CN102532147B - Preparation method of high purity dictamnine monomer - Google Patents
Preparation method of high purity dictamnine monomer Download PDFInfo
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- CN102532147B CN102532147B CN201110454155.9A CN201110454155A CN102532147B CN 102532147 B CN102532147 B CN 102532147B CN 201110454155 A CN201110454155 A CN 201110454155A CN 102532147 B CN102532147 B CN 102532147B
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- WIONIXOBNMDJFJ-UHFFFAOYSA-N Dictamnine Chemical compound C1=CC=C2C(OC)=C(C=CO3)C3=NC2=C1 WIONIXOBNMDJFJ-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 239000000178 monomer Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002904 solvent Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000000746 purification Methods 0.000 claims abstract description 5
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 39
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 27
- 230000011218 segmentation Effects 0.000 claims description 10
- 230000005526 G1 to G0 transition Effects 0.000 claims description 9
- 239000000284 extract Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- 230000002411 adverse Effects 0.000 claims description 7
- 238000005070 sampling Methods 0.000 claims description 7
- 238000010828 elution Methods 0.000 claims description 6
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000000741 silica gel Substances 0.000 claims description 5
- 229910002027 silica gel Inorganic materials 0.000 claims description 5
- 238000010898 silica gel chromatography Methods 0.000 claims description 5
- 239000000287 crude extract Substances 0.000 claims description 4
- 230000006837 decompression Effects 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- SRCZQMGIVIYBBJ-UHFFFAOYSA-N ethoxyethane;ethyl acetate Chemical compound CCOCC.CCOC(C)=O SRCZQMGIVIYBBJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 239000003208 petroleum Substances 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 238000010992 reflux Methods 0.000 claims description 2
- 238000013517 stratification Methods 0.000 claims description 2
- 238000002211 ultraviolet spectrum Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 15
- 239000003814 drug Substances 0.000 abstract description 5
- 238000004440 column chromatography Methods 0.000 abstract description 4
- 239000003960 organic solvent Substances 0.000 abstract description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 abstract description 3
- 150000002194 fatty esters Chemical class 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 239000000523 sample Substances 0.000 description 12
- 239000012071 phase Substances 0.000 description 11
- 238000010262 high-speed countercurrent chromatography Methods 0.000 description 10
- 238000005481 NMR spectroscopy Methods 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 6
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 5
- 229940090181 propyl acetate Drugs 0.000 description 4
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 4
- 244000182625 Dictamnus albus Species 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 238000001644 13C nuclear magnetic resonance spectroscopy Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000000825 ultraviolet detection Methods 0.000 description 2
- 235000010894 Artemisia argyi Nutrition 0.000 description 1
- 206010008909 Chronic Hepatitis Diseases 0.000 description 1
- 235000018274 Cunila origanoides Nutrition 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
- 235000014866 Dictamnus albus Nutrition 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 206010034972 Photosensitivity reaction Diseases 0.000 description 1
- 208000003251 Pruritus Diseases 0.000 description 1
- 241001093501 Rutaceae Species 0.000 description 1
- 208000025865 Ulcer Diseases 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 230000001887 anti-feedant effect Effects 0.000 description 1
- 230000001857 anti-mycotic effect Effects 0.000 description 1
- 239000002543 antimycotic Substances 0.000 description 1
- 244000030166 artemisia Species 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 208000010668 atopic eczema Diseases 0.000 description 1
- -1 biology Substances 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 239000000496 cardiotonic agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002330 electrospray ionisation mass spectrometry Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- HZQXXYJHLCSUGQ-UHFFFAOYSA-N ethyl acetate hexane methanol hydrate Chemical compound O.OC.CCCCCC.CCOC(C)=O HZQXXYJHLCSUGQ-UHFFFAOYSA-N 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 208000006454 hepatitis Diseases 0.000 description 1
- 230000007803 itching Effects 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- XELZGAJCZANUQH-UHFFFAOYSA-N methyl 1-acetylthieno[3,2-c]pyrazole-5-carboxylate Chemical compound CC(=O)N1N=CC2=C1C=C(C(=O)OC)S2 XELZGAJCZANUQH-UHFFFAOYSA-N 0.000 description 1
- 201000002266 mite infestation Diseases 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 208000007578 phototoxic dermatitis Diseases 0.000 description 1
- 231100000018 phototoxicity Toxicity 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 201000005404 rubella Diseases 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 208000010110 spontaneous platelet aggregation Diseases 0.000 description 1
- 238000007920 subcutaneous administration Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 231100000397 ulcer Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention relates to a process method of preparing a dictamnine monomer in a separation mode from traditional Chinese medicine cortex dictamni. The process route is (1) adopting organic solvent to extract the traditional Chinese medicine cortex dictamni, and obtaining total extractive; (2) conducting initial purification on the total extractive through single-pass column chromatography chromatography; (3) enabling a solvent system of an obtained sample to be composed of ether or alkane in liquid state, fatty esters, emtrol and water, the volume ratio of the ether or the alkane, the fatty esters, the emtrol and the water is 1:0.5-2:0.5-3:0.5-2. The dictamnine monomer with the purity higher than 99% is obtained in a separation mode by using the method. The process method has the advantages of being large in fractional dose, easy and simple to handle, fast, high in recovery and the like, and effectively reduces preparation cost of the dictamnine monomer.
