CN103254189B - Application berberine hydrochloride molecular imprinting column is separated the method for berberine hydrochloride - Google Patents
Application berberine hydrochloride molecular imprinting column is separated the method for berberine hydrochloride Download PDFInfo
- Publication number
- CN103254189B CN103254189B CN201310142511.2A CN201310142511A CN103254189B CN 103254189 B CN103254189 B CN 103254189B CN 201310142511 A CN201310142511 A CN 201310142511A CN 103254189 B CN103254189 B CN 103254189B
- Authority
- CN
- China
- Prior art keywords
- berberine hydrochloride
- column
- molecular imprinting
- berberine
- imprinted polymer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Nitrogen Condensed Heterocyclic Rings (AREA)
Abstract
The present invention discloses a kind of method applying berberine hydrochloride molecular imprinting column separation berberine hydrochloride, carries out in accordance with the following steps: (1) prepares sample solution: get appropriate amount of sample, with organic solvent dissolution, is mixed with the hydrochloric Berberine 1.0 × 10 of every 1L
-5-3.0 × 10
-4the sample solution of mol; Described sample is wherein a kind of mixture of berberine hydrochloride and ligustrazine hydrochloride, tetrahydropalmatine; (2) setup parameter: by berberine hydrochloride molecular imprinting column access liquid chromatograph, the flow rate of mobile phase arranging liquid chromatograph is 0.1-1mL/min, determined wavelength 345nm, column oven 30 ± 10 DEG C; (3) be separated: start sampling valve and sample solution is brought in berberine hydrochloride molecular imprinting column by moving phase, realize the separation of berberine hydrochloride.The present invention is highly sensitive, simple to operate, can not cause secondary pollution to medicine and healthcare products.
Description
Technical field
The invention belongs to high performance liquid chromatography field, particularly a kind of method applying berberine hydrochloride molecular imprinting column separation berberine hydrochloride.
Background technology
Berberine hydrochloride, chemical structural formula:
it is the hydrochloride of main component Berberine in the natural drug coptis, not only have effect of heat-clearing and damp-drying drug, eliminating fire and detoxication, the pharmacologically active such as antibacterial, hypoglycemic, antitumor and anti-arrhythmia, also has certain curative effect to pulmonary tuberculosis, scarlet fever, acute tonsillitis and respiratory tract infection in addition.
Molecular imprinting is as template molecule using the material of separated detection, be fixed in the polymkeric substance of high-crosslinking-degree, after removing template molecule, leave the space structure with the complementation of template molecule steric configuration, template molecule is had to the specific recognition ability of height.At present, molecularly imprinted polymer being separated of enantiomorph and isomer, pharmaceutical analysis, sensor, analogue enztme, field such as Solid-Phase Extraction and catalyzer in chromatogram is widely used.
Liquid-phase chromatographic analysis refers to that moving phase is the chromatographic technique of liquid, it is one the most ancient in chromatography, but by granularity and the post pressure of improvement filler, the basis of the liquid column chromatography of classics introduces the plate theory of gas-chromatography, have employed high pressure pump technically, high-effective fixed phase and highly sensitive detector, achieve that analysis speed is fast, separation efficiency is high and operation automation, this chromatographic technique be called as high performance liquid chromatography (
high performance liquid chromatography, be called for short HPLC).HPLC has following characteristics: speed is fast-usually analyze a sample at 15 ~ 30min, some sample even can complete in 5min from; Resolving power is high-compartment analysis can be carried out to the very little material of otherness to such as chiral material; Highly sensitive-UV-detector can reach 0.01ng, and fluorescence and electrochemical detector can reach 0.1pg; Pillar can Reusability, with the separable different compound of a root chromatogram column; Sample size is few, easily reclaims; Sample is not destroyed after chromatographic column, can collect one-component or do and prepare.
