CN103304490A - Method for separating and purifying five purine and pyrimidine bases from trichosanthes bark - Google Patents
Method for separating and purifying five purine and pyrimidine bases from trichosanthes bark Download PDFInfo
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Abstract
The invention relates to a method for separating and purifying five purine and pyrimidine bases (namely cytosine, uracil, hypoxanthine, guanine and xanthine) from trichosanthes bark. According to the method, five high-purity monomeric compounds, namely cytosine, uracil, hypoxanthine, guanine and xanthine, are obtained from the trichosanthes bark through the following steps of: (1) preparing a crude trichosanthes bark extract; (2) carrying out crude separation by using a macroporous adsorption resin column; and (3) carrying out separation and purification by using semi-preparative high-performance liquid chromatography: carrying out separation and purification on a sample 1 and a sample 2 by using the semi-preparative high-performance liquid chromatography, wherein the mobile phase is methanol-water. The method disclosed by the invention has the advantages that the process flow is environment-friendly, the damage to the environment is not serious, and the comprehensive cost is low.
Description
Technical field
The invention belongs to chemical field, specifically relate to a kind of from the Chinese medicine Snakegourd Peel method of 5 kinds of purine of separation and purification and pyrimidine bases (cytosine(Cyt), uridylic, xanthoglobulin, guanine and xanthine).
Background technology
Snakegourd Peel be Curcurbitaceae snake gourd plant snakegourd (
Trichosanthes kirilowiiMarim.) or trichosanthes rosthornii Harms (
Trichosanthes rosthorniiHarms.) dry mature skin belongs to conventional Chinese medicine, has the effects such as moistening the lung and resolving the phlegm, the wide chest of sharp gas, is widely used in clinically the diseases such as treatment phlegm heat cough, the turbid Huang of phlegm are thick, pharyngalgia, pectoralgia, haematemesis, bleeding from five sense organs or subcutaneous tissue, constipation, carbuncle pyogenic infections from tumour or sore.Modern pharmacology experiment and clinical practice show that Snakegourd Peel has coronary artery dilator, increases coronary flow, improves myocardial hypoxia tolerance, reduces serum cholesterol, the multiple pharmacological effect such as antibiotic, anticancer, especially cardiovascular disorder are had good therapeutic action.
Nucleic acid has comprised biological heredity information, purine, miazines Biological Base are the important component parts that consists of nucleic acid, the multiple vital movements such as wide participation heredity and metabolism, their metabolic disturbance often causes many serious diseases, such as renal failure, gout and male sterility etc.Xanthoglobulin is a kind of very important biological purine bases, have reducing blood pressure, relieving asthma, treat the pharmacologically actives such as gout, widely distributed in human body, can participate in some the important physiological functions in the balance the body, also can be used for treating the diseases such as leukopenia due to a variety of causes, thrombocytopenia, report that also the growth metabolism of xanthine, xanthoglobulin and tumour cell is in close relations abroad.
Now existing bibliographical information extracts the method for purifying purine and miazines Biological Base from Snakegourd Peel.Teng Yongrong [Snakegourd Peel and Pericarpium Trichosanthis injection chemical constitution study, Shandong Traditional Chinese Medicine University's master thesis, 2011] utilize repeatedly the separation means such as silica gel column chromatography, macroporous adsorbent resin column chromatography and preparative high performance liquid chromatography that the chemical composition of Snakegourd Peel is studied, obtain altogether 7 compounds, comprising 3 gradient elutions (the different inosine of VITAMIN B4, guanosine-and 6-).Shi Yanpeng [research of snakegourd chemical composition and the assay of hitodesterol (I) thereof, herbal medicine, 1 phase in 2002] utilize repeatedly silica gel column chromatography that the chemical composition of snakegourd is studied, obtain 12 compounds from petroleum ether part, chloroform extract, n-butanol portion separation, wherein 10 have obtained evaluation, comprise a kind of gradient elution-uridylic.Liu Dailin [the platelet aggregation inhibitory activity composition Study of Snakegourd Fruit. herbal medicine, 12 phases in 2004] utilize the active method for tracing of platelet aggregation-against, adopt Sephadex LH-20 column chromatography and repeatedly silica gel column chromatography separation, in Snakegourd Fruit, separate obtaining 7 compounds, comprising a kind of gradient elution-adenosine.
