CN101747393B - Method for simultaneously preparing chemical references of icariin, epimedin A, epimedin B and epimedin C - Google Patents
Method for simultaneously preparing chemical references of icariin, epimedin A, epimedin B and epimedin C Download PDFInfo
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- CN101747393B CN101747393B CN2008102298880A CN200810229888A CN101747393B CN 101747393 B CN101747393 B CN 101747393B CN 2008102298880 A CN2008102298880 A CN 2008102298880A CN 200810229888 A CN200810229888 A CN 200810229888A CN 101747393 B CN101747393 B CN 101747393B
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Abstract
The invention relates to a separation preparation method for simultaneously preparing chemical references of icariin, epimedin A, epimedin B and epimedin C, which comprises the following steps: using icariin extracts with the content between 10 percent and 50 percent as raw materials; carrying out primary column separation; using the preparation type high-efficient liquid phase chromatogram as a main separation measure; carrying out two steps of high-efficient liquid phase preparation; and directly concentrating an extracting solution through pressure reduction until the extracting solution is dried to obtain the chemical references of icariin, epimedin A, epimedin B and epimedin C with the purity higher than 98 percent. The invention has the advantages of simple process step, high purity and good color and luster effect, and can realize the large-scale production.
Description
Technical field
The present invention relates to a kind of separation novel preparation method for preparing icarin, epimedin A, B, C chemical reference substance simultaneously.Comprise that mainly post separates enrichment method and performance liquid preparation method removal of impurities fast and refining.The structural formula of four kinds of reference substances is following:
R1 R2 R3
Epimedin A:rha-(1-2) glu glu CH3
Epimedin B:rha-(1-2) xyl glu CH3
Epimedin: rha-(1-2) rha glu CH3
Icariine: rha glu CH3
Background technology
Herba Epimedii (Herba Epimedii) is that China uses one of the longest Chinese medicine, has the effect of kidney-replenishing, strengthening the bones and tendons, wind-damp dispelling.Modern study shows that Herba Epimedii has many-sided pharmacological actions such as osteoporosis, sexual function improving, increase cardiovascular and cerebrovascular blood flow.Icarin is the main active ingredient of Herba Epimedii, also is the assay composition of epimedium herb in 2005 editions NFs of China; And epimedin A, B, C to be the glycosyl of icarin replace analogue and belong to high-content composition (Zhang Huafeng etc., analytical test journal, 2007,26 (2): 198-201 of per mille level; Thank to beautiful equality, herbal medicine, 2007,38 (4): 613-614), therefore, the many index determinings that epimedium herb carried out simultaneously epimedin A, B, C and icarin are significant.But, as the quality control index composition, must there be a large amount of chemical reference substances to provide, at present, except that icarin, rare providing on other three kinds of reference substance markets.For preparing method's research of reference substance, concentrate on mainly at present that (Hu Yunfeng etc., Chinese patent CN200510061251.1 disclosed in 2007 in the separation and purification of icarin and epimedin; Guo Baolin etc., Chinese patent CN2007100002610.5,2007 are open; Wang Xiaochun etc., Chinese patent CN200610101222.5,2007 are open), and the preparation that separates of epimedin A and B is not almost reported.
Summary of the invention
The present invention is on the scale preparation basis of early-stage Study icarin and epimedin; Many-sided researchs such as, target reference substance enriching method research preferred and the exploitation of reference substance refined highly effective liquid phase process through bulk drug; The invention provides a kind of low cost, high performance liquid preparative chromatography method fast; Can prepare purity simultaneously greater than 98% epimedin A, B, C and icarin, and single reference substance preparative-scale can reach the 1g/ month, the accumulative total preparative-scale can reach monthly output 5g reference substance.
