CN202870047U - Bogus-dynamic two-dimensional liquid chromatography preparation system - Google Patents
Bogus-dynamic two-dimensional liquid chromatography preparation system Download PDFInfo
- Publication number
- CN202870047U CN202870047U CN 201220517278 CN201220517278U CN202870047U CN 202870047 U CN202870047 U CN 202870047U CN 201220517278 CN201220517278 CN 201220517278 CN 201220517278 U CN201220517278 U CN 201220517278U CN 202870047 U CN202870047 U CN 202870047U
- Authority
- CN
- China
- Prior art keywords
- chromatographic column
- liquid chromatography
- dimension
- dimension chromatographic
- dimensional
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Images
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The utility model discloses a bogus-dynamic two-dimensional liquid chromatography preparation system. The bogus-dynamic two-dimensional liquid chromatography preparation system comprises a three-way valve, an infusion system, separating systems and a detector, wherein each separating system comprises a first-dimensional chromatographic column and a second-dimensional chromatographic column; a sample feeding end of the first-dimensional chromatographic column is connected with the infusion system, and a sample discharging end of the first-dimensional chromatographic column is connected with one interface of the three-way valve; a sample feeding end of the second-dimensional chromatographic column is connected with another one interface of the three-way valve; a sample discharging end of the second-dimensional chromatographic column is connected to the detector; and an another joint of the three-way valve is connected to the detector by a pipeline. The bogus-dynamic two-dimensional liquid chromatography preparation system disclosed by the utility model has the advantages that according to the mode, the large sample feeding amount can be guaranteed, simultaneously the separating capability of the system is greatly improved; by the conversion of the three-way valve, the work of the two separating systems can be finished, so that the cost spent on hardware and production is greatly reduced; and the bogus-dynamic two-dimensional liquid chromatography preparation system is wide in application range and is suitable for separation and purification of trace components in complex samples.
Description
Technical field
The utility model relates to the chromatographic separation technology field, specifically relates to a kind of accurate Dynamic Two-dimensional preparative liquid chromatography system.
Background technology
Preparative liquid chromatography is a kind of high efficient separation technology that obtains the pure sample product, it is born in the thirties in 20th century, be applied at first the separation of pigment, so far obtained tremendous development, nowadays be widely used in medical industry, the fields such as separation and purification of protein are such as the separation and purification of secondary class metabolic product, natural products, macromolecular compound and medicinal organism activated protein, biological therapy product and diagnostic reagent that some is important.But relatively separation efficiency is not high with analyzing high performance liquid chromatography for preparative liquid chromatography, can not satisfy the demand of high-purity, high yield.So people endeavour to seek a kind of preparative chromatography pattern of high separating efficiency, reduce production costs, and obtain high-purity sample.Sample size and separation efficiency are two important indicators of liquid phantom preparing chromatogram, and sample size increases, and can reduce separation efficiency.The utility models such as Guan Yafeng the diminishing tapered pole of a kind of internal diameter.The diminishing tapered pole of this internal diameter is selected suitable cone angle, makes the chromatographic band broadening flow pattern near the sieve-like flow pattern, can Effective Raise post effect during its applied sample amount Datong District.But the post that this chromatographic column improves effect is limited, and is unsatisfactory to some complex material separating effects.Someone proposes parabolic chromatographic column and chromatogram ball by improving the post design, with further raising separation efficiency.The two-dimensional liquid chromatography (2D-LC) that two independent chromatographic systems are together in series, the component that in unidimensional system, can not separate fully, might in two-dimentional system, be separated preferably, so the separating power of whole two-dimentional system, systemic resolution, peak capacity have obtained greatly improving than the one dimension chromatographic system.In preparative chromatography, have the people at first to use the off-line two-dimensional model, with sample with the rough segmentation of low pressure preparative liquid chromatography, the eluent of collecting is concentrated after, separate with the middle high-pressure liquid chromatography again.This method complicated operation is wasted time and energy, and wastes a large amount of solvents, and production cost is high.Someone have the people with the standby liquid chromatographic system of basic, normal, high compacting in conjunction with making up online two-dimension preparation liquid chromatographic system, be used for the scale preparation and produce.But online two-dimensional liquid chromatography system needs two preparative liquid chromatography systems, and for single target thing separation and purification in the complex sample, initial investment is too high.