At present, about the report of berberine hydrochloride high performance liquid chromatography partition method, we find the following document:
1. application number: 200710017585.8, denomination of invention: a kind of quality determining method for the treatment of person in middle and old age's eye disease Chinese medicine preparation, wherein mention berberine hydrochloride content, be take octadecylsilane chemically bonded silica as weighting agent, the acetonitrile-0.05mol/L potassium dihydrogen phosphate with 43: 57 is for moving phase; Determined wavelength is 265nm; Number of theoretical plate calculates should be not less than 2000 by berberine hydrochloride peak; Accurate absorption reference substance solution and each 10 μ L of need testing solution respectively, injection liquid chromatography, measures.
2. Lee builds merit, Zhang Liang, the content of the refined precious .HPLC method Simultaneously test Berberine Hydrochloride in Sanhuang Tablet of king and yellow Cen glycosides. Chinese pharmacists .2005,8(6): 479-480; Adopt high performance liquid chromatography, use C
18chromatographic column (150mm × 4.6mm, 5 μm), with methyl alcohol-0.05molL
-1potassium dihydrogen phosphate-glacial acetic acid (40: 60: 1) is moving phase, and flow velocity is 1.0mlmin
-1, determined wavelength 333nm.
Be separated berberine hydrochloride about application berberine hydrochloride molecular imprinting column, up to the present have no report.
Summary of the invention
The object of the invention is to solve above-mentioned Problems existing, provide a kind of and apply the method that berberine hydrochloride molecular imprinting column is separated berberine hydrochloride, the method is highly sensitive, simple to operate, can not cause secondary pollution to medicine and healthcare products.
For achieving the above object, the invention provides following technical scheme:
Apply the method that berberine hydrochloride molecular imprinting column is separated berberine hydrochloride, carry out in accordance with the following steps:
(1) prepare sample solution: get appropriate amount of sample, with organic solvent dissolution, be mixed with the hydrochloric Berberine 1.0 × 10 of every 1L
-5-3.0 × 10
-4the sample solution of mol; Described sample is wherein a kind of mixture of berberine hydrochloride and ligustrazine hydrochloride or tetrahydropalmatine;
(2) setup parameter: by berberine hydrochloride molecular imprinting column access liquid chromatograph, the flow rate of mobile phase arranging liquid chromatograph is 0.1-1mL/min, determined wavelength 345nm, column oven 30 ± 10 DEG C;
(3) be separated: start sampling valve and sample solution is brought in berberine hydrochloride molecular imprinting column by moving phase, realize the separation of berberine hydrochloride.
As further instruction, the above berberine hydrochloride molecular imprinting column, its filling material is berberine hydrochloride molecularly imprinted polymer; Described berberine hydrochloride molecularly imprinted polymer is spherical porous material, and its particle diameter is 50 ~ 180 μm, and mean pore size is 2 ~ 100nm.
As further instruction, the above berberine hydrochloride molecular imprinting column, diameter and height of column ratio is 1: 1-300, and in post, caliber is at 1-100mm, post height 10-300mm.
As further instruction, the above berberine hydrochloride molecular imprinting column, is provided with internal thread outside column jecket two ends and is connected with pipeline, establishes sieve plate to prevent solid packing from leaking outside inside two ends, but liquid can be made to pass through.
As further instruction, the above organic solvent is methyl alcohol.
As further instruction, the above moving phase is acetate-methanol mixing solutions, and the volume ratio of described acetic acid and methyl alcohol is 0.01-1: 100.
Berberine hydrochloride molecularly imprinted polymer used in the present invention, be prepare by the following method out:
(1) in solvent, add template molecule, function monomer, linking agent, solvent, initiator and pore-creating agent, often add a kind of chemical reagent ultrasonic wave dissolution 5 minutes, dissolve completely and be oil phase; In there-necked flask, add deionized water, dispersion agent, after dispersion agent dissolves completely, be aqueous phase; Under agitation oil phase is slowly added in aqueous phase, prepare molecularly imprinted polymer by suspension polymerization.