Description
Technical field
The present invention relates to the separation purification method of Effective Component of Chinese Medicine, be specially and from Dictamnus dasycarpus Turcz, separate the method for preparing high purity dictamnine monomer.
Technical background
Root-bark of Densefruit Pittany be rutaceae shaggy-fruited dittany (
dictamus dasycarpusturcz.) root skin, has heat-clearing and damp-drying drug, effects such as removing toxic substances of dispeling the wind, and can be used for treating that damp and hot sore, yellow water are dripping, the disease such as eczema, rubella, skin itching, mange, yellow subcutaneous ulcer and acute, chronic hepatitis.The main chemical compositions that dictamine (Dictamnine) is Root-bark of Densefruit Pittany, has cardiac stimulant, shrinks unstriated muscle, the effect such as lax blood vessel, antimycotic, DNA phototoxicity, platelet aggregation-against, insect antifeedant, and is a kind of potential preservation agent.
The domestic patent that not yet has pair dictamnine monomer to separate at present, the existing literature method about dictamnine monomer separation preparation mainly adopts repeatedly silica gel column chromatography and Sephadex LH-20 gel column chromatography, its limitation be waste time and energy, contaminate environment, sample purity be low, and column chromatography has non-reversibility adsorption to sample repeatedly, separation obtains that dictamnine monomer preparation efficiency is low, cost is higher, is difficult to develop into the isolation technique that preparation amount is large.
High speed adverse current chromatogram (High-speed Counter-current Chromatography, HSCCC) be a kind of continuous efficient without any solid support growing up for nearly 30 years, liquid liquid distribution chromatography isolation technique fast, it has avoided the sample that solid state adhesion body or carrier bring easily extremely to be adsorbed, the variety of issue such as loss and sex change, while using other liquid phase chromatography to be prepared type separation, its allocative efficiency can significantly reduce, solvent-oil ratio is large, HSCCC guarantees higher peak type resolution, fractional dose is large, sample nondestructive loses, the rate of recovery is high, isolating environment relaxes, save solvent.High speed adverse current chromatogram can directly enter slightly get sample in a large number product or synthetic mixture, and separating resulting can reach quite high purity, has been widely used in preparation separation and the purifying of the field chemical substances such as biology, medicine, environmental protection.
Summary of the invention
The object of the invention is column chromatogram chromatography and high-speed countercurrent chromatography to combine, give full play to their advantages separately, develop a kind of preparation cost lower than prior art, easy and simple to handle, efficiency is high, can, more in enormous quantities from Dictamnus dasycarpus Turcz, separate and prepare the method for separating and preparing that purity is greater than 99% dictamnine monomer.
For achieving the above object, the present invention adopts following technical scheme to realize: a kind of preparation method of high purity dictamnine monomer, and it comprises the following steps:
(1) adopt organic solvent to extract Root-bark of Densefruit Pittany, extracting solution vacuum concentration is become to medicinal extract, obtain general extractive;
(2) by column chromatography single chromatography for gained general extractive, carry out preliminary purification, collect the component that contains dictamine, merge, solvent evaporated, obtains dictamine rough segmentation thing;
(3) adopt high-speed countercurrent chromatography purifying dictamine rough segmentation thing, separate and make purity higher than 99% dictamnine monomer.
The concrete feature of this programme also has, and in step (1), organic solvent is sherwood oil or ether.
The stationary phase that column chromatogram chromatography adopts is that granularity is 50～400 object silica gel, the binary liquid mixture that moving phase is made up of component A and B, and A component is sherwood oil; B component is ethyl acetate; The volume ratio of A and B is 1～10:1.
