CN106621460A - Automatic column chromatography liquid-phase separation method - Google Patents
Automatic column chromatography liquid-phase separation method Download PDFInfo
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- CN106621460A CN106621460A CN201510714644.1A CN201510714644A CN106621460A CN 106621460 A CN106621460 A CN 106621460A CN 201510714644 A CN201510714644 A CN 201510714644A CN 106621460 A CN106621460 A CN 106621460A
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- silica gel
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Abstract
The invention discloses an automatic column chromatography liquid-phase separation method. The method comprises the following steps: an up-and-down open-ended chromatography column moves to the upper part of a piston tunnel, and is fixed with the piston tunnel to form an integrated body; a silica gel metering pot moves to the upper part of a chromatography column, an uniformly stirred chromatography silica gel is arranged in the silica gel metering pot, silica gel is added in the silica gel metering pot; a mixing silica gel metering pot moves to the upper part of the chromatography column, a mixing silica gel of the to-be-separated product is arranged in the mixing silica gel metering pot, the mixing silica gel is added in the chromatography column and is positioned over the chromatography silica gel; the piston tunnel moves to the upper part of the chromatography column and is fixed with the chromatography column and sealed; the to-be-separated product is eluted, so that the to-be-separated product in the chromatography column is layered; an eluant in the chromatography column can be blown out by gas, the chromatography column of the to-be-separated product in the chromatography column is cut from a layering position, and then elution is carried out. The method is rapid and convenient.
Description
Technical field
The present invention relates to a kind of automatic column chromatography liquid phase separation method.
Background technology
At present in chemical purification technical process, usually using column chromatography carries out being separated between product and impurity.Its principle is in chromatographic silica gel to carry out crude product to mix sample, then the filler of chromatographic silica gel is carried out in chromatographic column, the chromatographic silica gel for mixing sample is equably layered on pure silicon glue again, successively eluting and the absorption of eluant, the product for eventually needing to is recycled to take chromatographic column out of by liquid phase eluant and obtain the technical process of sterling.
The shortcoming of the chromatography purification of industrialization at present：1. preparation is cumbersome, it is necessary to carry out cleaning-drying to equipment, then carries out uniform filler；2. need to use substantial amounts of eluant, eluant is highly inflammable and expensive solvent, and reclaim concentration and differ, it is easy to cause to waste and high cost；3. the addition for carrying out eluant for a long time is needed, it is necessary to someone's observation in real time, in case chromatographic column dried liquid stream, causes efficiency low；4. pair material for eluting will carry out real-time monitoring, in case product is flowed into again in impure eluant.Cause chromatography purification failure or efficiency low；6. due to chromatographic silica gel enormous amount, it is impossible to secondary utilization, not only high cost, can also cause than larger pollution to environment.
The content of the invention
It is an object of the invention to provide a kind of, it can solve the disadvantages mentioned above of prior art product.
The present invention is employed the following technical solutions：
A kind of automatic column chromatography liquid phase separation method, comprises the following steps：
The chromatographic column of one upper and lower opening is moved to the top of a piston funnel, and is integrally fixed with the piston funnel；
The metering of one silica gel is filled in the top for moving to the chromatographic column, and silica gel metering filling and is provided with the chromatographic silica gel for stirring, and is to add silica gel in the silica gel metering is filled；
One mixes the metering of sample silica gel fills and moves to the top of the chromatographic column, it is described mix the metering of sample silica gel fill in be provided with product to be separated mix sample silica gel, and the sample silica gel of mixing is added in the chromatographic column and in the top of the chromatographic silica gel；
The top for moving to the chromatographic column of one piston funnel, and fix and seal with the chromatographic column；
Eluting is carried out to product to be separated so that the product to be separated layering in chromatographic column；
The eluant in chromatographic column is blown out with gas；
The chromatographic column of the product to be separated in chromatographic column is cut off from its layering, and carries out eluting.
It is further comprising the steps of；
Another an equal amount of described chromatographic column is entered into piston funnel position, two closed chromatography column in series structures are formed, and piston funnel can be moved freely inside.