For realizing above-mentioned purpose, the technical scheme that the present invention adopts:
The method for preparing icarin, epimedin A, B, C chemical reference substance simultaneously; The icarin extract that with the mass content is 10%-50% is a raw material, separates through preliminary post, and be main separation means with preparative high performance liquid chromatography; Through the performance liquid preparation of two steps; Extracting solution directly is evaporated to do and can obtains purity greater than 98% corresponding reference substance, and scale be each reference substance monthly output 1 gram, totally produces the 5g reference substance per month; Concrete steps are following:
1) preliminary post separates:
Icarin extract water or the dissolving of volumetric concentration 40-80% aqueous ethanolic solution; Resin column or polyamide column separate, the ethanol-water solution gradient elution, and wherein the alcoholic acid volumetric concentration changes from 0%-100%; Collect 20%-80% ethanol elution thing, concentrate drying gets yellow powder I;
2) the first step performance liquid preparation:
Yellow powder I is configured to the need testing solution that concentration is 50～150mg/ml with the dissolving of volumetric concentration 40-80% aqueous ethanolic solution, through 0.45 μ m filtering with microporous membrane; Adopt the high performance liquid preparative chromatography post of column length 10-50cm, diameter 1-10cm to separate; Six-way valve or pump sample introduction; Sampling volume is 1-50ml, is that the methanol-water of 45-60% or acetonitrile-aqueous solution that volumetric concentration is 20-40% are eluent system with the volumetric concentration, and flow rate control is at 10-400ml/min; Online ultraviolet detection is collected the elutriant (stream part 1) that contains epimedin A and B respectively; The elutriant (stream part 2) that contains epimedin and icarin, more than two stream part dry respectively a yellow powder II and yellow powder III;
3) second step performance liquid preparation:
Yellow powder II is that the acetonitrile solution that contains of 20-40% is that eluent system is carried out the performance liquid preparation second time with the volumetric concentration, and all the other conditions are with step 2), the epimedin A that collects purity＞98% respectively flows stream part of the epimedin B of part and purity＞98%.
Yellow powder III is that the acetonitrile solution that contains of 20-40% is that eluent system is carried out the performance liquid preparation second time with the volumetric concentration, and all the other conditions are with step 2), collect purity respectively greater than high-purity stream part of containing epimedin and icarin of 98%;
4) acquisition of target chemical reference substance:
More than four kinds of high-purity stream parts directly be concentrated into to do and can obtain purity greater than 98% corresponding reference substance, it is the glassy yellow powder.
In the aforesaid method, preliminary post separates better with nonpolar macroporous adsorption resin with resin.The filler of performance liquid preparative column is C6, C8 or C18 bonded phase packings, and its particle diameter is 5～20 μ m, the preferred 270nm of ultraviolet detection wavelength, 318nm or 349nm, specifically detect wavelength per sample in target reference substance signal the overload situation and decide.
From Herba Epimedii extract, separate epimedin A, B, C and icarin chemical reference substance with the present invention and have following advantage and progress:
1. the present invention is a separation means with preparation type performance liquid, and separation efficiency is high, can guarantee the purity of reference substance.
2. the present invention carries out preliminary enrichment through the post separation to the target reference substance, adopts two step performance liquid preparing methods to carry out removal of impurities respectively with refining then, and technology is simpler.
3, the performance liquid preparation method of the present invention's development is a fast preparation method, and the single needle disengaging time was fit to the preparation of chemical reference substance in enormous quantities very much between 10-30 minute; Add the recycling of preparation solvent simultaneously, can realize the low cost of batch preparations.
4. the present invention adopts the online detection of UV-detector, and the separation case of each reference substance can directly detect, direct selective collection high purity sample, thus realize the high-recovery of purity under guaranteeing.
In a word, process step of the present invention is simple, purity is high, color and luster is good, and can be mass-produced.
Description of drawings
Fig. 1 is that the HPLC of epimedin A analyzes collection of illustrative plates (270nm), and its integration is reported as follows:
| ?Name | Retention?Time | Area | ％Area | |
| 1 | 2.568 | 251910 | 1.20 | |
| 2 | 3.087 | 13633 | 0.07 | |
| 3 | 3.361 | 1265 | 0.01 | |
| 4 | 3.520 | 54871 | 0.26 | |
| 5 | Epimedin A | 7.038 | 20635806 | 98.47 |
Fig. 2 is that the HPLC of epimedin B analyzes collection of illustrative plates (270nm), and its integration is reported as follows:
| ?Name | Retention?Time | Area | ％Area | |
| 1 | 1.368 | 48442 | 0.18 | |
| 2 | 1.571 | 25759 | 0.09 | |
| 3 | 1.793 | 36112 | 0.13 | |
| 4 | 2.527 | 320702 | 1.18 | |
| 5 | 3.364 | 5271 | 0.02 | |
| 6 | 3.509 | 3416 | 0.01 | |
| 7 | Epimedin B | 7.584 | 26786204 | 98.39 |
Fig. 3 is that the HPLC of epimedin analyzes collection of illustrative plates (270nm), and its integration is reported as follows:
| ?Name | Retention?Time | Area | ％Area | |
| 1 | 2.498 | 210103 | 1.02 | |
| 2 | 3.184 | 4929 | 0.02 | |
| 3 | 3.360 | 9203 | 0.04 | |
| 4 | Epimedin | 8.315 | 20358900 | 98.91 |
Fig. 4 is that the HPLC of icarin (epimedin D) analyzes collection of illustrative plates (270nm), and its integration is reported as follows:
| Name | Retention?Time | Area | ％Area | |
| 1 | 0.615 | 252448 | 0.92 | |
| 2 | 2.554 | 204808 | 0.75 | |
| 3 | Icarin | 10.264 | 26778047 | 98.33 |
Embodiment
Combine embodiment and accompanying drawing that the present invention is explained further details, embodiment only limits to explain the present invention at present, but not to qualification of the present invention.
