CN102101876A

CN102101876A - Preparation method of arctiin

Info

Publication number: CN102101876A
Application number: CN2010105541759A
Authority: CN
Inventors: 王峰; 王琳; 张发成
Original assignee: Suzhou Paiteng Biomedical Technology Co Ltd
Current assignee: Suzhou Paiteng Biomedical Technology Co Ltd
Priority date: 2010-11-23
Filing date: 2010-11-23
Publication date: 2011-06-22

Abstract

The invention relates to a preparation method of arctiin, which is simple to operate and has the advantages of low pollution and low energy consumption. The method comprises the following steps: taking dry ripe fruits of burdock,, adding into a CO2 supercritical extractor, extracting by using ethanol as an entrainer to obtain an extract, recovering the solvent while depressurizing, carrying out multistage countercurrent extraction by using an ethyl acetate-water (10:2) mixed solvent, merging the extract liquids, recovering the solvent while depressurizing, concentrating the solvent, adding the solvent to macroporous adsorbent resin columns to be adsorbed, eluting with ethanol, collecting the eluent, recovering ethanol while depressurizing, concentrating, adding acetone to crystallize, separating the crystals, washing and drying to obtain the arctiin. The method for preparing arctiin has the advantage of high product purity, and can easily implement industrial scale-up production.

Description

A kind of preparation method of arctinin

Technical field

The present invention relates to a kind of preparation method of arctinin, especially a kind of preparation method who from plant, extracts arctinin.

Background technology

Arctinin (Arctin), molecular formula: C ₂₇H ₃₄O ₁₁, molecular weight: 534.559, CAS accession number: 20362-31-6.Mainly be present among the feverfew burdock Arctium lappa L., raw material sources are abundant.Its molecular formula is as follows:

Modern study shows, arctinin has in platelet aggregation-against, anti-inflammatory, the inhibition urine various active such as PE, and it is also as the raw material of synthetic other reactive derivative simultaneously.

The dry mature fruit of feverfew burdock Arctium lappa L. is used as the Chinese medicine Great Burdock Achene and uses, and has dispelling wind and heat pathogens, a surname's lung promoting eruption, effects such as resolving toxin and disinhibiting the throat.

In the prior art, still be not applicable to preparation technology's report of high purity arctinin industrialized production.

Summary of the invention

Technical problem to be solved by this invention provides a kind of preparation method who is beneficial to big production operation, arctinin that product purity is high.

For solving the problems of the technologies described above, the present invention adopts following technical proposal:

Get the burdock dry mature fruit, join CO ₂In the supercritical extraction device, ethanol is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 2-5%, extracting pressure 20-40MPa, temperature 30-50 ℃, CO ₂Flow 1-3ml/g crude drug min, extraction time 120-180min gets extract, decompression and solvent recovery is that ethyl acetate-water mixed solvent of 10: 2 carries out the extraction of 3-8 stage countercurrent, combining extraction liquid with ratio, decompression and solvent recovery also concentrates, join on the macroporous adsorptive resins and adsorb, the 40-60% ethanol elution is collected 3-8 and is doubly measured the column volume elutriant, decompression recycling ethanol also concentrates, add the acetone crystallization, fractional crystallization washs, is drying to obtain.

CO ₂The volume percent that the supercritical extraction entrainment agent accounts for total extraction solvent is preferably 3%.

CO ₂Supercritical extraction pressure is preferably 30MPa, 40 ℃ of temperature, CO ₂Flow 2ml/g crude drug min.

CO ₂The supercritical extraction time is preferably 150min.

The progression of counter-current extraction is 6 grades.

Macroporous adsorbent resin is selected from a kind of in HPD-700 type, H-50 type, the CD-180 type macroporous adsorbent resin.

The macroporous adsorbent resin wash-out is preferably 50% with concentration of ethanol.

The collecting amount of macroporous adsorbent resin elutriant is preferably 5 times of amount column volumes.

Preparation gained arctinin can adopt following method to detect:

Test example 1 HPLC method is measured arctinin purity

Chromatographic condition

Chromatographic column: octadecylsilane bonding glue silica gel is weighting agent; Moving phase: methanol-water solution (45: 55); Flow velocity: 1.0mL/min; Detect wavelength: 280nm; Column temperature: 30 ℃.

Measuring method

Precision takes by weighing arctinin 2mg, places the 50mL measuring bottle, adds people's methyl alcohol 20mL, and sonic oscillation makes dissolving, and methanol constant volume is drawn 10 μ L to scale, injects high performance liquid chromatograph, adopts normalization method working sample purity.

Adopt the present invention to prepare arctinin, be beneficial to big production operation, energy consumption is little, pollutes little.

The present invention is further elaborated below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.

