel, cause to waste.Silica gel after chromatography can not be reused, and solid waste object amount is big,
Processing cost is high, is unfavorable for environmental protection.
(3) preparative high performance liquid chromatography or high speed adverse current chromatogram are required in separation process using a large amount of organic solvents,
Recovered solvent re-uses difficulty, and separation costs are high, and quantity of three wastes is big.
Solve the difficulty and meaning of above-mentioned technical problem:
The dosage of organic solvent how is reduced, organic solvent loss is reduced, recycles Extraction solvent and separation material, contracting
Short extraction disengaging time, improves recovery rate and the rate of recovery is urgent problem, finds the green of one kind efficiently, less toxic and extracts
Separation method is particularly important.Homogenate extraction method is based on historrhexis's principle, by material quick crashing, while with high-speed stirring
Mix, it is superpower vibration, negative pressure diafiltration the effects of realize extract, it retains effective ingredients in plant to the maximum extent and is notheated destruction,
It is small with solvent usage, extraction time is short, extraction efficiency is high, Extraction solvent lose small, low power consumption and other advantages.Macroporous absorbent resin
The features such as big with adsorption capacity, adsorption rate is fast, and consumption of organic solvent is few, resin renewable use.Homogenate extraction combines big
Resin separation in hole can shorten extraction time and effectively be enriched with the dehydrocorydaline content in extracting solution, the second recycled in extracting solution
Alcohol is used as the Extraction solvent of next group medicinal material after can diluting again, reduce extraction cost.Concentrate after recycling ethyl alcohol can be direct
Upper prop absorption shortens the production cycle and reduces energy consumption without further concentration and filtering.
Summary of the invention
In view of the problems of the existing technology, it is purple that the present invention provides dehydrogenations in a kind of D101 macroporous resin purification rhizoma corydalis
The method of violet alkali.It is dark brown solid powder by Corydalis P.E after purification, bitter can be used as and prepare Kedaling piece
Raw material, principle active component is dehydrocorydaline in Kedaling piece.Kedaling piece has activating microcirculation and removing stasis medicinal, the effect of sharp gas analgesic.
It can be used for coronary heart disease, the illness of angina pectoris, acute myocardial infarction, chest distress, palpitation and dizziness of remote myocardial infarction etc. is controlled
It treats.
The invention is realized in this way in a kind of D101 macroporous resin purification rhizoma corydalis dehydrocorydaline method, specifically
The following steps are included:
Step 1: dehydrocorydaline in rhizoma corydalis is extracted using flash method.It is appropriate to weigh corydalis tuber medicinal material, puts into flash mention
It takes in the container of device, 20 times of 50% ethyl alcohol of amount is then added, impregnate 20min, homogenate extraction 2min.Filtering, filtrate recycling ethanol
Into extracting solution, medicinal material containing 0.12g/mL solution is as macroreticular resin load solution；It is dilute after the alcohol determining concentration of alcohol of recycling
Release the Extraction solvent for being re-used as next group medicinal material to 50%；
Step 2: taking 140mL sample solution, passes through D101 macroporous resin column, coutroi velocity 2mL/min, loading absorption；
Step 3: macroreticular resin first uses the distillation water elution of 3BV after having adsorbed, then with 70mL ethanol solution is eluant, eluent,
It is eluted with the rate of 3mL/min, eluent is concentrated to dryness to obtain the final product.
Further, in step 2, D101 macroporous resin column, diameter height fills column than 1: 7,7.0g resin.
Further, in step 3, ethanol solution be 70% ethanol solution.
Another object of the present invention is to provide one kind by dehydrocorydaline in the D101 macroporous resin purification rhizoma corydalis
Method preparation dehydrocorydaline.
Another object of the present invention is to provide a kind of Kedaling tablet raw materials prepared by the dehydrocorydaline.
It is used to treat coronary heart disease by prepared by the dehydrocorydaline another object of the present invention is to provide a kind of, the heart twists
Bitterly, acute myocardial infarction, the drug of the chest distress of remote myocardial infarction, palpitation and dizziness.
In conclusion advantages of the present invention and good effect are as follows:, homogenate extraction method compares back the recovery rate of dehydrocorydaline
Stream extraction method is high by about 8%, and extraction time is only the 1/30 of reflux extraction.Homogenate extraction method has efficient, quick, energy-efficient
Advantage.