Embodiment 1
In the present embodiment; With content is that 20% icarin extract is a raw material; Preliminary post separates employing HPD post; The performance liquid preparation is a sorbent material with 10 μ mC18 bonded phase packings, and adopting a certain proportion of methanol-water and acetonitrile-water respectively is eluting solvent, prepares each reference substance through two step performance liquid.Concrete process step is following:
1) preliminary post separates
The icarin extract dissolves with 40% aqueous ethanolic solution, and the HPD-100 resin column separates, and the ethanol-water solution gradient elution is collected 20%-80% ethanol elution thing, and concentrate drying gets yellow powder I.
2) the first step performance liquid preparation
Yellow powder I dissolves with 40% aqueous ethanolic solution, is configured to the need testing solution that concentration is 150mg/ml, through 0.45 μ m filtering with microporous membrane; Preparation type performance liquid column packing brand is the ChromatorexC18 bonded phase packings; Particle diameter is 10 μ m, column length 22cm, diameter 7.5cm; Six-way valve sample introduction, sampling volume are 10ml, are eluent system with 55% methanol-water solution, and flow rate control is at 160ml/min, and online ultraviolet detection is collected the elutriant (stream part 1) that contains epimedin A and B respectively; The elutriant (stream part 2) that contains epimedin and icarin, more than two stream part respectively concentrating under reduced pressure dry yellow powder II and yellow powder III.
3) second step performance liquid preparation
Yellow powder II is that 30% the acetonitrile solution that contains is that eluent system is carried out the performance liquid preparation second time with volumetric concentration, and all the other conditions are with step 2), collect high-purity stream part of containing epimedin A, B respectively.
Yellow powder III with volumetric concentration be 30% the acetonitrile solution that contains be that eluent system is carried out the performance liquid preparation second time, all the other conditions are with step 2), collect high-purity stream part of containing epimedin and icarin respectively.
4) acquisition of each chemical reference substance
Above-mentioned each high-purity stream part directly is concentrated into to do and can obtains purity greater than 98% each corresponding reference substance epimedin A, B, C and icarin (Fig. 1-Fig. 4).
In the present embodiment; With content is that 20% icarin extract is a raw material; Preliminary post separates employing HPD post; The performance liquid preparation is a sorbent material with 10 μ mC18 bonded phase packings, and adopting a certain proportion of methanol-water and acetonitrile-water respectively is eluting solvent, prepares each corresponding reference substance through two step performance liquid.Concrete process step is following:
1) preliminary post separates
The icarin extract dissolves with the aqueous solution, and the HPD-100 resin column separates, and the ethanol-water solution gradient elution is collected 20%-80% ethanol elution thing, and concentrate drying gets yellow powder I.
2) the first step performance liquid preparation
Yellow powder I dissolves with 50% aqueous ethanolic solution, is configured to the need testing solution that concentration is 100mg/ml, through 0.45 μ m filtering with microporous membrane; Preparation type performance liquid column packing brand is the ChromatorexC18 bonded phase packings; Particle diameter is 10 μ m, column length 19cm, diameter 7.5cm; Pump sample introduction, sampling volume are 20ml, are eluent system with 60% methanol-water solution, and flow rate control is at 140ml/min, and online ultraviolet detection is collected the elutriant (stream part 1) that contains epimedin A and B respectively; The elutriant (stream part 2) that contains epimedin and icarin, more than two stream part respectively concentrating under reduced pressure dry yellow powder II and yellow powder III.