Also include：Two chromatographic columns are carried out into displacement cutting, and by piston funnel described in carries out sealing forming new chromatographic column respectively.
Sha Jing is provided with inside the piston funnel.
Eluting is carried out to new chromatographic column with the eluant of big polarity, product flows out, collects the product of the part and concentrate.
The number of plies of the product layering to be separated is three layers.
It is an advantage of the invention that：The present invention using multiple automatons in parallel, such as may be designed as 500ml each, can continuously fill up to 50L silica gel with 10 ~ 100 parallel connections.Fill process is using the uniform filling of nitrogen pressurization.Pressure can be set, complete chromatographic effect is reached；Eluant carries out from top to bottom chromatographic elution after allotment ratio, be typically washed till impurity and product post effect in efficiently separate absorption when, be greatly saved the consumption of eluant.After product scatter in post is imitated, the eluant in chromatographic column is blown away with nitrogen, reach drying purpose.Position of the product absorption in chromatographic column is automatically selected, is accurately cut.Active component is only taken, efficiency is greatly increased.Secondary big polar elution agent is carried out to effective product component carries out eluting.Quickly, it is convenient.Due to short per single post elution time.Therefore the technique can accomplish continuously to draw product, rather than the batch (-type) of primitive technology goes out product.
Description of the drawings
With reference to embodiment and accompanying drawing, the present invention is described in detail, wherein：
Fig. 1 is the structural representation of the present invention.
Specific embodiment
The specific embodiment of the present invention is expanded on further below in conjunction with the accompanying drawings：
A kind of automatic column chromatography liquid phase separation method, comprises the following steps：
The chromatographic column of one upper and lower opening is moved to the top of a piston funnel, and is integrally fixed with the piston funnel；
The metering of one silica gel is filled in the top for moving to the chromatographic column, and silica gel metering filling and is provided with the chromatographic silica gel for stirring, and is to add silica gel in the silica gel metering is filled；
One mixes the metering of sample silica gel fills and moves to the top of the chromatographic column, it is described mix the metering of sample silica gel fill in be provided with product to be separated mix sample silica gel, and the sample silica gel of mixing is added in the chromatographic column and in the top of the chromatographic silica gel；
The top for moving to the chromatographic column of one piston funnel, and fix and seal with the chromatographic column；
Eluting is carried out to product to be separated so that the product to be separated layering in chromatographic column；
The eluant in chromatographic column is blown out with gas；
The chromatographic column of the product to be separated in chromatographic column is cut off from its layering, and carries out eluting.
It is further comprising the steps of；
Another an equal amount of described chromatographic column is entered into piston funnel position, two closed chromatography column in series structures are formed, and piston funnel can be moved freely inside.
Also include：Two chromatographic columns are carried out into displacement cutting, and by piston funnel described in carries out sealing forming new chromatographic column respectively.
Sha Jing is provided with inside the piston funnel.
Eluting is carried out to new chromatographic column with the eluant of big polarity, product flows out, collects the product of the part and concentrate.
The number of plies of the product layering to be separated is three layers.