The problem that aforesaid method mainly exists is: the sepn process step is comparatively loaded down with trivial details, sometimes need to use chloroform as extraction agent or
Eluent human body and environment are all had serious harm, and the kind of the purine that obtains and pyrimidine bases is few, and the production cycle is longer, and production cost is higher.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of easy and simple to handle, environmental protection, the comprehensive cost fast method of separation and purification purine and pyrimidine bases from the Chinese medicine Snakegourd Peel low, with short production cycle are provided.
The solution of the present invention is as follows:
The method of separation and purification purine and pyrimidine bases the steps include: from the Chinese medicine Snakegourd Peel
(1) preparation of Snakegourd Peel crude extract: get the Snakegourd Peel medicinal material that crushes, the water heating and refluxing extraction, extracting solution is about 1.2 through being evaporated to relative density, adding 95% ethanol to the concentration of ethanol in the concentrated solution is about 70%, leave standstill 72 h, filter, get supernatant liquid, concentrating under reduced pressure gets crude extract;
(2) macroporous adsorptive resins roughing out: the Snakegourd Peel crude extract is soluble in water, upper HPD826 type macroporous adsorptive resins carries out chromatography, elder generation's water carries out wash-out, be that about 5% ethanol-water solution carries out wash-out with concentration again, collect respectively the alcohol-water elutriant about water and 5%, the former concentrating under reduced pressure gets sample 1, latter's concentrating under reduced pressure gets sample 2;
(3) the further separation and purification of sample 1: sample 1 usefulness Semipreparative chromatography is carried out separation and purification, and chromatographic column is YMC ODS-AQ post, and moving phase is methanol-water, and detecting wavelength is 254 nm;
(4) the further separation and purification of sample 2: sample 2 usefulness Semipreparative chromatographies are carried out separation and purification, and chromatographic column is YMC ODS-AQ post, and moving phase is methanol-water, and detecting wavelength is 254 nm;
Collect the target components cut, the cut concentrating under reduced pressure with obtaining namely obtains the monomeric compound that will separate.
Foregoing method, preferably scheme is, and extraction time is 1-3 hour during step (1) heating and refluxing extraction, and extraction time is 2-6 time.More preferably, extraction time is 1.5-2.5 hour (preferred 2 hours), and extraction time is 3-5 time (preferred 4 times).
Foregoing method, preferably scheme is, step (3) moving phase is the methanol-water elutriant (preferred 2%) of 0-5%, eluent flow rate is preferred 3.5 mL/min of 2.5-4.5 mL/min().
Foregoing method, preferred scheme is that when step (4) was carried out wash-out with the methanol-water elutriant, the mass concentration of used methyl alcohol was 2%-6%(preferred 4%).Eluent flow rate is preferred 3.5 mL/min of 2.5-4.5 mL/min().
Foregoing method, preferred scheme is, step (3) type of elution is methanol-water gradient elution/2% methanol-water isocratic elution/100% water isocratic elution/5% methanol-water isocratic elution, and preferably, eluent flow rate is preferred 3.5 mL/min of 2.5-4.5 mL/min().
Foregoing method, preferred scheme is, type of elution during step (4) separation and purification is 6% methanol-water isocratic elution/4% methanol-water isocratic elution/2% methanol-water isocratic elution/methanol-water gradient elution, preferably, eluent flow rate is preferred 3.5 mL/min of 2.5-4.5 mL/min().