The refining solvent system that step (3) high speed counter current chromatography adopts is made up of E, F, C, tetra-components of D, E component can be selected from sherwood oil or normal hexane, F component is ethyl acetate or propyl acetate, C component is methyl alcohol or ethanol, D component is water, and the volume ratio of E, F, C, D is 1:0.5～2:0.5～3:0.5～2.
Normal hexane in refining solvent system: ethyl acetate: methyl alcohol: water=1:1:1.2:1.
Particularly, step is as follows:
1. the preparation of total crude extract: after Root-bark of Densefruit Pittany pulverizing medicinal materials, use organic solvent extraction 3 times, filter, filtrate decompression is condensed into medicinal extract.
2. obtaining of dictamine rough segmentation thing: get and extract gained medicinal extract, carry out single silica gel column chromatography, the binary liquid mixture of different ratios for moving phase, A component is sherwood oil; B component is ethyl acetate.The volume ratio of A and B is 1～10:1.
3. high-speed countercurrent chromatography purifying dictamine: the dictamine rough segmentation thing that silica gel is separated carries out high-speed countercurrent chromatography separation, solvent system is made up of four components, E component can be selected from the ethers such as sherwood oil, normal hexane or alkanes, F component can be selected from the fatty ester such as ethyl acetate, propyl acetate class, C component can be selected from the fatty alcohol such as methyl alcohol, ethanol, D component is water, preferably normal hexane-ethyl acetate-methanol-water system, and the volume ratio of E, F, C, D is 1:0.5～2:0.5～3:0.5～2.Detailed process is: preparation solvent systems, fully shake up rear leaving standstill, and after layering, will separate mutually up and down; With pump by the upper separator column that injects mutually high-speed counter-current chromatograph of solvent systems; The upper and lower phase of getting solvent systems is dissolved dictamine rough segmentation matter sample; Open counter current chromatograph, inject the lower balance of carrying out mutually of solvent systems; Solvent systems reaches after fluid dynamic equilibrium, injects sample solution; Detect elutant by UV-detector, collect target components according to the color atlas of gained.
4. the evaluation at HPLC analysis and HSCCC peak: utilize high performance liquid chromatography (HPLC) to analyze extract.High-efficient liquid phase chromatogram condition: Shimadzu Shim pack VP-ODS post (4.6 mm × 250 mm), ultraviolet detection wavelength 236 nm, column temperature: 25 ℃, flow velocity: 1.0 mL/min, sample size: 10 μ L, moving phase adopts methyl alcohol: water=60:40.
The evaluation at HSCCC peak: application Agilent 5973N mass spectrograph and Varian 600 MHz nuclear magnetic resonance spectrometers carry out respectively MS,
1h-NMR and
13the mensuration of C-NMR spectrum.
Advantage of the present invention is: good separating effect, efficiency purity high, dictamnine monomer product reach more than 99%, the preparation cost of dictamnine monomer, far below prior art, is a kind of economy, the efficient method of preparing high purity dictamnine monomer that separates from Root-bark of Densefruit Pittany medicinal material.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention; Fig. 2 is the high speed adverse current chromatogram figure of embodiment 1; Fig. 3 is the high speed adverse current chromatogram figure of embodiment 2; Fig. 4 is the high-efficient liquid phase chromatogram of crude extract; Fig. 5 is the high-efficient liquid phase chromatogram of dictamnine monomer.
Embodiment
Below in conjunction with specific embodiment and accompanying drawing, the present invention will be described.
Embodiment 1:
As shown in Fig. 1 dictamnine monomer preparation flow figure.
1. after getting the 10 kg pulverizing of Root-bark of Densefruit Pittany medicinal material, by sherwood oil refluxing extraction, 3 times (each 2 h), filters, and filtrate decompression is condensed into medicinal extract, obtains Root-bark of Densefruit Pittany general extractive 101.7 g.
2. above-mentioned sherwood oil general extractive is carried out to single silica gel column chromatography (8.0 × 110 cm, silica gel amount 2 kg, 200-300 order), adopt the petroleum ether-ethyl acetate gradient elution of different ratios, high performance liquid chromatography is followed the tracks of and is detected petrol ether/ethyl acetate solvent elution 3:1 to 2:1 part, merge and contain dictamine component, obtain dictamine rough segmentation thing 11.2 g.