3) second step performance liquid preparation
Yellow powder II is that 25% the acetonitrile solution that contains is that eluent system is carried out the performance liquid preparation second time with volumetric concentration, and all the other conditions are with step 2), collect high-purity stream part of containing epimedin A, B respectively.
Yellow powder III with volumetric concentration be 25% the acetonitrile solution that contains be that eluent system is carried out the performance liquid preparation second time, all the other conditions are with step 2), collect high-purity stream part of containing epimedin and icarin respectively.
4) step is with embodiment 1.
In the present embodiment; With content is that 15% icarin extract is a raw material; Preliminary post separates the employing polyamide column; The performance liquid preparation is a sorbent material with 5 μ m C18 bonded phase packings, and adopting a certain proportion of methanol-water and acetonitrile-water respectively is eluting solvent, prepares each corresponding reference substance through two step performance liquid.Concrete process step is following:
1) preliminary post separates
The icarin extract dissolves with 45% aqueous ethanolic solution, and polyamide column separates, and the ethanol-water solution gradient elution is collected 20%-80% ethanol elution thing, and concentrate drying gets yellow powder I.
2) the first step performance liquid preparation
Yellow powder I dissolves with 45% aqueous ethanolic solution, is configured to the need testing solution that concentration is 120mg/ml, through 0.45 μ m filtering with microporous membrane; Preparation type performance liquid column packing brand is the McirosorbC18 bonded phase packings, and particle diameter is 5 μ m; Column length 17cm, diameter 5cm; Six-way valve sample introduction, sampling volume are 8ml, are eluent system with 50-60% methanol-water solution, and flow rate control is at 180ml/min, and online ultraviolet detection is collected the elutriant (stream part 1) that contains epimedin A and B respectively; The elutriant (stream part 2) that contains epimedin and icarin, more than two stream part respectively concentrating under reduced pressure dry yellow powder II and yellow powder III.
3) second step performance liquid preparation
Yellow powder II is that 25% the acetonitrile solution that contains is that eluent system is carried out the performance liquid preparation second time with volumetric concentration, and all the other conditions are with step 2), collect high-purity stream part of containing epimedin A, B respectively.
Yellow powder III with volumetric concentration be 25% the acetonitrile solution that contains be that eluent system is carried out the performance liquid preparation second time, all the other conditions are with step 2), collect high-purity stream part of containing epimedin and icarin respectively.
4) step is with embodiment 1.
Embodiment 4
In the present embodiment; With content is that 25% icarin extract is a raw material; Preliminary post separates the employing polyamide column; The performance liquid preparation is a sorbent material with 5 μ m C18 bonded phase packings, and adopting a certain proportion of methanol-water and acetonitrile-water respectively is eluting solvent, prepares each corresponding reference substance through two step performance liquid.Concrete process step is following:
1) preliminary post separates
The icarin extract dissolves with 40% aqueous ethanolic solution, and polyamide column separates, and the ethanol-water solution gradient elution is collected 20%-80% ethanol elution thing, and concentrate drying gets yellow powder I.
2) the first step performance liquid preparation
Yellow powder I is configured to the need testing solution that concentration is 80mg/ml with the dissolving of 40-80% aqueous ethanolic solution, through 0.45 μ m filtering with microporous membrane; Preparation type performance liquid column packing brand is the McirosorbC18 bonded phase packings, and particle diameter is 5 μ m; Column length 17cm, diameter 5cm; Pump sample introduction, sampling volume are 20ml, are eluent system with 60% methanol-water solution, and flow rate control is at 180ml/min, and online ultraviolet detection is collected the elutriant (stream part 1) that contains epimedin A and B respectively; The elutriant (stream part 2) that contains epimedin and icarin, more than two stream part respectively concentrating under reduced pressure dry yellow powder II and yellow powder III.
3) second step performance liquid preparation
Yellow powder II is that 28% the acetonitrile solution that contains is that eluent system is carried out the performance liquid preparation second time with volumetric concentration, and all the other conditions are with step 2), collect high-purity stream part of containing epimedin A, B respectively.
Yellow powder III with volumetric concentration be 28% the acetonitrile solution that contains be that eluent system is carried out the performance liquid preparation second time, all the other conditions are with step 2), collect high-purity stream part of containing epimedin and icarin respectively.
4) step is with embodiment 1.