(2) described in step (1), template molecule is berberine hydrochloride, function monomer is methacrylic acid, linking agent is that multiple crosslinking agent is made up of maleated rosin vinylformic acid glycol ester (cross-linking agents Ⅰ) and Ethylene glycol dimethacrylate (linking agent II), solvent is ethyl acetate, initiator is Diisopropyl azodicarboxylate, pore-creating agent is peanut oil, and dispersion agent is sodium lauryl sulphate and polyvinyl alcohol, described template molecule, function monomer, cross-linking agents Ⅰ, linking agent II, Diisopropyl azodicarboxylate, peanut oil, the mass ratio of ethyl acetate is (0.034 ~ 3.4) ︰ (0.25 ~ 25) ︰ 12 ︰ (2.4 ~ 36) ︰ (0.1 ~ 0.7) ︰ (3 ~ 20) ︰ (20 ~ 100), deionized water, sodium lauryl sulphate, the mass ratio of polyvinyl alcohol is 100 ︰ (0.022 ~ 0.11) ︰ (0.011 ~ 0.088), the mass ratio of oil phase and aqueous phase is 1 ︰ (2 ~ 9), stirring velocity is 200 ~ 600r/min, adopt temperature programming 55 ~ 80 DEG C reaction 20 ~ 90min, 80 ~ 100 DEG C of reaction 60 ~ 180min, obtain berberine hydrochloride molecularly imprinted polymer.
(3) molecularly imprinted polymer of step (2) gained, through acetate-methanol solution (volume ratio 3:1) wash-out after screening, until elutriant no longer contains berberine hydrochloride through ultraviolet detection, again with acetic acid, methyl alcohol in steam distillation removing polymkeric substance, obtain molecularly imprinted polymer.The preparation of non-molecularly imprinted polymer is not except adding except template molecule, and other conditions are identical.
The berberine hydrochloride molecularly imprinted polymer that the present invention prepares, turgidity is little, specific surface area is large, can be used for the effective constituent in separation and Extraction plant, and can use in organic solvent, can not because of expansion the network structure of saboteur's imprinted polymer, cause recognition capability to be lost.With the berberine hydrochloride molecular imprinting column that berberine hydrochloride molecularly imprinted polymer is prepared for filler, because being rich in pore structure not of uniform size, have that permeability is good, back pressure is low, the advantage such as efficient and high-throughput, under higher flow velocity and pressure, do not occur pressing the phenomenon of collapsing, can use under high flow rate.Further, good stability, reusable, after long-time use, the filler in chromatographic column does not still destroy, dissolves.
Compared with prior art, beneficial effect of the present invention is: (1) chromatographic column used in the present invention, and binding molecule engram technology, has specific recognition ability to target molecule berberine hydrochloride, can predict elution order; (2) rosinyl polymkeric substance is with the derivative of product of natural product rosin for raw material, and cheap and easy to get, physical strength is high, safety non-toxic; (3) HPLC is highly sensitive, simple to operate.
Accompanying drawing explanation
Fig. 1 is the analysis chart of the embodiment of the present invention 4 pairs of berberine hydrochlorides (b) and ligustrazine hydrochloride (a) mixing solutions;
Fig. 2 is the analysis chart of the embodiment of the present invention 5 pairs of berberine hydrochlorides (b) and ligustrazine hydrochloride (a) mixing solutions;
Fig. 3 is the analysis chart of the embodiment of the present invention 6 pairs of berberine hydrochlorides (b) and tetrahydropalmatine (c) mixing solutions;
Fig. 4 is flow velocity in the present invention-pressure curve table;
Fig. 5 is berberine hydrochloride molecular imprinting column structural representation of the present invention.
Reference numeral:
1-internal thread, 2-sieve plate, 3-column jecket, 4-column cap.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to the scope that embodiment represents.
embodiment 1:
(1) 0.034g berberine hydrochloride and 0.25g methacrylic acid are added in 50mL beaker successively, after template molecule mixes with berberine hydrochloride, add 12g maleated rosin vinylformic acid glycol ester and 2.4g Ethylene glycol dimethacrylate, 3g peanut oil, 20g ethyl acetate, 0.01g Diisopropyl azodicarboxylate more successively, ultrasonic wave dissolution, forms uniform oil phase.