The utility model content
The utility model fundamental purpose provides a kind of accurate Dynamic Two-dimensional preparative liquid chromatography system, and this accurate Dynamic Two-dimensional preparative liquid chromatography system can realize the separation demand of high-purity, high yield, and easy and simple to handle, and financial cost is low.
For achieving the above object, the technical solution adopted in the utility model is: a kind of accurate Dynamic Two-dimensional preparative liquid chromatography system, comprise T-valve, transfusion system, piece-rate system and detecting device, described piece-rate system comprises the first dimension chromatographic column and the second dimension chromatographic column, the sample introduction end of described the first dimension chromatographic column connects described transfusion system, an interface of the sample outlet end connecting tee valve of described the first dimension chromatographic column; An interface of the sample introduction end connecting tee valve of described the second dimension chromatographic column, the sample outlet end of described the second dimension chromatographic column is connected to described detecting device; Another interface of described T-valve is connected to described detecting device by pipeline.
Preferably, what described the first dimension chromatographic column and the second dimension chromatographic column all adopted is chromatograph tower, distributes in detachment process to make things convenient for material.
Preferably, described the first dimension chromatographic column and the second dimension are filled with fixedly phase in the chromatographic column, described fixing be a kind of in polymeric material, silica gel, the in-situ polymerization integral material mutually.The granularity of the fixedly phase in the utility model in the second dimension chromatographic column is not more than the granularity of the fixedly phase in the first dimension chromatographic column.
Further, described the second dimension chromatographic column internal diameter is less than the internal diameter of described the first dimension chromatographic column.
Further, described the second dimension chromatogram column length is longer than the length of described the first dimension chromatographic column.
Further, described detecting device is the ultra-violet analysis detecting device, can efficient detection evaluating objects thing.
Further, described transfusion system comprises two infusion pumps.
Further, described fixing be reverse phase filler, a kind of in phase filling, ion exchange resin filler, volume exclusion filler, whole filler, chirality padding and the affine filler just mutually.
Using method when utilizing a kind of accurate Dynamic Two-dimensional preparative liquid chromatography of the present utility model system to separate detection material, comprise the steps: step 1, at first utilize T-valve that the sample outlet end of the first dimension chromatographic column is linked to each other with detecting device, sample is separated in the first dimension chromatographic column, detected in real time by detecting device; Step 2, when detecting object when the first dimension elutes the chromatographic column, switch three-way valve so that the first dimension chromatographic column is connected with the second dimension chromatographic column, the mode of object by heartcut directly enters second and ties up chromatographic column, carries out wash-out; Step 3, until object enter fully second the dimension chromatographic column after, switch three-way valve, with first the dimension chromatographic column link to each other with detecting device, with rear material wash-out in the object wash-out, and detect; Step 4, switch three-way valve again make the first dimension chromatographic column be connected with the second dimension chromatographic column, and the material in the second dimension chromatographic column is carried out further separation and purification, again by detecting device detect determine after collection.
The beneficial effects of the utility model are: greatly improve system's separating power when the utility model guarantees large sample size; And by the conversion of T-valve, can finish the work of two piece-rate systems, greatly reduce hardware and production cost; Applied range is suitable for the separation and purification of microcomponent in the complex sample.
Description of drawings
Fig. 1 is the structural representation of the accurate Dynamic Two-dimensional preparative liquid chromatography of the utility model system one preferred embodiment;
Fig. 2 is that the HPLC of camellia sample among the utility model embodiment analyzes chromatogram;
Fig. 3 be among the utility model embodiment after the sample separation HPLC of object analyze chromatogram.
Embodiment
Below in conjunction with accompanying drawing preferred embodiment of the present utility model is described in detail, thereby so that advantage of the present utility model and feature can be easier to be it will be appreciated by those skilled in the art that protection domain of the present utility model is made more explicit defining.
Embodiment: see also Fig. 1, a kind of accurate Dynamic Two-dimensional preparative liquid chromatography of the utility model system, comprise T-valve 5, transfusion system 3, piece-rate system and detecting device 4, piece-rate system comprises the first dimension chromatographic column 1 and the second dimension chromatographic column 2, the sample introduction end of the first dimension chromatographic column 1 connects an interface of the sample outlet end connecting tee valve 5 of transfusion system 3, the first dimension chromatographic columns 1; An interface of the sample introduction end connecting tee valve 5 of the second dimension chromatographic column 2, the sample outlet end of the second dimension chromatographic column 2 is connected to detecting device 4; Another interface of T-valve 5 is connected to detecting device 4 by pipeline.