The present invention relates to the method for separation and purification purine and pyrimidine bases from the Chinese medicine Snakegourd Peel, step is: the preparation of (1) Snakegourd Peel crude extract: get the Snakegourd Peel medicinal material that crushes, the water heating and refluxing extraction, extracting solution is about 1.2 through being evaporated to relative density, adding 95% ethanol to the concentration of ethanol in the concentrated solution is about 70%, leaves standstill 72 h, filters, get supernatant liquid, concentrating under reduced pressure gets crude extract.(2) macroporous adsorptive resins roughing out: the Snakegourd Peel crude extract is soluble in water, upper HPD826 type macroporous adsorptive resins carries out chromatography, elder generation's water carries out wash-out, be that about 5% alcohol-water is that elutriant carries out wash-out with concentration again, collect respectively the alcohol-water elutriant about water and 5%, the former concentrating under reduced pressure gets sample 1, latter's concentrating under reduced pressure gets sample 2.(3) the further separation and purification of sample 1: sample 1 usefulness Semipreparative chromatography is carried out separation and purification, chromatographic column is YMC ODS-AQ post (250 mm * 10 mm I. D., 10 μ m, Science and Technology Ltd. is separated in large Shen, Liaanjiang county), moving phase is methanol-water, and detecting wavelength is 254 nm.(4) the further separation and purification of sample 2: sample 2 usefulness Semipreparative chromatographies are carried out separation and purification, chromatographic column is YMC ODS-AQ post (250 mm * 10 mm I. D., 10 μ m, Science and Technology Ltd. is separated in large Shen, Liaanjiang county), moving phase is methanol-water, and detecting wavelength is 254 nm.
The environmental protection of this technological process, without serious harm, comprehensive cost is low to environment.
The method of the present invention 5 kinds of purine of separation and purification and pyrimidine bases from the Chinese medicine Snakegourd Peel, at first adopt the macroporous adsorptive resins roughing out, carry out separation and purification with the Semipreparative chromatography method again, gained target compound purity is high, foreign matter content is extremely low, and this point can be found out from Fig. 5-Fig. 9.In addition, also have following advantage:
(1) can remove most impurity after the roughing out of extract process macroporous adsorptive resins; the composition of mixture is simplified; can reduce difficulty for follow-up mask work; and can protect the Semipreparative chromatography post not contaminated, effectively prolong the work-ing life of chromatographic column.
(2) use twice separation and purification of Semipreparative chromatography method just can obtain simultaneously cytosine(Cyt), uridylic, xanthoglobulin, guanine and 5 kinds of high-purity monomer compounds of xanthine, method is simple to operate, and efficient is high, and process cycle is short, save reagent, reduced production cost.
(3) do not use in the purge process environment and the large organic solvents such as chloroform of harm, macroporous adsorbent resin can be reused repeatedly environmental protection after regeneration.
(4) optimized the condition (composition of elutriant and flow velocity) of chromatography method, the purity of compound and efficient are all greatly improved.
Description of drawings
Fig. 1 is the high-efficient liquid phase chromatogram of sample 1.
Fig. 2 is the high-efficient liquid phase chromatogram of sample 2.
Fig. 3 is the Semipreparative chromatography figure of sample 1.
Fig. 4 is the Semipreparative chromatography figure of sample 2.
Fig. 5 is high-efficient liquid phase chromatogram and the ultraviolet spectrogram of cytosine(Cyt).
Fig. 6 is high-efficient liquid phase chromatogram and the ultraviolet spectrogram of uridylic.
Fig. 7 is hypoxanthic high-efficient liquid phase chromatogram and ultraviolet spectrogram.
Fig. 8 is high-efficient liquid phase chromatogram and the ultraviolet spectrogram of guanine.
Fig. 9 is xanthic high-efficient liquid phase chromatogram and ultraviolet spectrogram.
Embodiment
Describe technical scheme of the present invention in detail below in conjunction with embodiment and accompanying drawing, but protection domain is not by this restriction.Equipment used or raw material all can obtain from market among the embodiment.Agents useful for same is all available from Jinan reagent head factory, and institute's water is deionized water.
Embodiment:The method of separation and purification purine and pyrimidine bases the steps include: from the Chinese medicine Snakegourd Peel
(1) preparation of Snakegourd Peel crude extract: the Snakegourd Peel medicinal material after crushed, take water as the solvent heating and refluxing extraction 4 times, united extraction liquid, being evaporated to relative density is about 1.2, adding 95% ethanol to the concentration of ethanol in the concentrated solution is about 70%, leaves standstill 72 h, filters, get supernatant liquid, concentrating under reduced pressure gets crude extract.