The method of rhizoma corydalis extracting solution D101 macroporous resin purification provided by the invention, simple process can rationally become pure
The rapid and effective method of fluidized dehydrogenation corydaline.Using purification process provided by the invention, the content of dehydrocorydaline is from 0.33%
It is increased to 4.65%.
This experiment extracts dehydrocorydaline in rhizoma corydalis using flash method, and extracting solution is simultaneously carried out pure with D101 macroreticular resin
Change, the results showed that homogenate extraction method is better than reflux extraction and ultrasonic extraction, has high-efficient, extraction time short feature.
Concentration is used to can get higher DHC recovery rate for the extraction of 50% ethyl alcohol, but lower ethanol content will lead in extracting solution again
Water-solubility impurity increases, therefore by dehydrocorydaline in D101 macroporous resin purification rhizoma corydalis extracting solution, can remove major part
Water-solubility impurity, macroreticular resin can effectively be enriched with dehydrocorydaline, after purification the solid content in extracting solution
It is substantially reduced, the mass fraction of dehydrocorydaline is significantly increased.
Macroreticular resin has good suction-operated to dehydrocorydaline, and adsorption capacity is big, and adsorption rate is fast.Sample solution concentration
Higher, adsorption efficiency is higher, but with the increase of sample solution concentration, it is raw that new precipitating is had during solution continuous concentration
At needing filtration treatment before loading, increase filter progress, will cause new loss.In addition, the more highly enriched mistake of sample solution concentration
Journey energy consumption is bigger, and filters more difficult, the increase production cycle.Not only there is higher recovery rate using the extraction of 50% ethyl alcohol and obtains
Extracting solution recycling ethyl alcohol to no alcohol taste after to can reach concentration substantially be 0.12g medicinal material/mL, and solution is without new precipitating generation,
It can directly loading absorption without filtering.The process purification condition is scientific and reasonable, suitable for the purifying of dehydrocorydaline, is expected to be used for
Dehydrocorydaline large-scale production in rhizoma corydalis.
Detailed description of the invention
Fig. 1 is the method flow of dehydrocorydaline in D101 macroporous resin purification rhizoma corydalis provided in an embodiment of the present invention
Figure.
Fig. 2 is different temperatures adsorption curve figure provided in an embodiment of the present invention.
Fig. 3 is leakage plot figure provided in an embodiment of the present invention.
Fig. 4 is DHC elution curve provided in an embodiment of the present invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Application principle of the invention is further elaborated with reference to the accompanying drawing；
As shown in Figure 1, in D101 macroporous resin purification rhizoma corydalis provided in an embodiment of the present invention dehydrocorydaline method,
Specifically includes the following steps:
S101: dehydrocorydaline in rhizoma corydalis is extracted using flash method.It is appropriate to weigh corydalis tuber medicinal material, puts into homogenate extraction
In the container of device, 20 times of 50% ethyl alcohol of amount are then added, impregnate 20min, homogenate extraction 2min.Filtering, filtrate recycling ethanol is extremely
Medicinal material containing 0.12g/mL solution is as macroreticular resin load solution in extracting solution；It is diluted after the alcohol determining concentration of alcohol of recycling
The Extraction solvent for being re-used as next group medicinal material to 50%；
S102: taking 140mL sample solution, passes through D101 macroporous resin column, coutroi velocity 2mL/min, loading absorption；
S103: macroreticular resin first uses the distillation water elution of 3BV after having adsorbed, then with 70mL ethanol solution is eluant, eluent, with
The rate of 3mL/min elutes, and eluent is concentrated to dryness to obtain the final product.
In step S102, D101 macroporous resin column provided in an embodiment of the present invention, diameter height fills column than 1: 7,7.0g resin.
In step S103, ethanol solution provided in an embodiment of the present invention be 70% ethanol solution.
Application principle of the invention is further elaborated below with reference to specific experiment；
Experiment 1；
1, instrument and material
(1) instrument
JHBE-50T flash extracter (Henan Jin Ding development in science and technology Co., Ltd), SHA-C constant temperature oscillator (enterprise, China, state
Industry), Waters high performance liquid chromatograph (2487 ultraviolet spectrometry detector).
(2) material
Rhizoma corydalis (medicinal material parent company, the city Hao Zhou, Anhui Province, Pan'an produce)；Macroreticular resin (Dong Hong Chemical Co., Ltd.)；Dehydrogenation
Corydaline reference substance (Shanghai Ya Ji Biotechnology Co., Ltd)；Acetonitrile is chromatographically pure (the limited public affairs of Chinese medicines group chemical reagent
Department)；Water is pure water.
