CN107543870A - Semi-preparative supercritical fluid chromatograph - Google Patents
Semi-preparative supercritical fluid chromatograph Download PDFInfo
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- CN107543870A CN107543870A CN201610486745.2A CN201610486745A CN107543870A CN 107543870 A CN107543870 A CN 107543870A CN 201610486745 A CN201610486745 A CN 201610486745A CN 107543870 A CN107543870 A CN 107543870A
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- back pressure
- delivery pump
- liquid
- supercritical fluid
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- 239000012530 fluid Substances 0.000 title claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 230000003068 static effect Effects 0.000 claims abstract description 8
- 238000005057 refrigeration Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000007689 inspection Methods 0.000 claims 1
- 238000010923 batch production Methods 0.000 abstract description 3
- 238000011020 pilot scale process Methods 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 16
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 4
- 238000004808 supercritical fluid chromatography Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000033228 biological regulation Effects 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 230000005526 G1 to G0 transition Effects 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 150000002605 large molecules Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Abstract
The invention discloses a kind of semi-preparative supercritical fluid chromatograph.By three components, two-stage refrigeration cooling device, liquid CO2Delivery pump, entrainer delivery pump, static mixer, post position switching valve, column oven, chromatographic column, UV detectors, pressure sensor, two-stage back pressure regulator device, component collection device and host computer composition.The instrument can be used for pilot scale stage and the batch production of the products such as biological medicine.
Description
Technical field
The present invention relates to a kind of supercritical fluid chromatograph, belong to chromatographic field.
Background technology
Supercritical fluid chromatography (supercritical fluid chromatography, abbreviation SFC) is with overcritical
Fluid (a kind of state of material when higher than critical pressure and critical-temperature, have the low viscosity of gas, the high density of liquid with
And the feature such as higher diffusion coefficient between air-liquid) it is mobile phase, solid absorbent or the high polymer being bonded on carrier
For the chromatogram of stationary phase.Compared with common liquid chromatogram, mobile phase is generally the mixture of carbon dioxide and organic solvent, super to face
Boundary's Fluid Chromatography uses carbon dioxide and organic solvent（Methanol etc.）Mixture.It not only can segregation gas chromatography difficult separation
Thermally labile, relative molecular mass are higher, highly polar or non-volatile compounds, and can separate high performance liquid chromatography and be difficult to
The high-molecular weight compounds of separation, while the activity of target compound can be kept in preparation process is separated well, compared with it
It is carbon dioxide that his separation method, which has unrivaled advantage, the especially supercritical fluid used in it, with Traditional liquid phase ratio
Compared with caused Discarded organic solvent is few, and pollution is small, more environmentally friendly.
Although supercritical fluid chromatograph device is with a wide range of applications in chromatographic field, current supercritical fluid
Chromatographic apparatus is mainly based on analytic type instrument, applied to the separating-purifying of laboratory low dose sample and opening for experimental method
Hair, lack the supercritical fluid chromatograph device for being applied to pilot scale stage and batch production, therefore, develop it is a kind of efficiently, environmental protection and
The semi-preparative supercritical fluid chromatograph device of safety, turn into the target pursued in Supercritical fluid chromatography research.
The content of the invention
It is an object of the invention to：Develop a kind of semi-preparative supercritical fluid chromatograph device, applied to the pilot scale stage and
Batch production.
Technical scheme is as follows：
A kind of semi-preparative supercritical fluid chromatograph device is by three components 1, two-stage refrigeration cooling device 2, liquid CO2Delivery pump
3rd, entrainer delivery pump 4, static mixer 5, post position switching valve 6, column oven 7, chromatographic column 8, UV detectors 9, pressure sensor
10th, two-stage back pressure regulator device 11, component collection device 12 and host computer 13 form；Three components 1, two-stage refrigeration cooling device
2 and liquid CO2Delivery pump 3 is linked in sequence by pipeline, and entrainer delivery pump 4 passes through pipeline and liquid CO2Delivery pump 3 is in parallel,
Static mixer 5, post position switching valve 6, column oven 7, chromatographic column 8, UV detectors 9, pressure sensor 10, two-stage backpressure regulation dress
Put 11 and component collection device 12 be connected by pipeline order；It is characterized in that the diameter range of chromatographic column be 10cm ~
100cm；Two-stage back pressure regulator device 11 is made up of the automatic back pressure regulating valve 14 of one-level and two-stage hand back pressure regulating valve 15.