(2) macroporous adsorptive resins roughing out: the Snakegourd Peel crude extract is soluble in water, upper HPD826 type macroporous adsorptive resins carries out chromatography, elder generation's water carries out wash-out, be that about 5% ethanol-water solution carries out wash-out with concentration again, collect respectively the alcohol-water elutriant about water and 5%, the former concentrating under reduced pressure gets sample 1, latter's concentrating under reduced pressure gets sample 2.
(3) the further separation and purification of sample 1: sample 1 usefulness Semipreparative chromatography is carried out separation and purification, chromatographic column is YMC ODS-AQ post (250 mm * 10 mm I. D., 10 μ m, Science and Technology Ltd. is separated in large Shen, Liaanjiang county), moving phase is methanol-water, and detecting wavelength is 254 nm.
(4) the further separation and purification of sample 2: sample 2 usefulness Semipreparative chromatographies are carried out separation and purification, chromatographic column is YMC ODS-AQ post (250 mm * 10 mm I. D., 10 μ m, Science and Technology Ltd. is separated in large Shen, Liaanjiang county), moving phase is methanol-water, and detecting wavelength is 254 nm.
Collect the target components cut, the cut concentrating under reduced pressure with obtaining namely obtains the monomeric compound that will separate.
The contriver makes moving phase by the methyl alcohol that uses different concns, adopts different types of elution, and the flow velocity of control elutriant is preferred 3.5 mL/min of 2.5-4.5 mL/min(), optimized the purification condition of realizing the object of the invention, relevant experimental result is as follows:
The Semipreparative chromatography separation condition of table one sample 1
| ? | The elutriant condition |
| Embodiment 1 | 5% methanol-water isocratic elution |
| Embodiment 2 | 2% methanol-water isocratic elution |
| Embodiment 3 | 100% water isocratic elution |
| Embodiment 4 | The methanol-water gradient elution |
In embodiment 1, adopting 5% methanol-water is the elutriant isocratic elution, and each composition elution time is shorter, but separating effect is not ideal enough each other, and gained composition purity is lower.Adopting 2% methanol-water among the embodiment 2 is the elutriant isocratic elution, separates well between each composition, and disengaging time is also comparatively suitable.Adopting 100% water among the embodiment 3 is the elutriant isocratic elution, and each component separating is good, but disengaging time is oversize.Embodiment 4 adopts the methanol-water gradient elutions, and each component separating is good, disengaging time also can, but elutriant is because change in concentration causes recycling to have larger difficulty.
Fig. 3 is the color atlas when selecting embodiment 2 system, and as seen from Figure 3, each component separating is good, and disengaging time is also comparatively suitable.Collect each peak component according to color atlas, behind the recovery solvent, can obtain corresponding high-purity compound.Through high performance liquid chromatography area normalization method analytical test, the purity of embodiment 2 resulting each components is very high, and all more than 98%, this point can be found out from Fig. 5-Fig. 6.
The Semipreparative chromatography separation condition of table two sample 2
| ? | The |
| Embodiment | |
| 5 | 6% methanol-water isocratic elution |
| Embodiment 6 | 4% methanol-water isocratic elution |
| Embodiment 7 | 2% methanol-water isocratic elution |
| Embodiment 8 | The methanol-water gradient elution |
In embodiment 5, adopting 6% methanol-water is the elutriant isocratic elution, and each composition elution time is shorter, but separating effect is not ideal enough each other, and gained composition purity is lower.Adopting 4% methanol-water among the embodiment 6 is the elutriant isocratic elution, separates well between each composition, and disengaging time is also comparatively suitable.Adopting 2% methanol-water among the embodiment 7 is the elutriant isocratic elution, and each component separating is good, but disengaging time is oversize.Embodiment 8 adopts the methanol-water gradient elutions, and each component separating is good, disengaging time also can, but elutriant is because change in concentration causes recycling to have larger difficulty.