76g deionized water, 0.0836g sodium lauryl sulphate, 0.0669g polyvinyl alcohol adjustment stirring velocity is added successively to 600r/min in 1000mL there-necked flask, heating impels sodium lauryl sulphate, polyvinyl alcohol dissolves completely, after aqueous phase temperature rises to 55 DEG C, oil phase is slowly added in there-necked flask, pre-dispersed 10min makes oil phase in aqueous phase, form uniform small droplets, is slowly heated to free radical polymerization 1.5h under 85 DEG C of conditions.
(2) reaction terminates, and sieved by product, the sieve aperture of sieve is 60-120 order, preferably 100 orders.Through acetate-methanol solution (volume ratio 3:1) wash-out after screening, until elutriant no longer contains berberine hydrochloride through ultraviolet detection, then with acetic acid, methyl alcohol in steam distillation removing polymkeric substance, obtain molecularly imprinted polymer.The preparation of non-molecularly imprinted polymer is not except adding except template molecule, and other conditions are identical.
embodiment 2
(1) by 3.4g berberine hydrochloride and 25g methacrylic acid according in 500mL beaker, after template molecule mixes with berberine hydrochloride, add 12g maleated rosin vinylformic acid glycol ester and 36g Ethylene glycol dimethacrylate, 20g peanut oil, 100g ethyl acetate, 0.7g Diisopropyl azodicarboxylate more successively, ultrasonic wave dissolution, forms uniform oil phase.
1770g deionized water, 0.3894g sodium lauryl sulphate, 0.1947g polyvinyl alcohol adjustment stirring velocity is added successively to 200r/min in 3000mL there-necked flask, heating impels sodium lauryl sulphate, polyvinyl alcohol dissolves completely, after aqueous phase temperature rises to 80 DEG C, oil phase is slowly added in there-necked flask, pre-dispersed 10min makes oil phase in aqueous phase, form uniform small droplets, is slowly heated to free radical polymerization 4h under 95 DEG C of conditions.
(2) reaction terminates, and sieved by product, the sieve aperture of sieve is 60-120 order, preferably 100 orders.Through acetate-methanol solution (volume ratio 3:1) wash-out after screening, until elutriant no longer contains berberine hydrochloride through ultraviolet detection, then with acetic acid methanol in steam distillation removing polymkeric substance, obtain molecularly imprinted polymer.The preparation of non-molecularly imprinted polymer is not except adding except template molecule, and other conditions are identical.
embodiment 3
(1) 0.7442g berberine hydrochloride and 5g methacrylic acid are added in 150mL beaker, after template molecule mixes with berberine hydrochloride, add 30g maleated rosin vinylformic acid glycol ester and 10g Ethylene glycol dimethacrylate, 20g peanut oil, 120g ethyl acetate, 0.7875g Diisopropyl azodicarboxylate more successively, ultrasonic wave dissolution, forms uniform oil phase.
600g deionized water, 0.5325g sodium lauryl sulphate, 0.2663g polyvinyl alcohol adjustment stirring velocity is added successively to 500r/min in 2000mL there-necked flask, heating impels sodium lauryl sulphate, polyvinyl alcohol dissolves completely, after aqueous phase temperature rises to 65 DEG C, oil phase is slowly added in there-necked flask, pre-dispersed 10min makes oil phase in aqueous phase, form uniform small droplets, is slowly heated to free radical polymerization 3h under 85 DEG C of conditions.
(2) reaction terminates, and sieved by product, the sieve aperture of sieve is 60-120 order, preferably 100 orders.Through acetate-methanol solution (volume ratio 3:1) wash-out after screening, until elutriant no longer contains berberine hydrochloride through ultraviolet detection, then with acetic acid methanol in steam distillation removing polymkeric substance, obtain molecularly imprinted polymer.The preparation of non-molecularly imprinted polymer is not except adding except template molecule, and other conditions are identical.
embodiment 4
Embodiment 1 berberine hydrochloride molecularly imprinted polymer is loaded in chromatographic column, obtains berberine hydrochloride molecular imprinting column.By gained molecularly imprinted polymer chromatographic column volume ratio be 10% acetate-methanol composition mixing solutions rinse chromatographic column to baseline balance get final product sample introduction.