2, method and result
(1) assay of dehydrocorydaline
Precision weighs dehydrocorydaline reference substance 9.2mg, is placed in 50mL volumetric flask, and methanol dissolves and be diluted to scale,
It shakes up, as reference stock solution.Precision measure dehydrocorydaline reference stock solution methanol dilution at 0,9.2,18.4,
36.8,73.6 μ g/mL solution, it is accurate respectively to measure 20 μ L injection permaphase ODS (5um, 4.6mm × 250mm), with acetonitrile-
0.03mol/L sodium dihydrogen phosphate (19:41) is mobile phase, and flow velocity 0.6mL/min, Detection wavelength 345nm measure dehydrogenation corydalis
Alkali peak area, using peak area as ordinate, dehydrocorydaline content is that abscissa draws standard curve, and obtaining regression equation is Y=
97722X+17538, r=0.9992.The result shows that dehydrocorydaline is within the scope of mass concentration 0-73.6 μ g/mL and peak area
Linear relationship is good.
(2) determination of dehydrocorydaline extracting method
Tri- parts of corydalis tuber medicinal material 60.0g are weighed respectively, adds 20 times of 50% ethyl alcohol of amount, then respectively with homogenate extraction, reflux
It extracts and three kinds of methods of ultrasonic extraction is extracted, filtering, extracting solution is concentrated into no alcohol taste, and each extracting solution, which is settled to 500mL with water, to be held
It is spare in measuring bottle.
Extracting solution made from the accurate above-mentioned Different Extraction Method of measurement is appropriate respectively, is settled in 50mL volumetric flask, to
0.45 μm of filtering with microporous membrane is up to test solution.Dehydrocorydaline peak area is measured by the method under 2.1, calculates dehydrogenation
The recovery rate of corydaline, the results are shown in Table 1.
The content of dehydrocorydaline in 1 Different Extraction Method extracting solution of table
From table 1 it follows that homogenate extraction method will be mentioned better than other two kinds no matter from recovery rate or extraction time
It follows the example of, therefore dehydrocorydaline in rhizoma corydalis is extracted using homogenate extraction method.
(2) screening of resin
It accurately weighs above-mentioned various wet resin 1g, in the conical flask being respectively charged into, 20mL rhizoma corydalis extracting solution is added, it will
Above-mentioned sample is put into shaking table, oscillation absorption 2h.Extracting solution after absorption is filtered, filtrate surveys its peak area.Filtered wet tree
Rouge is refunded in original triangular flask, and the 70% ethyl alcohol 20mL oscillation desorption 2h of addition is placed for 24 hours.Solution after desorption filters, solution
Imbibition surveys its peak area after suitably diluting.The adsorption rate and desorption efficiency of each resin the results are shown in Table 2.Adsorbance Q=(C0-Cr)*V/
W adsorption rate=Q/C0* V desorption quantity=C*V/Q/W desorption efficiency=parsing amount/Q Q is adsorbance (mg/g), C0It is molten before absorption
DHC concentration in liquid, CrDHC concentration in solution after absorption, DHC concentration, V- adsorption liquid volume, W- resin in solution after C- desorption
Weight in wet base.
The resin Primary Screening Test result of 2 different model of table
The absorption property of this 3 kinds of resins of D101, AB-8, HP20 is preferable as can be seen from the table, but the desorption effect of AB-8
Not as good as other two kinds.The absorption of D101 resin and desorption effect are all preferable, therefore D101 may be selected as rhizoma corydalis extracting solution
Purification Resin.
(4) D101 macroreticular resin Static Adsorption dynamics is investigated
1) apparent adsorption rate measures
Filtered wet resin is accurately weighed, is put into band plug triangular flask, the rhizoma corydalis extracting solution of addition.At normal temperature
(25 DEG C) oscillation absorption.Its peak area is surveyed in sampling at regular intervals, calculates the adsorbance of DHC, experimental result is shown in Table 3.
3 adsorbance of table changes with time relationship
At 25 DEG C D101 resin to the curve of adsorption kinetics of DHC using first order kinetics parameter of curve t as abscissa, ln
(qe-qt) it is ordinate, fitting obtains straight line ln (0.974-qt)=- 0.0265t-0.9943, linearly dependent coefficient are
r2=0.8998, correlation is poor.Using second-order kinetics parameter of curve t as abscissa, t/qtFor ordinate, fitting obtains one
Straight line t/qt=0.391t+0.4627, linearly dependent coefficient r2=0.9998, correlation is very high.Pass through linearly related property coefficient
It can be seen that second-order kinetic equation is more suitable for than first _ order kinetics equation for describing the adsorption process, with second-order kinetics mould
Type obtains D101 to the equilibrium adsorption capacity theoretical value 2.557mgg of DHC-1Resin and measured value 2.56mgg-1Resin is consistent
It closes.It the results are shown in Table 4.
