CN105106305A - Continuous alcohol precipitation method - Google Patents
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- CN105106305A CN105106305A CN201510555023.3A CN201510555023A CN105106305A CN 105106305 A CN105106305 A CN 105106305A CN 201510555023 A CN201510555023 A CN 201510555023A CN 105106305 A CN105106305 A CN 105106305A
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Abstract
The invention provides a continuous alcohol precipitation method. According to the method, a micro mixer is used for continuous mixing of concentrated solutions and ethanol solutions. The method has the advantages that operation process is simple, effective component packet loss can be reduced, the whole alcohol precipitation process can be continuous and stable, control difficulty is reduced and quality stability of Chinese patent medicine obtained by a water extraction and alcohol precipitation method is finally improved, thereby being capable of being popularized and implemented in production of traditional Chinese medicine to serve as a novel method for alcohol precipitation.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicine pharmacy, particularly a kind of method of continuous alcohol precipitation.
Background technology
Precipitate with ethanol is the conventional isolation technics that Chinese patent medicine is produced, and is used for the concentrated solution processing Chinese medicine water boiling concentration gained, has purification capacity strong, solvent safety and the advantage such as easy and simple to handle.Because precipitate with ethanol can remove the plurality of impurities such as deproteinize, saccharide, inorganic salt, tannin and pigment, remarkable lifting drug safety, so the Chinese medicine very high to security requirement also have employed the production technology of water extract-alcohol precipitation in a large number, as Radix Salviae Miltiorrhizae Injection and GUANXINNING ZHUSHEYE etc.
Concentrated solution is generally first placed in Alcohol-settling tank by current Chinese medicine precipitate with ethanol, then adds moisture alcoholic solution while stirring, adds rear cold preservation and leaves standstill.There is a several outstanding difficult problem in this method.The first, in alcohol precipitation process, the loss of effective ingredient parcel is many.Because concentrated solution viscosity is large, density is high, adds alcohol postprecipitation and produces rapidly and measure large, so effective ingredient parcel loss phenomenon is very general aborning.In order to reduce parcel loss, the general method adopting " slow quickening stirs ".But in order to ensure production efficiency, ethanol adds speed can not be too slow.The second, it is large that alcohol precipitation process controls difficulty.Its reason one side and concentrated solution complicated component, alcohol precipitation process parameter is numerous relevant; Also intermittently operated is with current alcohol precipitation process on the other hand relevant.The precipitate with ethanol operation of current discontinuous makes to add system status in alcohol process and is changing always, and on-line monitoring difficulty is larger.
Micromixing technology is the new and effective fluid mixing techniques that eighties of last century the nineties starts to grow up gradually, and micro-mixer can be adopted to realize.Fluid passage in micro-mixer or dispersion yardstick are in micron dimension.The volume transmission quality coefficient of fluid in micro-mixer can reach 10 ~ 1000 times of legacy equipment, and volumetric heat transfer coefficient also can reach 10 ~ 50 times of legacy equipment.It is short that micro-mixer has incorporation time, and safety is high, can continued operation, and the advantages such as easy integrated multiple processes, so be applied to the different field such as biology, chemical industry, medicine and environment.
In sum, alcohol precipitation process has critical role in Chinese patent medicine is produced, but there is the many problems with controlling difficulty of effective ingredients loss.By introducing the technology such as microring array, likely reducing the loss of effective ingredient parcel, realizing adding alcohol continuously, lifting process controllability.
Summary of the invention
The present invention is directed to the loss of current alcohol precipitation process ubiquity effective ingredient parcel and control the large problem of difficulty, a kind of method of continuous alcohol precipitation being provided by introducing micromixing technology, being realized by following steps: concentrated solution and alcoholic solution carry out micro-mixer and realize mixing continuously.
Concentrated solution of the present invention is the liquid of Chinese medicine through a series of course of processing gained such as extraction and concentrations, and the mass fraction wherein shared by solid content is 20%-80%.
Alcoholic solution of the present invention, refers to the mixed liquor of second alcohol and water, and wherein ethanol mass fraction is between 60%-100%.Micro-mixer of the present invention, refers to dispersive film blender or microwell array blender.
Continuous mixing of the present invention, refers to that the alcoholic solution of continuous feed is mixed with the concentrated solution of continuous feed by film or micropore.The flow-rate ratio of alcoholic solution and concentrated solution is 1/1-8/1, and the maximum line velocity of concentrated solution in micro-mixer at least reaches 50cm/s, and mixed feed liquid flows out continuously from micro-mixer outlet.