In the present embodiment, what the first dimension chromatographic column 1 and the second dimension chromatographic column 2 all adopted is chromatograph tower, distributes in detachment process to make things convenient for material.
The first dimension chromatographic column 1 and the second dimension are filled with fixedly phase of reverse phase filler in the chromatographic column 2, and the reverse phase filler in the second dimension chromatographic column 2 fixedly the granularity of phase be not more than first and tie up the fixedly granularity of phase of the interior reverse phase filler of chromatographic column 1.Fix and to adopt polymeric material, silica gel, in-situ polymerization integral material etc. according to actual conditions mutually.
In the present embodiment, the first dimension chromatographic column 1 is internal diameter 40mm, the chromatograph tower of long 150mm, and top filling particle diameter is the C18 filler of 50 μ m, the bottom is the C18 filler of particle diameter 25 μ m.The second dimension chromatographic column 2 is internal diameter 25mm, the chromatograph tower of long 300mm, the C18 filler of filling particle diameter 25 μ m.
In the present embodiment, detecting device 4 is the ultra-violet analysis detecting device, can efficient detection evaluating objects thing.
In the present embodiment, transfusion system 3 is comprised of two infusion pumps.
What used fixing of the first dimension chromatographic column 1 and the second dimension chromatographic column 2 mutually can be in reverse phase filler, positive phase filling, ion exchange resin filler, volume exclusion filler, whole filler, chirality padding and the affine filler in the utility model is a kind of.
Further specify performance and the using method thereof of the accurate Dynamic Two-dimensional preparative liquid chromatography of the utility model system below in conjunction with practical operation.
Please refer to Fig. 1, Fig. 2 and Fig. 3, utilize the accurate Dynamic Two-dimensional preparative liquid chromatography of the utility model system to carry out following separation and detect: sample: the camellia extract, object is a low content impurity wherein, former state HPLC analysis chromatogram is as shown in Figure 2.Chromatographic condition: the detection wavelength is 230nm.The HPLC of sample all uses 0.1% trifluoroacetic acid aqueous solution, acetonitrile to be mobile phase, gradient elution when analyzing, utilizing the first dimension chromatographic column 1 to separate with the second dimension chromatographic column 2.HPLC analytic system chromatographic column is SinoChrom ODS-BP (4.6 * 150mm5um).
Operation steps is as follows: at first utilize T-valve 5 that the sample outlet end of the first dimension chromatographic column 1 is connected with detecting device 4, sample is separated in the first dimension chromatographic column 1, detected in real time by detecting device 4; When detecting object when the first dimension elutes the chromatographic column 1, switch three-way valve 5, so that the first dimension chromatographic column 1 is connected with the second dimension chromatographic column 2, the mode of object by heartcut directly enters second and ties up chromatographic column 2, carries out wash-out; After object entered the second dimension chromatographic column 2 fully, switch three-way valve 5 linked to each other the first dimension chromatographic column 1 with detecting device 4, with rear material wash-out in the object wash-out, and detect; Switch three-way valve 5 again, and the first dimension chromatographic column 1 is connected with the second dimension chromatographic column 2, and the material in the second dimension chromatographic column 2 is carried out further separation and purification, detect by detecting device 4 and determine rear the collection.The object of collecting is analyzed with HPLC, spectrogram as shown in Figure 3, the A peak is object among Fig. 3.
Compared with prior art, good effect of the present utility model is:
(1) the utility model organically combines the first dimension chromatographic system and the second dimension chromatographic column by T-valve, complex sample in unidimensional system through the mode by heartcut after the rough segmentation, object is changed in the second dimension chromatographic column, remove most impurity, then carry out further separation and purification, greatly improve system's separating power when guaranteeing large sample size;
(2) the utility model only needs to use after the one dimension piece-rate system T-valve to connect the second dimension chromatographic column, object mode by heartcut after the first dimension is separated can be entered the second dimension piece-rate system, further separation and purification, finish the work of two piece-rate systems, can greatly reduce hardware and production cost;
(3) the first dimension chromatographic column can be filled two kinds of fillers in the utility model, and the bottom is and the identical chromatograph packing material of the second dimension that top is the thicker filler of particle diameter.Therefore, when the second dimension chromatographic column filler when subsiding, the filler of the first dimension chromatographic column middle and lower part can enter the second dimension chromatographic column, and the repairing of realization chromatographic column has the function of accurate dynamic compression post, greatly improves chromatographic column serviceable life; To poorly soluble sample, can tie up chromatographic column top by mixing sample loading mode sample introduction, applied range first simultaneously.