Fig. 4 is the color atlas when selecting embodiment 6 system, and as seen from Figure 4, each component separating is good, and disengaging time is also comparatively suitable.Collect each peak component according to color atlas, behind the recovery solvent, can obtain corresponding high-purity compound.Through high performance liquid chromatography area normalization method analytical test, the purity of embodiment 6 resulting each components is very high, and all more than 98%, this point can be found out from Fig. 7-Fig. 9.
According to the test of proton nmr spectra and carbon spectrum, gained peak component is identified, obtained cytosine(Cyt), uridylic, xanthoglobulin, guanine and xanthine.The structural formula of 5 compounds that obtain through Modern spectroscopy purifying that data acknowledgement is extracted is as follows:
The qualification result of 5 kinds of compounds is as follows:
Compound I (cytosine(Cyt)):
1H-NMR(400 MHz, DMSO-d
6)
δPpm:10.47(1H, br s, 1-H), 7.32(1H, d,
J=6.8 Hz, 6-H), 7.04(2H, br s, 4-NH
2), 5.57(1H, d,
J=6.8 Hz, 5-H).
13C-NMR（100?MHz，DMSO-d
6）
δ?ppm：166.6（C-4），156.8（C-2），142.5（C-6），92.4（C-5）。
Compound I I(uridylic):
1H-NMR(400 MHz, DMSO-d
6)
δPpm:10.48(2H, br s, 1-H, 3-H), 7.39(1H, d,
J=7.6 Hz, H-6), 5.44(1H, d,
J=7.6 Hz, H-5).
13C-NMR（100?MHz，DMSO-d
6）
δ?ppm：164.1（C-4），151.4（C-2），142.1（C-6），100.0（C-5）。
Compound III (xanthoglobulin):
1H-NMR(400 MHz, DMSO-d
6)
δPpm:13.20(1H, br s, 9-H), 12.29(1H, br s, 1-H) and, 8.18(1H, s, 2-H), 8.11(1H, s, H-8).
13C-NMR（100?MHz，DMSO-d
6）
δ?ppm：155.6（C-6），153.7（C-4），152.7（C-8），144.1（C-2），119.5（C-5）。
Compound IV (guanine):
1H-NMR(400 MHz, D
2O)
δPpm:7.34(1H, s, 8-H).
13C-NMR（100?MHz，D
2O）
δ?ppm：155.8（C-6），149.1（C-4），147.2（C-2），136.7?（C-8），106.5（C-5）。
Compound V(xanthine):
1H-NMR(400 MHz, D
2O)
δPpm:7.35(1H, s, 8-H).
13C-NMR（100?MHz，D
2O）
δ?ppm：155.4（C-6），152.2（C-2），150.4（C-4），141.6（C-8），106.9（C-5）。
Should be pointed out that embodiment is the more representational example of the present invention, obvious technical scheme of the present invention is not limited to above-described embodiment.A lot of distortion can also be arranged.Those of ordinary skill in the art from then on disclosedly in the file mentions or associates, and all should think the claimed scope of this patent.
Claims (9)
1. the method for separation and purification purine and pyrimidine bases from the Chinese medicine Snakegourd Peel is characterized in that, step is:
(1) preparation of Snakegourd Peel crude extract: get the Snakegourd Peel medicinal material that crushes, the water heating and refluxing extraction, extracting solution is about 1.2 through being evaporated to relative density, adding 95% ethanol to the concentration of ethanol in the concentrated solution is about 70%, leave standstill 72 h, filter, get supernatant liquid, concentrating under reduced pressure gets crude extract;
(2) macroporous adsorptive resins roughing out: the Snakegourd Peel crude extract is soluble in water, upper HPD826 type macroporous adsorptive resins carries out chromatography, elder generation's water carries out wash-out, be that about 5% ethanol-water solution carries out wash-out with concentration again, collect respectively the alcohol-water elutriant about water and 5%, the former concentrating under reduced pressure gets sample 1, latter's concentrating under reduced pressure gets sample 2;
(3) the further separation and purification of sample 1: sample 1 usefulness Semipreparative chromatography is carried out separation and purification, and chromatographic column is YMC ODS-AQ post, and moving phase is methanol-water, and detecting wavelength is 254 nm;
(4) the further separation and purification of sample 2: sample 2 usefulness Semipreparative chromatographies are carried out separation and purification, and chromatographic column is YMC ODS-AQ post, and moving phase is methanol-water, and detecting wavelength is 254 nm;
Collect the target components cut, the cut concentrating under reduced pressure with obtaining namely obtains the monomeric compound that will separate.