Embodiment 1：Single clean chromatographic column 1 is run to filling pure silicon glue workshop section, and automatically upper shifting forms the husky crystalline substance piston funnel 2 of a lower bands to device and the open device of chromatographic apparatus 3 in top descends chromatographic silica gel 4 automatically, the uniform packed layer of formation in 1.Blanking is finished, and device enters Ban Yang silicone fillers workshop section, mixes in the device of sample silica gel measuring tank 5 and mixes the automatic blanking of sample silica gel 6, and the just populated upper end of chromatographic silica gel 4 forms uniform packed layer in chromatographic column 1.Blanking finishes the husky brilliant reverse piston funnel 7 of lower mouth band and enters filler upper end in chromatographic column 1, nitrogen 8 is rushed automatically and is compacted.Device enters eluting workshop section, and eluant 9 is entered in chromatographic column by nitrogen 8, and to the sample silica gel 6 of mixing in chromatographic column 1 eluting is carried out, and absorption and again eluting are carried out in chromatographic silica gel 4.The injection eluant time can set according to experimental data, so that product reaches best separation and 10,11,12 layers are formed in post（This three layers is it is assumed that can also form multilamellar）.After eluting layering workshop section completes, using the eluant in nitrogen 8 quickly blowout chromatographic column, eluant almost all is set to leave chromatographic column.Eluant is cleaned out, and another an equal amount of chromatographic column 1 enters the position of piston funnel 2, forms two closed cascaded structures of chromatographic column 1, and piston funnel 2 can be moved freely inside.Piston funnel 2 and piston funnel 7 are displaced downwardly to the upper end of 11 lower end impurity of product 12 in post effect simultaneously, two chromatographic columns 1 carry out displacement cutting, association of piston funnel 2 of another brand-new upper end in chromatographic column 1 is transferred to the lower end of chromatographic column 1 after former cutting, and remaining colloidal silica in chromatographic column 1 and chromatographic column 1 is blocked in sealing.Piston funnel 2 and piston funnel 7 continue to be displaced downwardly to the upper end of 10 lower end product of impurity 11 in post effect, two segmentation chromatographic columns move cutting, the silica gel of product 11 is completely cut another brand-new piston funnel 7 in the chromatographic column 1 of lower end and is entered the upper end of chromatographic column 1 equipped with the silica gel of product 11, fast injection enters the product 11 of big polar elution agent 13. of specified quantitative in chromatographic column 1 now with the outflow chromatographic column of eluant 13 after sealing, collects the portion of product.Concentrate and pure product 11 has been obtained after eluant 13.
Advantages of the present invention：
Packed art is the multiple automatons in parallel of fixed volume, such as may be designed as 500ml each, can continuously fill up to 50L silica gel with 10 ~ 100 parallel connections.Fill process is using the uniform filling of nitrogen pressurization.Pressure can be set, complete chromatographic effect is reached；Eluant carries out from top to bottom chromatographic elution after allotment ratio, be typically washed till impurity and product post effect in efficiently separate absorption when.It is greatly saved the consumption of eluant.After product scatter in post is imitated, the eluant in chromatographic column is blown away with nitrogen, reach drying purpose.Position of the product absorption in chromatographic column is automatically selected, is accurately cut.Active component is only taken, efficiency is greatly increased.Secondary big polar elution agent is carried out to effective product component carries out eluting.Quickly, it is convenient.Due to short per single post elution time.Therefore the technique can accomplish continuously to draw product, rather than the batch (-type) of primitive technology goes out product.
The present invention has following industrial significance：
The industrialization of previous 5 tons the 1st, carries out column chromatography, once need 20 days to 1 month, product could be separated, 5 tons of chromatographic column is divided in the automatic chromatographic column of each 500g now, is altogether 10000, chromatographed according to the device of 100 chromatographic column parallel combinations, each flow process takes around 20 minutes from filler to discharging, the separation that 50kg silica gel column chromatographies can be carried out in namely 20 minutes, 5MT is altogether 100 50kg, that is, needs 100 20 minutes.It is about 36 hours total time.
2nd, because chromatographic column is less, chromatographic effect is better, so the big chromatographic column of a 5MT is separated into into the little chromatographic column of 10000 500g, yield and purity can be much larger than the former.
3rd, the consumption of eluant, due to the silica gel for only using 50kg every time, so eluant ampoule need not be too big, and can be with recycling.So eluant loss is much smaller than the former.
4th, due to whole-course automation control.As long as early stage setting data has no problem.It is main to need technical staff's real-time watch device to run well, without the need for other monitorings.
5th, place uses, and originally the chromatographic column of 5MT may require that the space where 20 square meter areas highly for 15 meters carries out equipment installation, and using new equipment 20 square meter space storage equipments are only needed to.It is so high without the need for floor height.
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc., be should be included within the scope of the present invention.