(4) the utility model is simple to operate, easily is automated.Only need switch T-valve three times after the sample introduction, can finish online two dimensional separation;
(5) applied range of the present utility model can be used for separation and purification, the separation and purification of biological sample, the separation of medicine and the separation of chirality sample of natural products, is particularly suitable for the separation and purification of microcomponent in the complex sample.
The above only is embodiment of the present utility model; be not so limit claim of the present utility model; every equivalent structure or equivalent flow process conversion that utilizes the utility model instructions and accompanying drawing content to do; or directly or indirectly be used in other relevant technical fields, all in like manner be included in the scope of patent protection of the present utility model.
Claims (8)
1. accurate Dynamic Two-dimensional preparative liquid chromatography system, comprise T-valve, transfusion system, piece-rate system and detecting device, it is characterized in that, described piece-rate system comprises the first dimension chromatographic column and the second dimension chromatographic column, the sample introduction end of described the first dimension chromatographic column connects described transfusion system, an interface of the sample outlet end connecting tee valve of described the first dimension chromatographic column; An interface of the sample introduction end connecting tee valve of described the second dimension chromatographic column, the sample outlet end of described the second dimension chromatographic column is connected to described detecting device; Another interface of described T-valve is connected to described detecting device by pipeline.
2. a kind of accurate Dynamic Two-dimensional preparative liquid chromatography according to claim 1 system is characterized in that what described the first dimension chromatographic column and the second dimension chromatographic column all adopted is chromatograph tower.
3. according to a kind of accurate Dynamic Two-dimensional preparative liquid chromatography according to claim 1 system, it is characterized in that, described the first dimension chromatographic column and the second dimension are filled with fixedly phase in the chromatographic column, described fixing be a kind of in polymeric material, silica gel, the in-situ polymerization integral material mutually.
4. according to claim 1 and 2 or 3 described a kind of accurate Dynamic Two-dimensional preparative liquid chromatography systems, it is characterized in that described the second dimension chromatographic column internal diameter is less than the internal diameter of described the first dimension chromatographic column.
5. according to claim 1 and 2 or 3 described a kind of accurate Dynamic Two-dimensional preparative liquid chromatography systems, it is characterized in that described the second dimension chromatogram column length is longer than the length of described the first dimension chromatographic column.
6. according to claim 1 and 2 or 3 described a kind of accurate Dynamic Two-dimensional preparative liquid chromatography systems, it is characterized in that described detecting device is the ultra-violet analysis detecting device.
7. according to claim 1 and 2 or 3 described a kind of accurate Dynamic Two-dimensional preparative liquid chromatography systems, it is characterized in that described transfusion system comprises two infusion pumps.