Dispersive film blender of the present invention, film surface apertures scope is 0.1 micron-500 microns.
Microwell array blender of the present invention, on microwell plate, pore diameter range is 0.1 micron-500 microns.
Operating process of the present invention is simple, can reduce the loss of effective ingredient parcel, whole precipitate with ethanol process also can be made to become continuous steady-state process, reduce and control difficulty, finally contribute to stable Quality of Chinese Traditional Proprietary Medicine.Therefore, be expected to promote in Chinese medicine manufacturing enterprise, as the new method realizing precipitate with ethanol.
Accompanying drawing explanation
Fig. 1 is that continuous alcohol precipitation method provided by the invention realizes schematic diagram.
Detailed description of the invention
Below in conjunction with accompanying drawing, method provided by the present invention is further described.Following examples are for illustration of this method, and its protection domain non-limiting.
embodiment 1
Get Radix Salviae Miltiorrhizae water extracting liquid 6L, wherein total solid content is 80%, is divided into two parts that volume is 3L.Get alcoholic solution 9L, wherein ethanol mass fraction is 60%, is divided into two parts that volume is 4.5L.
Get a Radix Salviae Miltiorrhizae water extracting liquid and a alcoholic solution, adopt method shown in Fig. 1 to carry out precipitate with ethanol.Alcoholic solution and concentrated solution enter dispersive film blender with the flow velocity of 300mL/min and 200mL/min respectively.Dispersive film blender adopts homemade aperture to be the stainless steel membrane of 0.1 micron.Alcoholic solution mixes continuously with concentrated solution after fenestra, concentrated solution in micro-mixer maximum line velocity more than 220cm/s.Collect gained precipitate with ethanol supernatant, and be designated as sample S1.
Get another part of Radix Salviae Miltiorrhizae water extracting liquid and another part of alcoholic solution, adopt the method for mechanical agitation precipitate with ethanol to carry out precipitate with ethanol.Rotating speed of agitator is 200rpm, and it is 150mL/min that ethanol adds speed.Collect gained precipitate with ethanol supernatant after adding ethanol, and be designated as sample S2.
Sample S1 and S2 is carried out liquid-phase chromatographic analysis respectively.Liquid phase analysis condition is as follows: chromatographic column is TigerkinC18 post (200mm × 4.6mm, 5.0 μm); Mobile phase: 0.05% formic acid acetonitrile (B)-0.05% aqueous formic acid (A) gradient elution, elution requirement is 0-10min, 5%-20%B; 10-17min, 20%-25%B; 17-35min, 25%-55%B; After running 35min, balance 5min; Flow velocity: 1.0mL/min; Column temperature: 30 DEG C; Determined wavelength: 0-13min, 280nm; 13-23.5min, 326nm; 23.5-35min, 286nm; Sample size: 20 μ L.
Detect content of danshinolic acid B in gained S1 and reach 0.68mg/mL, in S2, salvianolic acid B is containing being 0.56mg/mL.In continuous alcohol precipitation method gained supernatant, content of danshinolic acid B is higher.
embodiment 2
Get the mixed of Radix Salviae Miltiorrhizae Flos Carthami and decoct water extracting liquid 6L, wherein total solid content is 20%, is divided into two parts that volume is 3L.Get alcoholic solution 12L, wherein ethanol mass fraction is 100%, is divided into two parts that volume is 6L.
Get that a Radix Salviae Miltiorrhizae Flos Carthami is mixed decocts water extracting liquid and a alcoholic solution, adopt method shown in Fig. 1 to carry out precipitate with ethanol.Alcoholic solution and concentrated solution enter dispersive film blender with the flow velocity of 400mL/min and 200mL/min respectively.Dispersive film blender adopts homemade aperture to be the stainless steel membrane of 500 microns.Alcoholic solution mixes continuously with concentrated solution after fenestra, concentrated solution in micro-mixer maximum line velocity more than 50cm/s.Collect gained precipitate with ethanol supernatant, and be designated as sample S3.
Get that another part of Radix Salviae Miltiorrhizae Flos Carthami is mixed decocts water extracting liquid and another part of alcoholic solution, adopt the method for mechanical agitation precipitate with ethanol to carry out precipitate with ethanol.Rotating speed of agitator is 300rpm, and it is 450mL/min that ethanol adds speed.Collect gained precipitate with ethanol supernatant after adding ethanol, and be designated as sample S4.