Claims (3)
1. the method for preparing icarin, epimedin A, B, C chemical reference substance simultaneously; It is characterized in that: the icarin extract that with the mass content is 10%-50% is a raw material; Separate through preliminary post; With preparative high performance liquid chromatography is main separation means, and through two step performance liquid preparations, extracting solution directly is evaporated to do and can obtains purity greater than 98% corresponding reference substance; Concrete steps are following:
1) preliminary post separates:
Icarin extract water or the dissolving of volumetric concentration 40-80% aqueous ethanolic solution; Resin column or polyamide column separate, the ethanol-water solution gradient elution, and wherein the alcoholic acid volumetric concentration changes from 0%-100%; Collect 20%-80% ethanol elution thing, concentrate drying gets yellow powder I;
2) the first step performance liquid preparation:
Yellow powder I is configured to the need testing solution that concentration is 50～150mg/ml with the dissolving of volumetric concentration 40-80% aqueous ethanolic solution, through 0.45 μ m filtering with microporous membrane; Adopt the high performance liquid preparative chromatography post of column length 10-50cm, diameter 1-10cm to separate; Six-way valve or pump sample introduction, sampling volume is 1-50ml, is that the methanol-water of 45-60% or acetonitrile-aqueous solution that volumetric concentration is 20-40% are eluent system with the volumetric concentration; Flow rate control is at 10-400ml/min; Online ultraviolet detection is collected the elutriant that contains epimedin A and B respectively, and it is stream part 1; The elutriant that contains epimedin and icarin, it is stream parts 2, more than two stream part dry respectively a yellow powder II and yellow powder III;
3) second step performance liquid preparation:
Yellow powder II is that the acetonitrile solution that contains of 20-40% is that eluent system is carried out the performance liquid preparation second time with the volumetric concentration, and all the other conditions are with step 2), the epimedin A that collects purity＞98% respectively flows stream part of the epimedin B of part and purity＞98%.
Yellow powder III is that the acetonitrile solution that contains of 20-40% is that eluent system is carried out the performance liquid preparation second time with the volumetric concentration, and all the other conditions are with step 2), collect purity respectively greater than high-purity stream part of containing epimedin and icarin of 98%;
4) acquisition of target chemical reference substance:
More than four kinds of high-purity stream parts directly be concentrated into to do and can obtain purity greater than 98% corresponding reference substance, it is the glassy yellow powder;
The filler of the preparative column that the process for preparing the first step or the second step performance liquid adopts is C6, C8 or C18 bonded phase packings, and particle diameter is 5-20 μ m.
2. method according to claim 1 is characterized in that: the resin column that column separation process adopts is the non-polar resin post.
3. method according to claim 1 is characterized in that: performance liquid prepares process and adopts online ultraviolet detection, and it detects the preferred 270nm of wavelength, 318nm or 349nm.
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| CN103698454B (en) * | 2013-12-17 | 2017-01-04 | 广西中烟工业有限责任公司 | A kind of measure the detection method of epimedium active constituent in cigarette shreds and main flume thereof |
| CN104910216B (en) * | 2015-03-07 | 2017-11-03 | 宝鸡文理学院 | It is a kind of with preparing liquid phase method while obtaining the separation method of a variety of epimedium flavones |
| CN104788517A (en) * | 2015-04-27 | 2015-07-22 | 汉中天洋生物科技有限责任公司 | Method of using epimedium medicinal material to extract icariin |
| CN109187810B (en) * | 2018-10-29 | 2021-06-08 | 广州白云山陈李济药厂有限公司 | Detection method of traditional Chinese medicine composition for treating rheumatoid arthritis |
| CN111675741A (en) * | 2020-06-23 | 2020-09-18 | 遵义医科大学 | Separation method for simultaneously obtaining four kinds of epimedium rare flavone by using preparative liquid phase method |
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| CN1970566A (en) * | 2006-12-06 | 2007-05-30 | 贵州同济堂制药有限公司 | Epimedin C contrast preparation method and its product |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1970566A (en) * | 2006-12-06 | 2007-05-30 | 贵州同济堂制药有限公司 | Epimedin C contrast preparation method and its product |
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| 王丽霞.淫羊藿药材高效液相色谱指纹图谱及质量评估研究.《中国优秀博硕士学位论文全文数据库(硕士)工程科技I辑》.2006,第2006卷(第3期),第B016-81页. * |
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