8. according to claim 1 and 2 or 3 described a kind of accurate Dynamic Two-dimensional preparative liquid chromatography systems, it is characterized in that, described fixing be reverse phase filler, a kind of in phase filling, ion exchange resin filler, volume exclusion filler, whole filler, chirality padding and the affine filler just mutually.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220517278 CN202870047U (en) | 2012-10-10 | 2012-10-10 | Bogus-dynamic two-dimensional liquid chromatography preparation system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201220517278 CN202870047U (en) | 2012-10-10 | 2012-10-10 | Bogus-dynamic two-dimensional liquid chromatography preparation system |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN202870047U true CN202870047U (en) | 2013-04-10 |
Family
ID=48036756
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201220517278 Expired - Lifetime CN202870047U (en) | 2012-10-10 | 2012-10-10 | Bogus-dynamic two-dimensional liquid chromatography preparation system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN202870047U (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102914610A (en) * | 2012-10-10 | 2013-02-06 | 苏州汇通色谱分离纯化有限公司 | Dynamic two-dimensional preparative liquid chromatography system and substance separating and purifying method |
| CN103575832A (en) * | 2013-11-13 | 2014-02-12 | 天津中医药大学 | System and method for separating comprehensive two-dimensional liquid chromatography on line |
| CN108226358A (en) * | 2018-03-09 | 2018-06-29 | 山东省分析测试中心 | For the multidimensional counter-current chromatograph and method of work of complex sample multi-cycle separation |
-
2012
- 2012-10-10 CN CN 201220517278 patent/CN202870047U/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102914610A (en) * | 2012-10-10 | 2013-02-06 | 苏州汇通色谱分离纯化有限公司 | Dynamic two-dimensional preparative liquid chromatography system and substance separating and purifying method |
| CN103575832A (en) * | 2013-11-13 | 2014-02-12 | 天津中医药大学 | System and method for separating comprehensive two-dimensional liquid chromatography on line |
| CN103575832B (en) * | 2013-11-13 | 2015-05-20 | 天津中医药大学 | System and method for separating comprehensive two-dimensional liquid chromatography on line |
| CN108226358A (en) * | 2018-03-09 | 2018-06-29 | 山东省分析测试中心 | For the multidimensional counter-current chromatograph and method of work of complex sample multi-cycle separation |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Nováková et al. | Advantages of ultra performance liquid chromatography over high‐performance liquid chromatography: Comparison of different analytical approaches during analysis of diclofenac gel | |
| CN104713973A (en) | Two-dimensional preparative chromatography instrument system having online enrichment function, and applications thereof | |
| CN103884785B (en) | A kind of detection method of selenium | |
| CN202870047U (en) | Bogus-dynamic two-dimensional liquid chromatography preparation system | |
| CN102879498A (en) | Three-section two-dimensional liquid chromatogram system and application method thereof | |
| CN104941611B (en) | The preparation method of graft type high power capacity dendrimer chromatography of ions fixed phase stuffing | |
| CN101791491B (en) | Online low-pressure, middle-pressure and high-pressure combined two-dimension preparation liquid chromatographic system | |
| CN103558320A (en) | Boronic acid affinity monolithic column solid-phase micro-extraction-high performance liquid chromatography on-line combined system | |
| CN103497277A (en) | Baicalein molecularly imprinted polymer, preparation method and application thereof | |
| CN105241984A (en) | Array multi-dimensional liquid-phase chromatographic column system | |
| CN103852531B (en) | Method for detecting malto-oligosaccharide in beer through HPLC-ELSD (High-Performance Liquid Chromatography-Evaporative Light Scattering Detector) | |
| CN202870045U (en) | Three-section type two-dimensional liquid chromatography system | |
| CN102914610B (en) | Dynamic two-dimensional preparative liquid chromatography system and substance separating and purifying method | |
| CN101177499A (en) | Method for preparing estradiol molecular engram polymer | |
| CN103575832B (en) | System and method for separating comprehensive two-dimensional liquid chromatography on line | |
| CN112611825A (en) | Method and device for purifying plant polysaccharide by two-dimensional liquid chromatography | |
| Yang et al. | Application of monolithic stationary phases in solid-phase extraction and pharmaceutical analysis | |
| Connolly et al. | High‐performance separation of small inorganic anions on a methacrylate‐based polymer monolith grafted with [2 (methacryloyloxy) ethyl] trimethylammonium chloride | |
| CN103293262A (en) | Method for detecting tert-butyl hydrazine hydrochloride by using ion chromatography | |
| CN106290603A (en) | A kind of utilize Vavle switching method to detect the inorganic anion in plant, organic acid and the method for three kinds of phytochemicalss and application simultaneously | |
| CN2847290Y (en) | Self colume loading device | |
| CN104849384A (en) | Method for establishing fingerprint spectrum of Jian Ganle preparation | |
| CN104645667A (en) | Expanded bed chromatography and counter-current chromatography on-line combination method, application and apparatus thereof | |
| CN104407088A (en) | Quantitative analysis method for dioscin in compounded traditional Chinese medicine preparation | |
| CN103852542A (en) | Method for detecting complete degradation product of low molecular weight heparin based on post-column derivatization |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term |
Granted publication date: 20130410 |
|
| CX01 | Expiry of patent term |