Apply the method that berberine hydrochloride molecular imprinting column is separated berberine hydrochloride, carry out in accordance with the following steps:
(1) prepare sample solution: get appropriate hydrochloric acid Berberine, ligustrazine hydrochloride, with dissolve with methanol, be mixed with the hydrochloric Berberine 2.5 × 10 of every 1L
-5the berberine hydrochloride of mol and ligustrazine hydrochloride mixing solutions; Meanwhile, prepare concentration and be 2.5 × 10
-5the berberine hydrochloride methanol solution of mol/L, ligustrazine hydrochloride methanol solution; Sample introduction respectively;
(2) setup parameter: by berberine hydrochloride molecular imprinting column access liquid chromatograph, the flow rate of mobile phase arranging liquid chromatograph is 1mL/min, determined wavelength 345nm and 295nm, column oven 20 DEG C;
(3) be separated: start sampling valve make volume ratio be 0.01: 100 acetate-methanol mixing solutions sample solution is brought in berberine hydrochloride molecular imprinting column, sample size is 20 μ L, realize the separation of berberine hydrochloride, acquired results as shown in Figure 1, ligustrazine hydrochloride peak is there is when retention time 8.62min, occur berberine hydrochloride peak when retention time is 39.81min, separation factor is 18.17.
In the present embodiment, berberine hydrochloride molecular imprinting column, diameter and height of column ratio is 1: 1, and its filling material is berberine hydrochloride molecularly imprinted polymer, and berberine hydrochloride molecularly imprinted polymer is spherical porous material, its particle diameter is 50 ~ 150 μm, and mean pore size is 2 ~ 80nm.Berberine hydrochloride molecular imprinting column, has internal thread 1 to be connected with pipeline outside column jecket 3 two ends, has sieve plate 2 inside two ends.
embodiment 5
Embodiment 3 berberine hydrochloride molecularly imprinted polymer is loaded in chromatographic column, obtains berberine hydrochloride molecular imprinting column.By gained molecularly imprinted polymer chromatographic column volume ratio be 5% acetate-methanol composition mixing solutions rinse chromatographic column to baseline balance get final product sample introduction.
Apply the method that berberine hydrochloride molecular imprinting column is separated berberine hydrochloride, carry out in accordance with the following steps:
(1) prepare sample solution: get appropriate hydrochloric acid Berberine, ligustrazine hydrochloride, with dissolve with methanol, be mixed with the hydrochloric Berberine 3.0 × 10 of every 1L
-4the berberine hydrochloride of mol and ligustrazine hydrochloride mixing solutions; Meanwhile, prepare concentration and be 3.0 × 10
-4the berberine hydrochloride methanol solution of mol/L, ligustrazine hydrochloride methanol solution; Sample introduction respectively;
(2) setup parameter: by berberine hydrochloride molecular imprinting column access liquid chromatograph, the flow rate of mobile phase arranging liquid chromatograph is 0.5mL/min, determined wavelength 345nm and 280nm, column oven 40 DEG C;
(3) be separated: start sampling valve make volume ratio be 0.5: 100 acetate-methanol mixing solutions sample solution is brought in berberine hydrochloride molecular imprinting column, sample size is 20 μ L, realize the separation of berberine hydrochloride, acquired results as shown in Figure 2, ligustrazine hydrochloride peak is there is when retention time 9.10min, occur berberine hydrochloride peak when retention time is 20.95min, separation factor is 8.56.
In the present embodiment, berberine hydrochloride molecular imprinting column, diameter and height of column ratio is 1: 54, its filling material is berberine hydrochloride molecularly imprinted polymer, berberine hydrochloride molecularly imprinted polymer is spherical porous material, its particle diameter 80 ~ 150 μm, and mean pore size is 20 ~ 60nm.Berberine hydrochloride molecular imprinting column, has internal thread 1 to be connected with pipeline outside column jecket 3 two ends, has sieve plate 2 inside two ends.
embodiment 6
Embodiment 2 berberine hydrochloride molecularly imprinted polymer is loaded in chromatographic column, obtains berberine hydrochloride molecular imprinting column.By gained molecularly imprinted polymer chromatographic column volume ratio be 5% acetate-methanol composition mixing solutions rinse chromatographic column to baseline balance get final product sample introduction.