Embodiment

Embodiment 1

Get burdock dry mature fruit 10Kg, join CO ₂In the supercritical extraction device, ethanol is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 2%, extracting pressure 20MPa, 30 ℃ of temperature, CO ₂Flow 1ml/g crude drug min, extraction time 120min, get extract, decompression and solvent recovery, with ratio is that ethyl acetate-water mixed solvent of 10: 2 carries out the extraction of 3 stage countercurrents, combining extraction liquid, and decompression and solvent recovery also concentrates, join on the HPD-700 type macroporous adsorptive resins and adsorb, 40% ethanol elution is collected 3 times of amount column volume elutriants, and decompression recycling ethanol also concentrates, add the acetone crystallization, fractional crystallization washs, is drying to obtain arctinin 50.3g, detects through HPLC, purity is 95.7%, UV, IR, MS, ²HNMR, ¹³The data of its physical behavior of sign such as CNMR are consistent with prior art.

Embodiment 2

Get burdock dry mature fruit 10Kg, join CO ₂In the supercritical extraction device, ethanol is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 5%, extracting pressure 40MPa, 50 ℃ of temperature, CO ₂Flow 3ml/g crude drug min, extraction time 180min, get extract, decompression and solvent recovery, with ratio is that ethyl acetate-water mixed solvent of 10: 2 carries out the extraction of 8 stage countercurrents, combining extraction liquid, and decompression and solvent recovery also concentrates, join on the H-50 type macroporous adsorptive resins and adsorb, 60% ethanol elution is collected 8 times of amount column volume elutriants, and decompression recycling ethanol also concentrates, add the acetone crystallization, fractional crystallization washs, is drying to obtain arctinin 57.2g, detects through HPLC, purity is 94.4%, UV, IR, MS, ²HNMR, ¹³The data of its physical behavior of sign such as CNMR are consistent with prior art.

Embodiment 3

Get burdock dry mature fruit 10Kg, join CO ₂In the supercritical extraction device, ethanol is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 3%, extracting pressure 30MPa, 40 ℃ of temperature, CO ₂Flow 2ml/g crude drug min, extraction time 150min, get extract, decompression and solvent recovery, with ratio is that ethyl acetate-water mixed solvent of 10: 2 carries out the extraction of 6 stage countercurrents, combining extraction liquid, and decompression and solvent recovery also concentrates, join on the CD-180 type macroporous adsorptive resins and adsorb, 50% ethanol elution is collected 5 times of amount column volume elutriants, and decompression recycling ethanol also concentrates, add the acetone crystallization, fractional crystallization washs, is drying to obtain arctinin 53.6g, detects through HPLC, purity is 98.2%, UV, IR, MS, ²HNMR, ¹³The data of its physical behavior of sign such as CNMR are consistent with prior art.

Claims

1. the preparation method of an arctinin is characterized in that described method is made up of the following step: get the burdock dry mature fruit, join CO ₂In the supercritical extraction device, ethanol is as entrainment agent, and the volume percent that entrainment agent accounts for total extraction solvent is 2-5%, extracting pressure 20-40MPa, temperature 30-50 ℃, CO ₂Flow 1-3ml/g crude drug min, extraction time 120-180min gets extract, decompression and solvent recovery is that ethyl acetate-water mixed solvent of 10: 2 carries out the extraction of 3-8 stage countercurrent, combining extraction liquid with ratio, decompression and solvent recovery also concentrates, join on the macroporous adsorptive resins and adsorb, the 40-60% ethanol elution is collected 3-8 and is doubly measured the column volume elutriant, decompression recycling ethanol also concentrates, add the acetone crystallization, fractional crystallization washs, is drying to obtain.

2. according to the preparation method of the described a kind of arctinin of claim 1, it is characterized in that described CO ₂The volume percent that the supercritical extraction entrainment agent accounts for total extraction solvent is 3%.

3. according to the preparation method of the described a kind of arctinin of claim 1, it is characterized in that described CO ₂Supercritical extraction pressure 30MPa, 40 ℃ of temperature, CO ₂Flow 2ml/g crude drug min.

4. according to the preparation method of the described a kind of arctinin of claim 1, it is characterized in that described CO ₂Supercritical extraction time 150min.

5. according to the preparation method of the described a kind of arctinin of claim 1, the progression that it is characterized in that described counter-current extraction is 6 grades.

6. according to the preparation method of the described a kind of arctinin of claim 1, it is characterized in that described macroporous adsorbent resin is selected from a kind of in HPD-700 type, H-50 type, the CD-180 type macroporous adsorbent resin.

7. according to the preparation method of the described a kind of arctinin of claim 1, it is characterized in that described macroporous adsorbent resin wash-out concentration of ethanol is 50%.

8. according to the preparation method of the described a kind of arctinin of claim 1, the collecting amount that it is characterized in that described macroporous adsorbent resin elutriant is 5 times of amount column volumes.