3. application high speed adverse current chromatogram separation and purification dictamine rough segmentation thing
Solvent systems is normal hexane: ethyl acetate: methyl alcohol: water=1:1:1.2:1, and high-speed counter-current chromatograph column volume is 260 mL, applied sample amount 500 mg, rotating speed 800rpm, upper is stationary phase mutually, lower is moving phase mutually, flow velocity 2.0 mL/min, stationary phase retention rate 65%, detects wavelength 254 nm.
Concrete operation steps is: by above-mentioned solvent ratios preparation solvent systems, be placed in separating funnel, shake up rear stratification, after ready to balance for some time, upper and lower two-phase is separated, upper is stationary phase mutually, lower is moving phase mutually, and getting 500 mg dictamine crude extracts, to be dissolved in 5 mL upper stand-by in the mixture of phase mutually and under 5 mL.Adopt the semi-preparative high-speed counter-current chromatograph of Beijing Chinese mugwort Mrrrill Lynch development, it is by ram pump, sampling valve, Ultraviolet Detector, registering instrument and the chromatography column (spiral tube being formed by polyfluortetraethylene pipe multiple wraps, capacity is 260mL) etc. composition, first make sampling valve in sample introduction state, stationary phase is filled to chromatography column with pump with certain flow rate, termination of pumping.Opening speed controller, make the chromatographic chromatography column forward of high speed flow, when turn up 800rpm, it is 2.0 mL/min that flow rate of mobile phase is set, start pump moving phase, reach after fluid dynamic equilibrium, the sample having dissolved is injected to the liquid storage tube of counter current chromatograph sampling valve with syringe, rotation sampling valve, for connecing column state, makes sample enter chromatography column.Then receive and receive target component according to detector ultraviolet spectrogram (Fig. 2), obtain dictamnine monomer 245 mg, HPLC purity assay is 99.8%.
Utilize efficient liquid phase chromatographic analysis isolate, liquid-phase condition: Shimadzu Shim pack VP-ODS post (4.6 mm × 250 mm), ultraviolet detection wavelength 236 nm, column temperature: 25 ℃, flow velocity: 1.0 ml/min, sample size: 10 μ L, moving phase is methyl alcohol: water=60:40.
Structural Identification: Agilent 5973N mass spectrograph is carried out in the dictamine application obtaining and Varian 600 MHz nuclear magnetic resonance spectrometers carry out respectively MS to separating,
1h-NMR and
13the mensuration of C-NMR spectrum, the data obtained is as follows:
White powder, ESI-MS (positive mode),
m/z[200.0 M+H]
+.
1h-NMR (600 MHz, CDCl
3)
δppm:4.43 (3H, s, OCH
3), 7.06 (1H, d,
j=3.0 Hz, H-3), 7.44 (1H, t,
j=7.8 Hz, H-6), 7.61 (1H, d,
j=3.0 Hz, H-2), 7.68 (1H, t,
j=7.8 Hz, H-7), 8.01 (1H, d,
j=2.4 Hz, H-8), 8.25 (1H, d,
j=8.4 Hz, H-5).
13c-NMR (150 MHz, CDCl
3)
δppm:143.5 (C-2), 104.7 (C-3), 118.6 (C-3a), 156.9 (C-4), 103.4 (C-4a), 122.4 (C-5), 123.7 (C-6), 129.7 (C-7), 127.6 (C-8), 145.5 (C-8a), 163.8 (C-9a), 59.0 (OCH
3).
Embodiment 2
As shown in Fig. 1 dictamnine monomer preparation flow figure.
1. after getting the 10 kg pulverizing of Root-bark of Densefruit Pittany medicinal material, with aether backflow extraction 3 times, (each 2 h), filters, and filtrate decompression is condensed into medicinal extract, obtains Root-bark of Densefruit Pittany general extractive 152.4 g.
2. above-mentioned ether general extractive is carried out to single silica gel column chromatography (8.0 × 110 cm, silica gel amount 2.5 kg, 200-300 order), adopt the petroleum ether-ethyl acetate gradient elution of different ratios, high performance liquid chromatography is followed the tracks of and is detected petrol ether/ethyl acetate solvent elution 3:1 to 2:1 part, merge and contain dictamine component, obtain dictamine rough segmentation thing 12.3 g.