The fitting absorption of table 4:2 kind kinetic model takes the parameter and related coefficient of curve
Note: k1It is first order kinetics rate constant；k2It is second-order kinetics rate constant.
2) temperature influences to investigate on Static Adsorption
Wet resin 2g after pre-processing is weighed, rhizoma corydalis extracting solution 30mL is added, sets and vibrates certain time in constant-temperature table, point
Kong Zhi not be 25 DEG C, 35 DEG C and 45 DEG C of temperature, the content of dehydrocorydaline is measured by sampling at regular intervals, drafting is inhaled at each temperature
Attached kinetic curve, the influence of investigation and temperature to adsorption dynamics adsorption kinetics, experimental result are as shown in Figure 2.
As shown in Fig. 2, different temperatures adsorption curve figure provided in an embodiment of the present invention.
As shown in Fig. 2, 30min curve is all relatively steep before adsorbing under different temperatures, it is very fast to illustrate that adsorbance increases.60-90min
Plateau, adsorbance increase slowly, and more than occurring flat line after 90min, absorption basically reaches balance.At different temperatures
D101 essentially coincides the Static Adsorption curve of DHC, and temperature change influence dynamic (dynamical) on D101 resin Static Adsorption is unobvious.
Therefore, room temperature may be selected as adsorption temp.
3) influence of the sample concentration to macroporous resin adsorption effect
Concentration 0.06,0.12,0.24,0.36g medicinal material/mL solution is made by dilution and concentration in sample solution, is respectively taken
30mL is added separately to 2.0g macroreticular resin, and 25 DEG C of oscillations adsorb 2h, measure each adsorption equilibrium liquid DHC mass concentration, calculates absorption
Amount, respectively 1.27,2.54,4.97,6.20mg/g resin.Sample solution concentration is too low to make loading to adsorb identical amount
Volume increases, and increases separation cycle.The excessively high macroporous resin adsorption that will lead to of sample solution concentration is insufficient, reduces adsorption rate.When upper
Macroreticular resin has been saturated the adsorbance of dehydrocorydaline when sample liquid concentration is 0.36g medicinal material/mL, has part DHC unadsorbed.
In addition, can generate new precipitating in extracting solution concentration process needs when sample solution concentration increases to 0.12g medicinal material/mL or more
It filters.Therefore, choosing 0.12g medicinal material/mL is best sample solution concentration.
4) influence of the strippant concentration of alcohol to desorption effect
After the macroreticular resin adsorbed washing, then being separately added into 30mL volume fraction is 30%, 50%, 70%, 90%
Ethanol solution, 25 DEG C of oscillations desorb 2h, measure dehydrocorydaline mass concentration in each stripping liquid, calculate desorption efficiency, respectively
59.59%, 94.15%, 96.62% and 79.27%.With the increase of volume fraction of ethanol, dehydrocorydaline desorption takes the lead in fast
Speed reduces after increasing.When volume fraction of ethanol is 70%, desorption efficiency is up to 96.62%, is further continued for increasing ethyl alcohol volume point
Number, desorption efficiency declines instead this is because DHC is not easy to elute in 90% ethyl alcohol solubility reduction.Therefore 70% second of selection
Alcoholic solution is strippant.
(5) D101 macroreticular resin Dynamic Adsorption dynamics is investigated
1) loading volume investigates (leakage plot investigation)
D101 macroreticular resin loading volume is determined by measuring the leakage curve of dehydrocorydaline.Precision measures 0.12g
Medicinal material/mL sample solution 200mL, by D101 macroporous resin column (diameter height fills column than 1: 7,7.0g resin), coutroi velocity is about
For 1mL/min, Fractional Collections efflux, every 20mL collects a, the mass concentration of dehydrocorydaline in the every portion of measurement, with stream
Liquid stream part is abscissa out, and dehydrocorydaline mass concentration is ordinate, draws leakage curve, and experimental result is as shown in Figure 3.
As shown in figure 3, leakage plot figure provided in an embodiment of the present invention.