Claims (6)
1. a kind of automatic column chromatography liquid phase separation method, it is characterised in that comprise the following steps：
The chromatographic column of one upper and lower opening is moved to the top of a piston funnel, and is integrally fixed with the piston funnel；
The metering of one silica gel is filled in the top for moving to the chromatographic column, and silica gel metering filling and is provided with the chromatographic silica gel for stirring, and is to add silica gel in the silica gel metering is filled；
One mixes the metering of sample silica gel fills and moves to the top of the chromatographic column, it is described mix the metering of sample silica gel fill in be provided with product to be separated mix sample silica gel, and the sample silica gel of mixing is added in the chromatographic column and in the top of the chromatographic silica gel；
The top for moving to the chromatographic column of one piston funnel, and fix and seal with the chromatographic column；
Eluting is carried out to product to be separated so that the product to be separated layering in chromatographic column；
The eluant in chromatographic column is blown out with gas；
The chromatographic column of the product to be separated in chromatographic column is cut off from its layering, and carries out eluting.
2. automatic column chromatography liquid phase separation method according to claim 1, it is characterised in that further comprising the steps of；
Another an equal amount of described chromatographic column is entered into piston funnel position, two closed chromatography column in series structures are formed, and piston funnel can be moved freely inside.
3. automatic column chromatography liquid phase separation method according to claim 2, it is characterised in that
Also include：Two chromatographic columns are carried out into displacement cutting, and by piston funnel described in carries out sealing forming new chromatographic column respectively.
4. automatic column chromatography liquid phase separation method according to claim 3, it is characterised in that be provided with Sha Jing inside the piston funnel.
5. automatic column chromatography liquid phase separation method according to claim 4, it is characterised in that carry out eluting to new chromatographic column with the eluant of big polarity, product flows out, collects the product of the part and concentrate.
6. automatic column chromatography liquid phase separation method according to claim 5, it is characterised in that the number of plies of the product layering to be separated is three layers.
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| CN201510714644.1A CN106621460B (en) | 2015-10-29 | 2015-10-29 | A kind of automatic column chromatography liquid phase separation method |
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| CN201510714644.1A CN106621460B (en) | 2015-10-29 | 2015-10-29 | A kind of automatic column chromatography liquid phase separation method |
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| CN106621460A true CN106621460A (en) | 2017-05-10 |
| CN106621460B CN106621460B (en) | 2019-08-09 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6103195A (en) * | 1997-08-08 | 2000-08-15 | Shukla; Ashok K. | Micro-volume spin columns for sample preparation |
| CN101241115A (en) * | 2007-02-08 | 2008-08-13 | 常晓宇 | Highly effective column chromatography and uses thereof |
| JP2012202765A (en) * | 2011-03-24 | 2012-10-22 | Kurita Water Ind Ltd | Column assembly, fluid processing column, and its characteristic measuring method |
| CN104220872A (en) * | 2012-03-30 | 2014-12-17 | 株式会社岛津制作所 | Segmentable container and method of segmenting substance contained in container |
-
2015
- 2015-10-29 CN CN201510714644.1A patent/CN106621460B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6103195A (en) * | 1997-08-08 | 2000-08-15 | Shukla; Ashok K. | Micro-volume spin columns for sample preparation |
| CN101241115A (en) * | 2007-02-08 | 2008-08-13 | 常晓宇 | Highly effective column chromatography and uses thereof |
| JP2012202765A (en) * | 2011-03-24 | 2012-10-22 | Kurita Water Ind Ltd | Column assembly, fluid processing column, and its characteristic measuring method |
| CN104220872A (en) * | 2012-03-30 | 2014-12-17 | 株式会社岛津制作所 | Segmentable container and method of segmenting substance contained in container |
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| CN106621460B (en) | 2019-08-09 |
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Effective date of registration: 20190910 Address after: Room 410, Building No. 1, 199 Jiangkai Road, Pujiang, Minhang District, Shanghai, 20114 Patentee after: Shanghai Yaofeng Intelligent Technology Co., Ltd. Address before: 201114 Shanghai city Minhang District River Road No. 199 Building No. 1 Room 401 Patentee before: Shanghai Zhu Feng Pharmaceutical Technology Co. Ltd. |
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