Sample S3 and S4 is carried out liquid-phase chromatographic analysis respectively.Liquid phase analysis condition is as follows: chromatographic column is ZorbaxEclipsePlusC18 chromatographic column (4.6mm × 100mm, 1.8 μm); Mobile phase A is formic acid-500mmolL
-1ammonium formate-water (0.5:10:90) (often liter contains 5mL formic acid, 50mmol ammonium formate), Mobile phase B is 0.5% formic acid-acetonitrile, elution program, 0-10min, 2%-9%B; 10-13min, 9%-10%B; 13-17min, 10%-17%B; 17-20min, 17%B; 20-37min, 17%-20%B; 37-47min, 20%-25%B; 47-50min, 25%-80%B; Column temperature 30 DEG C; Ultraviolet detection wavelength 0-15.9min, 280nm; 15.9-17.9min, 380nm; 17.9-50min, 280nm; Flow rate of mobile phase is 0.5mLmin
-1; Sample size: 10 μ L.
Detecting content of danshinolic acid B in gained sample S3 is 0.15mg/mL, and S-A Hydroxysafflor yellow A content is 0.024mg/mL; In sample S4, content of danshinolic acid B is 0.14mg/mL, and S-A Hydroxysafflor yellow A content is 0.022mg/mL.In continuous alcohol precipitation method gained supernatant salvianolic acid B and S-A Hydroxysafflor yellow A content all higher.
embodiment 3
Get the mixed water extracting liquid 10L that decocts of the gomi herbs such as Radix Astragali Preparata, Radix Codonopsis, Radix Ophiopogonis, Fructus Schisandrae Chinensis and Fructus Schisandrae Sphenantherae, wherein total solid mass content is 70%, is divided into two parts that volume is 5L.Get alcoholic solution 15L, wherein ethanol mass fraction is 85%, is divided into two parts that volume is 7.5L.
Get the mixed of a gomi herbs and decoct water extracting liquid and a alcoholic solution, adopt method shown in Fig. 1 to carry out precipitate with ethanol.Gomi herbs mixed decocts water extracting liquid and alcoholic solution enters microwell array blender continuously with the flow velocity of 200mL/min and 300mL/min respectively.Microwell plate aperture in microwell array blender is 0.1 micron.Alcoholic solution mixes continuously with concentrated solution after microwell plate, concentrated solution in micro-mixer maximum line velocity more than 80cm/s.Collect gained precipitate with ethanol supernatant, and be designated as sample S5.
Get the mixed of another part of gomi herbs and decoct water extracting liquid and another part of alcoholic solution, adopt the method for mechanical agitation precipitate with ethanol to carry out precipitate with ethanol.Rotating speed of agitator is 250rpm, and it is 300mL/min that ethanol adds speed.Collect gained precipitate with ethanol supernatant after adding ethanol, and be designated as sample S6.
Sample S5 and S6 is carried out liquid-phase chromatographic analysis respectively.The liquid phase analysis condition of schisandrin B and lobetyolin is as follows: chromatographic column is AgilentEclipseC
18post (250mm × 4.6mm, 5.0 μm); Mobile phase: acetonitrile (B)-0.1% glacial acetic acid aqueous solution (A) gradient elution, elution requirement is 0min, 5%B; 5min, 7%B; 10min, 10%B; 20min, 25%B; 50min, 60%B; Flow velocity: 1.0mL/min; Column temperature: 30 DEG C; Determined wavelength: 280nm; Sample size: 10 μ L.The liquid-phase chromatographic analysis condition of astragaloside is: chromatographic column AgilentC
18post (250mm × 4.6mm, 5.0 μm); Mobile phase: methanol-water (80:20); Column temperature: 30 DEG C; Flow velocity: 0.5mL/min; Detector: evaporative light scattering detector; Drift tube temperature 73
oc; Gas flow rate 1.9L/min.Sample size: 10 μ L.