2. method according to claim 1 is characterized in that, extraction time is 1-3 hour during step (1) reflux.
3. method according to claim 2 is characterized in that, step (1) extraction time is 1.5-2.5 hour (preferred 2 hours).
4. method according to claim 1 is characterized in that, step (1) extraction time is 2-6 time.
5. method according to claim 1 is characterized in that, step (1) extraction time is 3-5 time (preferred 4 times).
6. method according to claim 1 is characterized in that, step (3) type of elution is methanol-water gradient elution/2% methanol-water isocratic elution/100% water isocratic elution/5% methanol-water isocratic elution.
7. method according to claim 6 is characterized in that, eluent flow rate is preferred 3.5 mL/min of 2.5-4.5 mL/min().
8. method according to claim 1 is characterized in that, the type of elution during step (4) separation and purification is 6% methanol-water isocratic elution/4% methanol-water isocratic elution/2% methanol-water isocratic elution/methanol-water gradient elution.
9. method according to claim 1 is characterized in that, eluent flow rate is preferred 3.5 mL/min of 2.5-4.5 mL/min().
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| CN105541944A (en) * | 2016-03-02 | 2016-05-04 | 上海上药第一生化药业有限公司 | Preparation method of chemical components in trichosanthes kirilowii Maxim injection and application of chemical components |
| CN105646628A (en) * | 2016-03-02 | 2016-06-08 | 上海上药第生化药业有限公司 | Method for preparing chemical constituent in pericarpium trichosanthis injection and application of chemical constituents |
| CN105669806A (en) * | 2016-03-02 | 2016-06-15 | 上海上药第一生化药业有限公司 | Preparation method and application of chemical component in trichosanthes kirilowii Maxim peel |
| CN110330541A (en) * | 2019-05-22 | 2019-10-15 | 南阳师范学院 | A kind of separation method to 5 '-guanylic acids and 5 '-cytidylic acids |
| CN111603499A (en) * | 2020-05-22 | 2020-09-01 | 甘肃岷海医药科技有限公司 | Traditional Chinese medicine for preventing and treating cancer and preparation method thereof |
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|---|---|---|---|---|
| CN105541944A (en) * | 2016-03-02 | 2016-05-04 | 上海上药第一生化药业有限公司 | Preparation method of chemical components in trichosanthes kirilowii Maxim injection and application of chemical components |
| CN105646628A (en) * | 2016-03-02 | 2016-06-08 | 上海上药第生化药业有限公司 | Method for preparing chemical constituent in pericarpium trichosanthis injection and application of chemical constituents |
| CN105669806A (en) * | 2016-03-02 | 2016-06-15 | 上海上药第一生化药业有限公司 | Preparation method and application of chemical component in trichosanthes kirilowii Maxim peel |
| CN105541944B (en) * | 2016-03-02 | 2017-12-26 | 上海上药第一生化药业有限公司 | The preparation method and its usage of chemical composition in Pericarpium Trichosanthis injection |
| CN110330541A (en) * | 2019-05-22 | 2019-10-15 | 南阳师范学院 | A kind of separation method to 5 '-guanylic acids and 5 '-cytidylic acids |
| CN110330541B (en) * | 2019-05-22 | 2023-03-21 | 南阳师范学院 | Method for separating 5 '-guanine nucleotide and 5' -cytosine nucleotide |
| CN111603499A (en) * | 2020-05-22 | 2020-09-01 | 甘肃岷海医药科技有限公司 | Traditional Chinese medicine for preventing and treating cancer and preparation method thereof |
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