3. separating selected solvent systems is sherwood oil: ethyl acetate: ethanol: water=1:0.9:1.1:1, all the other steps are with embodiment 1.Obtain purity and be 99.6% dictamnine monomer 224 mg, high speed adverse current chromatogram separates ultraviolet spectrogram and sees Fig. 3.
Embodiment 3
Separating selected solvent systems is sherwood oil: propyl acetate: ethanol: water=1:0.7:1:0.7, all the other steps are with embodiment 1.Obtain purity and be 99.2% dictamnine monomer 231 mg.
Embodiment 4
Separating selected solvent systems is normal hexane: ethyl acetate: methyl alcohol: water=1:1:1.1:0.9, all the other steps are with embodiment 1.Obtain purity and be 99.5% dictamnine monomer 236 mg.
Embodiment 5
Separating selected solvent systems is sherwood oil: propyl acetate: methyl alcohol: water=1:0.8:0.9:0.8, all the other steps are with embodiment 1.Obtain purity and be 99.2% dictamnine monomer 221 mg.
Embodiment 6
Separating selected solvent systems is normal hexane: ethyl acetate: ethanol: water=1:0.9:1:1.1, all the other steps are with embodiment 1.Obtain purity and be 99.4% dictamnine monomer 229 mg.
Embodiment 7
Separating selected solvent systems is normal hexane: propyl acetate: ethanol: water=1:0.7:0.9:1.2, all the other steps are with embodiment 1.Obtain purity and be 99.5% dictamnine monomer 232 mg.
Claims (1)
1. a preparation method for dictamnine monomer, is characterized in that it comprises the following steps:
(1) get after Root-bark of Densefruit Pittany medicinal material 10 kg pulverize and use sherwood oil refluxing extraction 3 times, each 2 h, filter, and filtrate decompression is condensed into medicinal extract, obtains Root-bark of Densefruit Pittany general extractive 101.7 g;
(2) above-mentioned sherwood oil general extractive is carried out to single silica gel column chromatography: 8.0 × 110 cm, silica gel amount 2 kg, 200-300 order, adopt the petroleum ether-ethyl acetate gradient elution of different ratios, high performance liquid chromatography is followed the tracks of and is detected petrol ether/ethyl acetate solvent elution 3:1 to 2:1 part, merge and contain dictamine component, obtain dictamine rough segmentation thing 11.2 g;
(3) application high speed adverse current chromatogram separation and purification dictamine rough segmentation thing; Solvent systems is normal hexane: ethyl acetate: methyl alcohol: water=1:1:1.2:1, and high-speed counter-current chromatograph column volume is 260 mL, applied sample amount 500 mg, rotating speed 800rpm, upper is stationary phase mutually, lower is moving phase mutually, flow velocity 2.0 mL/min, stationary phase retention rate 65%, detects wavelength 254 nm; Concrete operation steps is: by above-mentioned solvent ratios preparation solvent systems, be placed in separating funnel, shake up rear stratification, after ready to balance for some time, upper and lower two-phase is separated, upper is stationary phase mutually, lower is moving phase mutually, and getting 500 mg dictamine crude extracts, to be dissolved in 5 mL upper stand-by in the mixture of phase mutually and under 5 mL; Adopt semi-preparative high-speed counter-current chromatograph, chromatography column is the spiral tube being formed by polyfluortetraethylene pipe multiple wraps, and capacity is 260mL; First make sampling valve in sample introduction state, stationary phase is filled to chromatography column with pump with certain flow rate, termination of pumping; Opening speed controller, make the chromatographic chromatography column forward of high speed flow, when turn up 800rpm, it is 2.0 mL/min that flow rate of mobile phase is set, start pump moving phase, reach after fluid dynamic equilibrium, the sample having dissolved is injected to the liquid storage tube of counter current chromatograph sampling valve with syringe, rotation sampling valve, for connecing column state, makes sample enter chromatography column; Then according to detector UV spectrum Fig. 2 receiving target composition, obtain dictamnine monomer 245 mg.
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| Title |
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| 张红晶.白鲜皮中化学成分的提取分离及活性评价研究.《吉林农业大学硕士学位论文》.2011,第15-28页. |
| 李翔，等.从白鲜皮中同时制备梣酮、白鲜碱、黄柏酮单体的方法.《四川大学学报(工程科学版)》.2007,第39卷(第41期),第68-72页. * |
| 白鲜皮中化学成分的提取分离及活性评价研究;张红晶;《吉林农业大学硕士学位论文》;20111103;第15-28页 * |
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