Detecting Astragaloside content in gained sample S5 is 0.62mg/mL, and lobetyolin's content is 0.07mg/mL, and schisandrin B content is 0.34mg/mL.In sample S6, Astragaloside content is 0.57mg/mL, and lobetyolin's content is 0.06mg/mL, and schisandrin B content is 0.33mg/mL.The content of astragaloside in continuous alcohol precipitation method gained supernatant, lobetyolin and schisandrin B is all higher.
embodiment 4
Get Salvia miltiorrhiza Bge water extract to concentrate, add after concentrated mass fraction be 95% alcoholic solution carry out first time precipitate with ethanol.Carry out first time precipitate with ethanol gained supernatant to concentrate the concentrated solution 8L before obtaining second time precipitate with ethanol, wherein total solid mass content is 50%.Get alcoholic solution 64L, wherein ethanol mass fraction is 95%.Concentrated solution before second time precipitate with ethanol is divided into two parts of 4L, alcoholic solution is divided into two parts of 32L.
Get the concentrated solution before a Radix Salviae Miltiorrhizae second time precipitate with ethanol and a alcoholic solution, adopt method shown in Fig. 1 to carry out second time precipitate with ethanol.Concentrated solution and alcoholic solution enter microwell array blender with the flow velocity of 200mL/min and 1600mL/min respectively.Microwell plate aperture in microwell array blender is 500 microns.Alcoholic solution mixes continuously with concentrated solution after microwell plate, concentrated solution in micro-mixer maximum line velocity more than 90cm/s.Collect gained precipitate with ethanol supernatant, and be designated as sample S7.
Get the concentrated solution before another part of Radix Salviae Miltiorrhizae second time precipitate with ethanol and another part of alcoholic solution, adopt the method for mechanical agitation precipitate with ethanol to carry out precipitate with ethanol.Rotating speed of agitator is 200rpm, and it is 500mL/min that ethanol adds speed.Collect gained precipitate with ethanol supernatant after adding ethanol, and be designated as sample S8.
Sample S7 and S8 is carried out liquid-phase chromatographic analysis respectively.Liquid phase analysis condition is as follows: chromatographic column is TigerkinC18 post (200mm × 4.6mm, 5.0 μm); Mobile phase: 0.05% formic acid acetonitrile (B)-0.05% aqueous formic acid (A) gradient elution, elution requirement is 0-10min, 5%-20%B; 10-17min, 20%-25%B; 17-35min, 25%-55%B; After running 35min, balance 5min; Flow velocity: 1.0mL/min; Column temperature: 30 DEG C; Determined wavelength: 0-13min, 280nm; 13-23.5min, 326nm; 23.5-35min, 286nm; Sample size: 20 μ L.
Detecting content of danshinolic acid B in gained S7 is that in 0.11mg/mL, S8, content of danshinolic acid B is 0.10mg/mL.In continuous alcohol precipitation method gained supernatant, content of danshinolic acid B is higher.
embodiment 5
Get Radix Salviae Miltiorrhizae water extracting liquid 8L, wherein total solid content is 60%, is divided into two parts that volume is 4L.Get alcoholic solution 8L, wherein ethanol mass fraction is 90%, is divided into two parts that volume is 4L.
Get a Radix Salviae Miltiorrhizae water extracting liquid and a alcoholic solution, adopt method shown in Fig. 1 to carry out precipitate with ethanol.Alcoholic solution and concentrated solution enter dispersive film blender with the flow velocity of 200mL/min and 200mL/min respectively.Dispersive film blender adopts homemade aperture to be the stainless steel membrane of 1 micron.Alcoholic solution mixes continuously with concentrated solution after fenestra, concentrated solution in micro-mixer maximum line velocity more than 150cm/s.Collect gained precipitate with ethanol supernatant, and be designated as sample S9.
Get another part of Radix Salviae Miltiorrhizae water extracting liquid and another part of alcoholic solution, adopt the method for mechanical agitation precipitate with ethanol to carry out precipitate with ethanol.Rotating speed of agitator is 400rpm, and it is 350mL/min that ethanol adds speed.Collect gained precipitate with ethanol supernatant after adding ethanol, and be designated as sample S10.
Sample S9 and S10 is carried out liquid-phase chromatographic analysis respectively.Liquid phase analysis condition is as follows: chromatographic column is TigerkinC18 post (200mm × 4.6mm, 5.0 μm); Mobile phase: 0.05% formic acid acetonitrile (B)-0.05% aqueous formic acid (A) gradient elution, elution requirement is 0-10min, 5%-20%B; 10-17min, 20%-25%B; 17-35min, 25%-55%B; After running 35min, balance 5min; Flow velocity: 1.0mL/min; Column temperature: 30 DEG C; Determined wavelength: 0-13min, 280nm; 13-23.5min, 326nm; 23.5-35min, 286nm; Sample size: 20 μ L.