Three linked piece 1 is used for showing CO2Pressure of storage tank, regulation gas output and filtering gaseous impurity, two-stage refrigerating plant 2 are used for
By CO2It is cooled to liquid；CO2Delivery pump 3 is used to convey CO2Liquid, entrainer delivery pump 4 is used for conveyer gripping belt agent, static
Blender 5 is used for liquid CO2Phase is closed with entrainer；Post position switching valve 6 is used to inject product to be separated in chromatographic column 8,
UV detectors 9 are used to detect the material in the mobile phase for flowing through chromatographic column；Pressure sensor 10 is used to measure loine pressure, two-stage
The pressure that back pressure regulator device 11 is used for instrument is adjusted, and component collection device 12 is used to collect separation component, and host computer 13 is used for
Control semi-preparative supercritical fluid chromatograph device.
The present invention can reach disposable from multicomponent system by the design of semi-preparative supercritical fluid chromatograph device
The separation of batch obtains one of which target compound, and the lot splitting that the instrument is used for compound purifies, and can bring obvious
Economic and social benefit.
Brief description of the drawings
Fig. 1 is the structural representation of the present invention.
As shown in the figure：
1st, three component
2nd, two-stage refrigeration cooling device
3rd, liquid CO2Delivery pump
4th, entrainer delivery pump
5th, static mixer
6th, post position switching valve
7th, column oven
8th, chromatographic column
9th, UV detectors
10th, pressure sensor
11st, two-stage back pressure regulator device
12nd, component collection device
13rd, host computer
14th, the automatic back pressure regulating valve of one-level
15th, two-stage hand back pressure regulating valve.
Embodiment
Illustrate the embodiment of the present invention with reference to accompanying drawing 1.CO2Gas is after storage tank outflow, by three linked piece 1, three
Join part 1 and show outlet pressure, adjust CO2Go out gas velocity, while filter out objectionable impurities, pure CO2Gas passes through by host computer 13
It is changed into CO after the cooling down of the two-stage refrigeration cooling device 2 of control2Liquid, by CO2Delivery pump 3 conveys, with entrainer delivery pump
The modifying agent of 4 conveyings carries out conjunction phase in static mixer 5, closes point of the gas-liquid mixed material after phase by post position switching valve 6
To match somebody with somebody, into column oven 7, above-critical state is formed after heating, chromatographic column 8 elutes to above-critical state material, after elution
To component materials separated and detected into UV detectors 9, pressure sensor 10 is by the entrance of above-critical state component materials
Pressure value feeds back to host computer 13, and under the control of host computer 13, the component after separation passes through the regulation of two-stage back pressure apparatus 11
And stably, it is collected by component collection device 12.
The technological thought of above example only to illustrate the invention, it is impossible to protection scope of the present invention is limited with this, it is all
It is any change for being done on the basis of technical scheme according to technological thought proposed by the present invention, each falls within protection of the present invention
Within the scope of.
Claims (1)
- A kind of 1. semi-preparative supercritical fluid chromatograph, by three components（1）, two-stage refrigeration cooling device（2）, liquid CO2It is defeated Send pump（3）, entrainer delivery pump（4）, static mixer（5）, post position switching valve（6）, column oven（7）, chromatographic column（8）, UV inspection Survey device（9）, pressure sensor（10）, two-stage back pressure regulator device（11）, component collection device（12）And host computer（13）Composition； Three components（1）, two-stage refrigeration cooling device（2）With liquid CO2Delivery pump（3）It is linked in sequence by pipeline, entrainer conveying Pump（4）Pass through pipeline and liquid CO2Delivery pump（3）It is in parallel, static mixer（5）, post position switching valve（6）, column oven（7）、 Chromatographic column（8）, UV detectors（9）, pressure sensor（10）, two-stage back pressure regulator device（11）And component collection device（12）It is logical Piping order is connected；It is characterized in that the diameter range of chromatographic column is 10cm ~ 100cm；Two-stage back pressure regulator device（11） By the automatic back pressure regulating valve of one-level（14）With two-stage hand back pressure regulating valve（15）Composition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610486745.2A CN107543870A (en) | 2016-06-29 | 2016-06-29 | Semi-preparative supercritical fluid chromatograph |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610486745.2A CN107543870A (en) | 2016-06-29 | 2016-06-29 | Semi-preparative supercritical fluid chromatograph |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107543870A true CN107543870A (en) | 2018-01-05 |