Apply the method that berberine hydrochloride molecular imprinting column is separated berberine hydrochloride, carry out in accordance with the following steps:
(1) prepare sample solution: get appropriate hydrochloric acid Berberine, tetrahydropalmatine, with dissolve with methanol, be mixed with the hydrochloric Berberine 1.0 × 10 of every 1L
-5the berberine hydrochloride of mol and tetrahydropalmatine mixing solutions; Meanwhile, prepare concentration and be 1.0 × 10
-5the berberine hydrochloride methanol solution of mol/L, tetrahydropalmatine methanol solution; Sample introduction respectively;
(2) setup parameter: by berberine hydrochloride molecular imprinting column access liquid chromatograph, the flow rate of mobile phase arranging liquid chromatograph is 0.1mL/min, determined wavelength 345nm and 280nm, column oven 30 DEG C;
(3) be separated: start sampling valve make volume ratio be 1: 100 acetate-methanol mixing solutions sample solution is brought in berberine hydrochloride molecular imprinting column, sample size is 20 μ L, realize the separation of berberine hydrochloride, acquired results as shown in Figure 3, tetrahydropalmatine peak is there is when retention time 34.70min, occur berberine hydrochloride peak when retention time is 78.67min, separation factor is 4.44.
In the present embodiment, berberine hydrochloride molecular imprinting column, diameter and height of column ratio is 1: 300, its filling material is berberine hydrochloride molecularly imprinted polymer, berberine hydrochloride molecularly imprinted polymer is spherical porous material, its particle diameter 100 ~ 180 μm, and mean pore size is 40 ~ 100nm.Berberine hydrochloride molecular imprinting column, has internal thread 1 to be connected with pipeline outside column jecket 3 two ends, has sieve plate 2 inside two ends.
Claims (2)
1. apply the method that berberine hydrochloride molecular imprinting column is separated berberine hydrochloride, it is characterized in that, carry out in accordance with the following steps:
(1) prepare sample solution: get appropriate amount of sample, with organic solvent dissolution, be mixed with the hydrochloric Berberine 1.0 × 10 of every 1L
-5-3.0 × 10
-4the sample solution of mol; Described sample is wherein a kind of mixture of berberine hydrochloride and ligustrazine hydrochloride or tetrahydropalmatine; Described organic solvent is methyl alcohol;
(2) setup parameter: by berberine hydrochloride molecular imprinting column access liquid chromatograph, the flow rate of mobile phase arranging liquid chromatograph is 0.1-1mL/min, determined wavelength 345nm, column oven 30 ± 10 DEG C; Described moving phase is acetate-methanol mixing solutions, and the volume ratio of described acetic acid and methyl alcohol is 0.01-1: 100;
(3) be separated: start sampling valve and sample solution is brought in berberine hydrochloride molecular imprinting column by moving phase, realize the separation of berberine hydrochloride;
Described berberine hydrochloride molecular imprinting column, its filling material is berberine hydrochloride molecularly imprinted polymer, and described berberine hydrochloride molecularly imprinted polymer is spherical porous material, and its particle diameter is 50-180 μm, and mean pore size is 2-100nm;
Described berberine hydrochloride molecular imprinting column, is provided with internal thread (1) and is connected with pipeline, be provided with sieve plate (2) inside two ends outside column jecket (3) two ends;
Described berberine hydrochloride molecularly imprinted polymer, be prepare by the following method out:
(1) in solvent, add template molecule, function monomer, linking agent, solvent, initiator and pore-creating agent, often add a kind of chemical reagent ultrasonic wave dissolution 5 minutes, dissolve completely and be oil phase; In there-necked flask, add deionized water, dispersion agent, after dispersion agent dissolves completely, be aqueous phase; Under agitation oil phase is slowly added in aqueous phase, prepare molecularly imprinted polymer by suspension polymerization;