Detect content of danshinolic acid B in gained S9 and reach 0.56mg/mL, in S10, content of danshinolic acid B is 0.50mg/mL.In continuous alcohol precipitation method gained supernatant, content of danshinolic acid B is higher.
embodiment 6
Get Radix Salviae Miltiorrhizae water extracting liquid 8L, wherein total solid content is 40%, is divided into two parts that volume is 4L.Get alcoholic solution 56L, wherein ethanol mass fraction is 70%, is divided into two parts that volume is 28L.
Get a Radix Salviae Miltiorrhizae water extracting liquid and a alcoholic solution, adopt method shown in Fig. 1 to carry out precipitate with ethanol.Alcoholic solution and concentrated solution enter dispersive film blender with the flow velocity of 200mL/min and 1400mL/min respectively.Dispersive film blender adopts homemade aperture to be the stainless steel membrane of 20 microns.Alcoholic solution mixes continuously with concentrated solution after fenestra, concentrated solution in micro-mixer maximum line velocity more than 120cm/s.Collect gained precipitate with ethanol supernatant, and be designated as sample S11.
Get another part of Radix Salviae Miltiorrhizae water extracting liquid and another part of alcoholic solution, adopt the method for mechanical agitation precipitate with ethanol to carry out precipitate with ethanol.Rotating speed of agitator is 300rpm, and it is 200mL/min that ethanol adds speed.Collect gained precipitate with ethanol supernatant after adding ethanol, and be designated as sample S12.
Sample S11 and S12 is carried out liquid-phase chromatographic analysis respectively.Liquid phase analysis condition is as follows: chromatographic column is TigerkinC18 post (200mm × 4.6mm, 5.0 μm); Mobile phase: 0.05% formic acid acetonitrile (B)-0.05% aqueous formic acid (A) gradient elution, elution requirement is 0-10min, 5%-20%B; 10-17min, 20%-25%B; 17-35min, 25%-55%B; After running 35min, balance 5min; Flow velocity: 1.0mL/min; Column temperature: 30 DEG C; Determined wavelength: 0-13min, 280nm; 13-23.5min, 326nm; 23.5-35min, 286nm; Sample size: 20 μ L.
Detect content of danshinolic acid B in gained S11 and reach 0.10mg/mL, in S12, content of danshinolic acid B is 0.09mg/mL.In continuous alcohol precipitation method gained supernatant, content of danshinolic acid B is higher.
embodiment 7
Get Radix Salviae Miltiorrhizae water extracting liquid 8L, wherein total solid content is 50%, is divided into two parts that volume is 4L.Get alcoholic solution 48L, wherein ethanol mass fraction is 65%, is divided into two parts that volume is 24L.
Get a Radix Salviae Miltiorrhizae water extracting liquid and a alcoholic solution, adopt method shown in Fig. 1 to carry out precipitate with ethanol.Alcoholic solution and concentrated solution enter microwell array blender with the flow velocity of 200mL/min and 1200mL/min respectively.Microwell plate aperture in microwell array blender is 200 microns.Alcoholic solution mixes continuously with concentrated solution after microwell plate, concentrated solution in micro-mixer maximum line velocity more than 200cm/s.Collect gained precipitate with ethanol supernatant, and be designated as sample S13.
Get another part of Radix Salviae Miltiorrhizae water extracting liquid and another part of alcoholic solution, adopt the method for mechanical agitation precipitate with ethanol to carry out precipitate with ethanol.Rotating speed of agitator is 200rpm, and it is 350mL/min that ethanol adds speed.Collect gained precipitate with ethanol supernatant after adding ethanol, and be designated as sample S14.
Sample S13 and S14 is carried out liquid-phase chromatographic analysis respectively.Liquid phase analysis condition is as follows: chromatographic column is TigerkinC18 post (200mm × 4.6mm, 5.0 μm); Mobile phase: 0.05% formic acid acetonitrile (B)-0.05% aqueous formic acid (A) gradient elution, elution requirement is 0-10min, 5%-20%B; 10-17min, 20%-25%B; 17-35min, 25%-55%B; After running 35min, balance 5min; Flow velocity: 1.0mL/min; Column temperature: 30 DEG C; Determined wavelength: 0-13min, 280nm; 13-23.5min, 326nm; 23.5-35min, 286nm; Sample size: 20 μ L.