Family
ID=60962663
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610486745.2A Pending CN107543870A (en) | 2016-06-29 | 2016-06-29 | Semi-preparative supercritical fluid chromatograph |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107543870A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109406694A (en) * | 2018-12-19 | 2019-03-01 | 江苏汉邦科技有限公司 | A kind of chromatographic column temperature control device for supercritical fluid chromatography system |
| CN110201420A (en) * | 2019-06-27 | 2019-09-06 | 上海渔霁生物技术有限公司 | A kind of chromatographic system and method separating organic acid and organic acid esters |
| CN117130297A (en) * | 2023-10-25 | 2023-11-28 | 北京豪思生物科技股份有限公司 | Upper computer control method, device and equipment of liquid chromatograph |
Citations (6)
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|---|---|---|---|---|
| US5719302A (en) * | 1993-04-29 | 1998-02-17 | Pronova A.S | Processes for chromatographic fractionation of fatty acids and their derivatives |
| US20090049891A1 (en) * | 2005-02-25 | 2009-02-26 | Mohamed Shaimi | Supercritical-Phase Mixed Chromatography Method and Installation for Implementing Same |
| CN103788146A (en) * | 2012-11-01 | 2014-05-14 | 江苏汉邦科技有限公司 | SFC separation and purification method for preparing salidroside |
| CN103804171A (en) * | 2014-02-25 | 2014-05-21 | 国家海洋局第三海洋研究所 | Preparation method and device for polyenoic acid and ester monomer thereof |
| CN104275767A (en) * | 2013-07-12 | 2015-01-14 | 宁波大学 | Supercritical fluid conveying device |
| CN205720119U (en) * | 2016-06-29 | 2016-11-23 | 江苏汉邦科技有限公司 | Semi-preparative supercritical fluid chromatograph |
-
2016
- 2016-06-29 CN CN201610486745.2A patent/CN107543870A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5719302A (en) * | 1993-04-29 | 1998-02-17 | Pronova A.S | Processes for chromatographic fractionation of fatty acids and their derivatives |
| US20090049891A1 (en) * | 2005-02-25 | 2009-02-26 | Mohamed Shaimi | Supercritical-Phase Mixed Chromatography Method and Installation for Implementing Same |
| CN103788146A (en) * | 2012-11-01 | 2014-05-14 | 江苏汉邦科技有限公司 | SFC separation and purification method for preparing salidroside |
| CN104275767A (en) * | 2013-07-12 | 2015-01-14 | 宁波大学 | Supercritical fluid conveying device |
| CN103804171A (en) * | 2014-02-25 | 2014-05-21 | 国家海洋局第三海洋研究所 | Preparation method and device for polyenoic acid and ester monomer thereof |
| CN205720119U (en) * | 2016-06-29 | 2016-11-23 | 江苏汉邦科技有限公司 | Semi-preparative supercritical fluid chromatograph |
Non-Patent Citations (3)
| Title |
|---|
| C. BERGER ET AL: "Preparative supercritical fluid chromatography", vol. 505, pages 37 - 43, XP026476032, DOI: 10.1016/S0021-9673(01)93067-5 * |
| MARTIN ENMARK DENNIS ET AL: "Evaluation of Scale-up From Analytical to Preparative Supercritical Fluid Chromatography", vol. 1425, pages 280 - 286, XP029334549, DOI: 10.1016/j.chroma.2015.11.001 * |
| WATERS: "Prep 15 SFC System System Guide", 715004396 REV. A, pages 21 - 38 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109406694A (en) * | 2018-12-19 | 2019-03-01 | 江苏汉邦科技有限公司 | A kind of chromatographic column temperature control device for supercritical fluid chromatography system |
| CN110201420A (en) * | 2019-06-27 | 2019-09-06 | 上海渔霁生物技术有限公司 | A kind of chromatographic system and method separating organic acid and organic acid esters |
| CN117130297A (en) * | 2023-10-25 | 2023-11-28 | 北京豪思生物科技股份有限公司 | Upper computer control method, device and equipment of liquid chromatograph |
| CN117130297B (en) * | 2023-10-25 | 2023-12-29 | 北京豪思生物科技股份有限公司 | Upper computer control method, device and equipment of liquid chromatograph |
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Address after: 223005 no.1-9 Jixian Road, Huaian Economic and Technological Development Zone, Jiangsu Province Applicant after: Jiangsu Hanbang Technology Co.,Ltd. Address before: 223005 no.1-9 Jixian Road, Huaian Economic and Technological Development Zone, Jiangsu Province Applicant before: JIANGSU HANBON SCIENCE & TECHNOLOGY Co.,Ltd. |