As shown in figure 3, leakage rate increases suddenly when loading volume reaches 160mL, flowed out when loading volume reaches 180ml
DHC gradually tends towards stability in liquid.Selected loading volume of the DHC amount of leakage no more than 5% is best loading volume.Loading volume
When 140mL, amount of leakage 2.93%, and when loading volume 160mL, amount of leakage 11.96%.In order to be sufficiently reserved ingredient,
The loss of DHC during reduction loading, therefore select 140mL for best loading volume.
2) loading flow velocity is investigated
Precision measures each 3 parts of 0.12g medicinal material/mL sample solution 140mL, passes through 3 D101 type macropore exchange resin columns respectively,
And coutroi velocity is about the absorption of 1mL/min, 2mL/min, 3mL/min loading respectively, collects efflux, measurement efflux dehydrogenation is purple
The mass concentration of violet alkali calculates adsorption rate, respectively 98.15%, 97.11%, 88.37%.Loading flow velocity increases, sample and big
Hole resin contact time shortens, and will lead to sample cannot sufficiently adsorb[6].Flow velocity compared with being conducive to sample and macroreticular resin is abundant slowly
Contact increases adsorption rate.But flow velocity will lead to separation cycle extension slowly excessively, and production efficiency reduces, therefore uses 2mL/min flow velocity
Loading absorption.
3) washing dosage is investigated
Precision measures sample solution 140mL, and by D101 type macropore exchange resin column, coutroi velocity is about 2mL/min stream
Measure loading, respectively use 1BV, the water elution of 3BV, 5BV, then use 70% ethyl alcohol, elution speed 3mL/min be eluted to without obviously
Color collects eluent, measures the mass concentration of dehydrocorydaline, calculates DHC yield, respectively 95.56%, 95.34%,
95.10%, it is not much different in yield, and solid content is less after 3BV and 5BV elution, the mass concentration of dehydrocorydaline is higher,
Therefore the water elution of 3BV is used.
4) determination of elution flow rate
By sample solution upper prop, after the completion of Dynamic Adsorption, distillation water elution is first used, then take 70% ethanol solution of certain volume
Respectively with 2mL/min, 3mL/min, 4mL/min flow velocity elution collects eluent, measures the mass concentration of dehydrocorydaline, counts
Calculate eluting rate, respectively 97.15%, 96.15% and 92.33%.Elution flow rate is too fast, eluant, eluent and resin insufficient contact,
Elution not exclusively, will reach the dosage that identical elution effect needs to increase eluant, eluent.The too slow then elution time of elution flow rate becomes
It is long.Dehydrocorydaline desorption efficiency is higher when elution flow rate is 3mL/min, and elution time is also shorter.Thus select washing for 3mL/min
Separation of flow speed is eluted.
5) elution volume determines
By sample solution upper prop, after Dynamic Adsorption is complete, distillation water elution is first used, then take 70% ethanol solution of certain volume
With the elution of 3mL/min flow velocity, every 10mL is one group of collection eluent, and measures dehydrocorydaline mass concentration in eluent, is drawn
Dynamic elution curve, experimental result is as shown in Figure 4.
As shown in figure 4, DHC elution curve provided in an embodiment of the present invention.
As shown in figure 4, when 70% ethanol elution volume reaches 20mL, dehydrocorydaline mass concentration highest in eluent,
Elution speed is very fast.It is further added by elution volume later, the dehydrocorydaline mass concentration afforded is gradually reduced, when elution body
When product is 70mL, curve tends to be horizontal, and dehydrocorydaline has been eluted completely substantially, therefore eluting agent 70mL is preferred.
(6) macroporous resin purification DHC technique determines
Dehydrocorydaline in rhizoma corydalis is extracted using flash method, and it is molten as loading that 0.12g medicinal material/mL is made in extracting solution
Liquid takes 140mL sample solution, passes through D101 macroporous resin column (diameter height fills column than 1: 7,7.0g resin), coutroi velocity 2mL/
Min, loading absorption first with the distillation water elution of 3BV after adsorb, then with 70mL70% ethanol solution are eluant, eluent, with 3mL/
The rate of min elutes, and eluent is concentrated to dryness to obtain the final product.
(7) before purification after in Corydalis P.E dehydrocorydaline comparision contents
3 batches of samples are prepared by above-mentioned technique, measure the mass fraction of DHC.After 50% ethyl alcohol homogenate extraction of rhizoma corydalis, extract
Liquid concentration, concentrate is again through D101 macroporous resin purification.The mass fraction of DHC in medicinal material, crude extract and purified is compared
Compared with the results are shown in Table 5.Dehydrocorydaline content is increased to by 0.33% in Corydalis P.E after macroporous resin purification
The mass fraction of 4.65%, DHC improve 13.5 times, and solid object amount is substantially reduced in purified solution.