Detect content of danshinolic acid B in gained S13 and reach 0.14mg/mL, in S14, content of danshinolic acid B is 0.12mg/mL.In continuous alcohol precipitation method gained supernatant, content of danshinolic acid B is higher.
embodiment 8
Get Radix Salviae Miltiorrhizae water extracting liquid 8L, wherein total solid content is 30%, is divided into two parts that volume is 4L.Get alcoholic solution 40L, wherein ethanol mass fraction is 75%, is divided into two parts that volume is 20L.
Get a Radix Salviae Miltiorrhizae water extracting liquid and a alcoholic solution, adopt method shown in Fig. 1 to carry out precipitate with ethanol.Alcoholic solution and concentrated solution enter microwell array blender with the flow velocity of 200mL/min and 1000mL/min respectively.Microwell plate aperture in microwell array blender is 30 microns.Alcoholic solution mixes continuously with concentrated solution after microwell plate, concentrated solution in micro-mixer maximum line velocity more than 180cm/s.Collect gained precipitate with ethanol supernatant, and be designated as sample S15.
Get another part of Radix Salviae Miltiorrhizae water extracting liquid and another part of alcoholic solution, adopt the method for mechanical agitation precipitate with ethanol to carry out precipitate with ethanol.Rotating speed of agitator is 300rpm, and it is 250mL/min that ethanol adds speed.Collect gained precipitate with ethanol supernatant after adding ethanol, and be designated as sample S16.
Sample S15 and S16 is carried out liquid-phase chromatographic analysis respectively.Liquid phase analysis condition is as follows: chromatographic column is TigerkinC18 post (200mm × 4.6mm, 5.0 μm); Mobile phase: 0.05% formic acid acetonitrile (B)-0.05% aqueous formic acid (A) gradient elution, elution requirement is 0-10min, 5%-20%B; 10-17min, 20%-25%B; 17-35min, 25%-55%B; After running 35min, balance 5min; Flow velocity: 1.0mL/min; Column temperature: 30 DEG C; Determined wavelength: 0-13min, 280nm; 13-23.5min, 326nm; 23.5-35min, 286nm; Sample size: 20 μ L.
Detect content of danshinolic acid B in gained S15 and reach 0.12mg/mL, in S16, content of danshinolic acid B is 0.11mg/mL.In continuous alcohol precipitation method gained supernatant, content of danshinolic acid B is higher.
embodiment 9
Get Radix Salviae Miltiorrhizae water extracting liquid 8L, wherein total solid content is 65%, is divided into two parts that volume is 4L.Get alcoholic solution 24L, wherein ethanol mass fraction is 75%, is divided into two parts that volume is 12L.
Get a Radix Salviae Miltiorrhizae water extracting liquid and a alcoholic solution, adopt method shown in Fig. 1 to carry out precipitate with ethanol.Alcoholic solution and concentrated solution enter microwell array blender with the flow velocity of 200mL/min and 600mL/min respectively.Microwell plate aperture in microwell array blender is 2 microns.Alcoholic solution mixes continuously with concentrated solution after microwell plate, concentrated solution in micro-mixer maximum line velocity more than 70cm/s.Collect gained precipitate with ethanol supernatant, and be designated as sample S17.
Get another part of Radix Salviae Miltiorrhizae water extracting liquid and another part of alcoholic solution, adopt the method for mechanical agitation precipitate with ethanol to carry out precipitate with ethanol.Rotating speed of agitator is 200rpm, and it is 250mL/min that ethanol adds speed.Collect gained precipitate with ethanol supernatant after adding ethanol, and be designated as sample S18.
Sample S17 and S18 is carried out liquid-phase chromatographic analysis respectively.Liquid phase analysis condition is as follows: chromatographic column is TigerkinC18 post (200mm × 4.6mm, 5.0 μm); Mobile phase: 0.05% formic acid acetonitrile (B)-0.05% aqueous formic acid (A) gradient elution, elution requirement is 0-10min, 5%-20%B; 10-17min, 20%-25%B; 17-35min, 25%-55%B; After running 35min, balance 5min; Flow velocity: 1.0mL/min; Column temperature: 30 DEG C; Determined wavelength: 0-13min, 280nm; 13-23.5min, 326nm; 23.5-35min, 286nm; Sample size: 20 μ L.