(2) described in step (1), template molecule is berberine hydrochloride, function monomer is methacrylic acid, linking agent is multiple crosslinking agent, be made up of cross-linking agents Ⅰ maleated rosin vinylformic acid glycol ester and linking agent II Ethylene glycol dimethacrylate, solvent is ethyl acetate, initiator is Diisopropyl azodicarboxylate, and pore-creating agent is peanut oil, and dispersion agent is sodium lauryl sulphate and polyvinyl alcohol, described template molecule, function monomer, cross-linking agents Ⅰ, linking agent II, Diisopropyl azodicarboxylate, peanut oil, the mass ratio of ethyl acetate is (0.034 ~ 3.4): (0.25 ~ 25): 12: (2.4 ~ 36): (0.1 ~ 0.7): (3 ~ 20): (20 ~ 100), deionized water, sodium lauryl sulphate, the mass ratio of polyvinyl alcohol is 100: (0.022 ~ 0.11): (0.011 ~ 0.088), the mass ratio of oil phase and aqueous phase is 1: (2 ~ 9), stirring velocity is 200 ~ 600r/min, adopt temperature programming 55 ~ 80 DEG C reaction 20 ~ 90min, 80 ~ 100 DEG C of reaction 60 ~ 180min, obtain berberine hydrochloride molecularly imprinted polymer,
(3) molecularly imprinted polymer of step (2) gained, through the acetate-methanol eluant solution of volume ratio 3: 1 after screening, until elutriant no longer contains berberine hydrochloride through ultraviolet detection, again with acetic acid, methyl alcohol in steam distillation removing polymkeric substance, obtain molecularly imprinted polymer.
2. application berberine hydrochloride molecular imprinting column according to claim 1 is separated the method for berberine hydrochloride, and it is characterized in that: described berberine hydrochloride molecular imprinting column, diameter and height of column ratio is 1: 1-300.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310142511.2A CN103254189B (en) | 2013-04-23 | 2013-04-23 | Application berberine hydrochloride molecular imprinting column is separated the method for berberine hydrochloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310142511.2A CN103254189B (en) | 2013-04-23 | 2013-04-23 | Application berberine hydrochloride molecular imprinting column is separated the method for berberine hydrochloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103254189A CN103254189A (en) | 2013-08-21 |
| CN103254189B true CN103254189B (en) | 2015-11-04 |
Family
ID=48958453
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310142511.2A Active CN103254189B (en) | 2013-04-23 | 2013-04-23 | Application berberine hydrochloride molecular imprinting column is separated the method for berberine hydrochloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103254189B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105548310B (en) * | 2015-12-21 | 2017-12-01 | 广西民族大学 | A kind of preparation method of the pafenolol molecular imprinting electrochemical sensor of highly sensitive nano zircite doping |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1049485A1 (en) * | 1981-04-17 | 1983-10-23 | Понерт Йиржи (ЧССР) | Process for separating alkaloids produced from plants of genuses berberis, magnola, grataegis and containing tertiary atom of nitrogen or from their quaternary salts and/or impurities |
| JP2001270835A (en) * | 2000-03-15 | 2001-10-02 | Korea Yakult Co Ltd | Extract of perilla frutescens var. acuta kudo effective for prophylaxis and therapy of gastric ulcer, its use and process for obtaining berberine from the extract |
| CN101029889A (en) * | 2007-04-04 | 2007-09-05 | 西安碑林药业股份有限公司 | Method for inspecting Chinese medicinal preparation quality in treatment of old man eyes dieases |
-
2013
- 2013-04-23 CN CN201310142511.2A patent/CN103254189B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1049485A1 (en) * | 1981-04-17 | 1983-10-23 | Понерт Йиржи (ЧССР) | Process for separating alkaloids produced from plants of genuses berberis, magnola, grataegis and containing tertiary atom of nitrogen or from their quaternary salts and/or impurities |
| JP2001270835A (en) * | 2000-03-15 | 2001-10-02 | Korea Yakult Co Ltd | Extract of perilla frutescens var. acuta kudo effective for prophylaxis and therapy of gastric ulcer, its use and process for obtaining berberine from the extract |