Table 5 before purification after in Corydalis P.E dehydrocorydaline comparision contents
3, conclusion
The present invention extracts dehydrocorydaline in rhizoma corydalis using flash method, and extracting solution is simultaneously carried out pure with D101 macroreticular resin
Change, the results showed that homogenate extraction method is better than other two kinds of extraction methods, has high-efficient, extraction time short feature.Using concentration
It can get higher DHC recovery rate for the extraction of 50% ethyl alcohol, but to will lead to water solubility in extracting solution again miscellaneous for lower ethanol content
Matter increases, therefore by dehydrocorydaline in D101 macroporous resin purification rhizoma corydalis extracting solution, can remove most of water-soluble miscellaneous
Matter, macroreticular resin can effectively be enriched with dehydrocorydaline, and the solid content in extracting solution is substantially reduced after purification,
The mass fraction of dehydrocorydaline is significantly increased.
Macroreticular resin has good suction-operated to dehydrocorydaline, and adsorption capacity is big, and adsorption rate is fast.Sample solution concentration
Higher, adsorption efficiency is higher, but with the increase of sample solution concentration, it is raw that new precipitating is had during solution continuous concentration
At needing filtration treatment before loading, increase filter progress, will cause new loss.In addition, the more highly enriched mistake of sample solution concentration
Journey energy consumption is bigger, and filters more difficult, the increase production cycle.Not only there is higher recovery rate using the extraction of 50% ethyl alcohol and obtains
Extracting solution recycling ethyl alcohol to no alcohol taste after to can reach concentration substantially be 0.12g medicinal material/mL, and solution is without new precipitating generation,
It can directly loading absorption without filtering.The process purification condition is scientific and reasonable, suitable for the purifying of dehydrocorydaline, is expected to be used for
Dehydrocorydaline large-scale production in rhizoma corydalis.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (6)
1. a kind of method of dehydrocorydaline in D101 macroporous resin purification rhizoma corydalis, which is characterized in that the D101 macropore
In purifying resin rhizoma corydalis dehydrocorydaline method the following steps are included:
Step 1: dehydrocorydaline in rhizoma corydalis is extracted using flash method；It is appropriate to weigh corydalis tuber medicinal material, puts into flash extracter
Container in, then be added 20 times of 50% ethyl alcohol of amount, immersion 20min, homogenate extraction 2min.Filtering, filtrate recycling ethanol is to mentioning
Take medicinal material containing 0.12g in liquid/mL solution as macroreticular resin load solution；It is diluted to after the alcohol determining concentration of alcohol of recycling
50% is re-used as the Extraction solvent of next group medicinal material；
Step 2: taking 140mL sample solution, passes through D101 macroporous resin column, coutroi velocity 2mL/min, loading absorption；
Step 3: macroreticular resin first uses the distillation water elution of 3BV after having adsorbed, then with 70mL ethanol solution is eluant, eluent, with
The rate of 3mL/min elutes, and eluent is concentrated to dryness to obtain the final product.
2. the method for dehydrocorydaline in D101 macroporous resin purification rhizoma corydalis as described in claim 1, which is characterized in that institute
It states in step 2, D101 macroporous resin column, diameter height fills column than 1: 7,7.0g resin.
3. the method for dehydrocorydaline in D101 macroporous resin purification rhizoma corydalis as described in claim 1, which is characterized in that institute
It states in step 3, the ethanol solution that ethanol solution is 70%.
4. the dehydrogenation of the method preparation of dehydrocorydaline is purple in a kind of D101 macroporous resin purification rhizoma corydalis as described in claim 1
Violet alkali.
5. a kind of Kedaling tablet raw material of the preparation of the dehydrocorydaline as described in claim 4.
6. a kind of preparation of the dehydrocorydaline as described in claim 4 for treating coronary heart disease, angina pectoris, acute myocardial infarction,
The drug of the chest distress of remote myocardial infarction, palpitation and dizziness.
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| CN116602966A (en) * | 2023-05-11 | 2023-08-18 | 华宝民康(广东)医药集团有限公司 | Application of 13-methyl-palmatine in preparation of medicines for resisting myocardial ischemia injury and heart fibrosis |
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