Detect content of danshinolic acid B in gained S17 and reach 0.33mg/mL, in S18, content of danshinolic acid B is 0.31mg/mL.In continuous alcohol precipitation method gained supernatant, content of danshinolic acid B is higher.
embodiment 10
Get Radix Salviae Miltiorrhizae water extracting liquid 8L, wherein total solid content is 55%, is divided into two parts that volume is 4L.Get alcoholic solution 32L, wherein ethanol mass fraction is 80%, is divided into two parts that volume is 16L.
Get a Radix Salviae Miltiorrhizae water extracting liquid and a alcoholic solution, adopt method shown in Fig. 1 to carry out precipitate with ethanol.Alcoholic solution and concentrated solution enter dispersive film blender with the flow velocity of 200mL/min and 800mL/min respectively.Dispersive film blender adopts homemade aperture to be the stainless steel membrane of 100 microns.Alcoholic solution mixes continuously with concentrated solution after fenestra, concentrated solution in micro-mixer maximum line velocity more than 130cm/s.Collect gained precipitate with ethanol supernatant, and be designated as sample S19.
Get another part of Radix Salviae Miltiorrhizae water extracting liquid and another part of alcoholic solution, adopt the method for mechanical agitation precipitate with ethanol to carry out precipitate with ethanol.Rotating speed of agitator is 260rpm, and it is 280mL/min that ethanol adds speed.Collect gained precipitate with ethanol supernatant after adding ethanol, and be designated as sample S20.
Sample S19 and S20 is carried out liquid-phase chromatographic analysis respectively.Liquid phase analysis condition is as follows: chromatographic column is TigerkinC18 post (200mm × 4.6mm, 5.0 μm); Mobile phase: 0.05% formic acid acetonitrile (B)-0.05% aqueous formic acid (A) gradient elution, elution requirement is 0-10min, 5%-20%B; 10-17min, 20%-25%B; 17-35min, 25%-55%B; After running 35min, balance 5min; Flow velocity: 1.0mL/min; Column temperature: 30 DEG C; Determined wavelength: 0-13min, 280nm; 13-23.5min, 326nm; 23.5-35min, 286nm; Sample size: 20 μ L.
Detect content of danshinolic acid B in gained S19 and reach 0.22mg/mL, in S20, content of danshinolic acid B is 0.19mg/mL.In continuous alcohol precipitation method gained supernatant, content of danshinolic acid B is higher.
Claims (7)
1. a method for continuous alcohol precipitation, is characterized in that, is realized by following steps: concentrated solution and alcoholic solution adopt micro-mixer to realize mixing continuously.
2. the method for a kind of continuous alcohol precipitation according to claim 1, is characterized in that, described concentrated solution is the liquid of Chinese medicine through a series of course of processing gained such as extraction and concentrations, and the mass fraction wherein shared by solid content is 20%-80%.
3. the method for a kind of continuous alcohol precipitation according to claim 1, is characterized in that, described alcoholic solution refers to the mixed liquor of second alcohol and water, and wherein ethanol mass fraction is between 60%-100%.
4. the method for a kind of continuous alcohol precipitation according to claim 1, is characterized in that, described micro-mixer, refers to dispersive film blender or microwell array blender.
5. the method for a kind of continuous alcohol precipitation according to claim 1, it is characterized in that, described continuous mixing, refer to that the alcoholic solution of continuous feed is mixed with the concentrated solution of continuous feed by film or micropore, the flow-rate ratio of alcoholic solution and concentrated solution is 1/1-8/1, the maximum line velocity of concentrated solution in micro-mixer reaches more than 50cm/s, and mixed feed liquid flows out continuously from micro-mixer outlet.
6. the method for a kind of continuous alcohol precipitation according to claim 4, is characterized in that, described dispersive film blender, and film surface apertures scope is 0.1 micron-500 microns.
7. the method for a kind of continuous alcohol precipitation according to claim 4, is characterized in that, described microwell array blender, and on microwell plate, pore diameter range is 0.1 micron-500 microns.
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| CN112129863A (en) * | 2020-09-04 | 2020-12-25 | 浙江大学 | Method for quantitatively evaluating mixing condition in alcohol precipitation process |
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| CN104042520A (en) * | 2014-06-30 | 2014-09-17 | 广西润深农林科技有限公司 | Water extraction and alcohol precipitation method of sarcandra glabra liquid extract |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112129863A (en) * | 2020-09-04 | 2020-12-25 | 浙江大学 | Method for quantitatively evaluating mixing condition in alcohol precipitation process |
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