| CN101029889A (en) * | 2007-04-04 | 2007-09-05 | 西安碑林药业股份有限公司 | Method for inspecting Chinese medicinal preparation quality in treatment of old man eyes dieases |
Non-Patent Citations (2)
| Title |
|---|
| 分子印迹技术分离中草药功能因子的研究与应用;郭利飞等;《药物分析杂志》;20091231;第29卷(第6期);1055-1062 * |
| 生物碱分子印迹聚合物的制备与其性能研究;陈移姣;《万方学位论文》;20070429;第7、32-36、45页；摘要 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103254189A (en) | 2013-08-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Pardeshi et al. | Precipitation polymerization: a versatile tool for preparing molecularly imprinted polymer beads for chromatography applications | |
| Tang et al. | Application of ionic liquid for extraction and separation of bioactive compounds from plants | |
| CN103497277B (en) | Scutellarin molecularly imprinted polymer and its preparation method and application | |
| Li et al. | Rosin‐based molecularly imprinted polymers as the stationary phase in high‐performance liquid chromatography for selective separation of berberine hydrochloride | |
| CN105628844B (en) | Method determining residue benzimidazole medicine in animal tissue | |
| CN103772595B (en) | A kind of preparation method of multi-template molecular engram monolithic rod | |
| CN103664942A (en) | Method for extracting matrine by coupling molecular imprinting with ultrasonic extraction | |
| Nakamura et al. | Preparation of molecularly imprinted polymers for strychnine by precipitation polymerization and multistep swelling and polymerization and their application for the selective extraction of strychnine from nux‐vomica extract powder | |
| Zhu et al. | Application of ionic liquids in an online ultrasonic assisted extraction and solid-phase trapping of rhodiosin and rhodionin from Rhodiola rosea for UPLC | |
| CN103055831A (en) | Preparation method of inorganic core-shell type quercetin molecularly imprinted polymer microsphere | |
| CN101177499A (en) | Method for preparing estradiol molecular engram polymer | |
| CN103645251B (en) | A kind of fingerprint atlas detection method of compound donkey-hide gelatin preparation | |
| CN105315397B (en) | A kind of preparation method and application for the false template molecule imprinted polymer of hydrophily for being used to detect Gardenoside | |
| CN103254189B (en) | Application berberine hydrochloride molecular imprinting column is separated the method for berberine hydrochloride | |
| CN104316628A (en) | Method for preparing molecularly-imprinted monolithic column by using molecular crowding reagent and ionic liquid as pore-foaming agent | |
| CN103396512A (en) | Hybrid template molecularly imprinted polymer as well as preparation method and application of hybrid template molecularly imprinted solid-phase extraction column | |
| CN103224590B (en) | Glabridin molecularly imprinted polymer, as well as preparation method and application thereof | |
| CN101210041A (en) | Method for separating and preparing tanshinone IIA chemical reference substance | |
| CN106589190B (en) | A kind of preparation method and application of Superhydrophilic molecularly imprinted polymer | |
| CN101851318B (en) | Preparation method of punicalagin molecular imprinted polymer microspheres | |
| CN103884803B (en) | Preparation method for enrofloxacin molecular imprinting monolithic column | |
| CN101012294A (en) | Method of preparing benzodiazepines pharmaceutical molecular engram solid phase extractant | |
| Mou et al. | Highly selective extraction of baicalin in natural herbs and medicinal preparations by molecularly imprinted polymer | |
| Hsu et al. | Rapid chromatographic separation of sulfa drugs by used molecularly imprinted polymer | |
| CN103265665A (en) | Camphor molecular imprinted polymer and preparation method and application of monolithic column and packed column thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20130821 Assignee: GUANGXI DINGHONG RESIN CO.,LTD. Assignor: GUANGXI UNIVERSITY FOR NATIONALITIES Contract record no.: X2022450000425 Denomination of invention: Separation of berberine hydrochloride by molecularly imprinted chromatographic column Granted publication date: 20151104 License type: Exclusive License Record date: 20221227 |
|
| EE01 | Entry into force of recordation of patent licensing contract |