CN105572266A - Preparation supercritical fluid chromatographic instrument with multi-way valve and separation and purification method of preparation supercritical fluid chromatographic instrument - Google Patents
Preparation supercritical fluid chromatographic instrument with multi-way valve and separation and purification method of preparation supercritical fluid chromatographic instrument Download PDFInfo
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Abstract
The invention provides a preparation supercritical fluid chromatographic instrument with a multi-way valve and a separation and purification method of the preparation supercritical fluid chromatographic instrument. Complicated mixed components to be separated are efficiently separated through on/off switching of the multi-way valve by adopting a separation mode including pre-separation performed by a pre-separation column, capturing performed by a plurality of capturing columns and separation performed by a plurality of main separation columns; the separated components are collected in a collector through the on/off switching of the valve, and a mobile phase without the separated components is returned back to a system for cyclic utilization. The supercritical fluid chromatographic instrument provided by the invention is simple in design, good in separation effect and extremely high in practicability, and is applicable to separation and purification of various types of complicated mixtures.
Description
Technical field
The invention belongs to instrument and equipment manufacturing technology field, particularly relate to and a kind ofly prepare supercritical fluid chromatograph and the method for the preparation of separation and purification with multiport valve.
Background technology
Supercritical fluid chromatography (supercriticalfluidchromatography; SFC) doing mobile phase with supercritical fluid is rely on the solvability of mobile phase to carry out the chromatographic process being separated, analyzing, and is a kind of new technology that the eighties in 20th century, development and improvement got up.
Supercritical fluid is material higher than a kind of state when emergent pressure and critical temperature, it has some character of gas and liquid, there is the features such as the low viscosity of gas, the high density of liquid and coefficient of diffusion higher between gas, liquid, SFC is supplementing of GC and LC, SFC can solve a difficult problem for vapour liquid chromatography, it can analyze the involatile sample of gas chromatography difficulty vaporization, and have the efficiency higher than high performance liquid chromatography, analysis time is shorter simultaneously.At present, supercritical fluid chromatography has developed into the important isolation technics in field widespread uses such as chemistry, life science, pharmacy.
Application publication number CN103376297A(application number 201210114350.1) Chinese invention patent document disclose a kind of supercritical fluid chromatograph and for asymmetric six-way injection valve wherein, by liquefied fluid tank, reduction valve, tensimeter, plate type heat exchanger, liquid CO 2 discharge pump, modifier discharge pump, mixer, automatic sampler, chromatographic column, detecting device, automatic back pressure regulator, pressure transducer, fraction collector forms.Use Novel asymmetric six-way injection valve, adopt the non-decile of rotor, asymmetric design, makes supercritical CO 2 in quantitative loop discharge in advance, in conjunction with non-return valve, realizes the slowly-releasing of supercritical fluid in sample introduction quantitative loop in sample introduction handoff procedure, solves vaporization shock problem.
Common supercritical fluid chromatograph is made up of carbon dioxide steel cylinder, carbon dioxide pump, improver pump, injector, chromatographic column, detecting device, registering instrument etc., and clastotype is that one dimension is separated.But when carrying out sample separation, be difficult to obtain desirable separating effect for complex sample, the purity of the separating obtained product of one dimension is undesirable sometimes, needs to collect after mobile phase is reclaimed in chromatographic fraction and carrying out sub-sampling separation again.In addition, when carrying out sample separation, need to use a large amount of eluents, this also makes separation costs increase.
Summary of the invention
For solving the above-mentioned defect existing for the separation of common supercritical fluid chromatograph, the invention provides and a kind ofly prepare supercritical fluid chromatograph with multiport valve, by the switching over of multiport valve, the clastotype that COMPLEX MIXED component to be separated is separated through the pre-separation of pre-separation post, the trapping of many trapping column, how main separating column is efficiently separated, the component separated is collected at gatherer by the switching over of valve, and the mobile phase not containing separated component gets back to systemic circulation use.
To achieve these goals, the technical solution used in the present invention is:
A kind ofly prepare supercritical fluid chromatograph with multiport valve, be made up of pre-separating system and main piece-rate system, pre-separating system is made up of induction system 1, sampling system Cs, pre-separation post C1, detecting device D1, multiport valve V1, trapping column system C2, multiport valve V2, detecting device D2, counterbalance valve B1; Main piece-rate system is made up of induction system 2, multiport valve V3, trapping column system C2, multiport valve V4, multiport valve V5, separating column system C3, multiport valve V6, detecting device D3, multiport valve V7, fraction collector S, counterbalance valve B2.Induction system 1 is made up of supercritical carbon dioxide discharge pump P1 and improver 1 discharge pump P2, and induction system 2 is made up of supercritical carbon dioxide discharge pump P3 and improver 2 discharge pump P4.
Annexation between each parts is: the outlet of induction system 1 is connected with Cs C1 D1 pipeline, the entrance of multiport valve V1 exports with D1 and is connected, the multiple exit of V1 respectively with the trapping column a in trapping column system C2, b, c, d, e, f is connected, trapping column a, b, c, d, e, f is connected with multiple imports of multiport valve V2 more respectively, the outlet of multiport valve V2 is connected with D2 entrance, D2 outlet is connected with counterbalance valve B1, B1 is connected with induction system 1, form induction system 1 Cs C1 D1 V1 C2(a, b, c, d, e, f) connected mode of V2 D2 B1 induction system 1.The outlet of induction system 2 is connected with the entrance of multiport valve V3, the multiple exit of V3 respectively with the trapping column a in trapping column system C2, b, c, d, e, f is connected, trapping column a, b, c, d, e, f is connected with multiple imports of multiport valve V4 more respectively, the outlet of multiport valve V4 is connected with the entrance of multiport valve V5, multiple outlets of multiport valve V5 respectively with the separating column I in separating column system C3, II, III, the entrance of IV is connected, separating column I, II, III, the outlet of IV is connected with the multiple entry of multiport valve V6 respectively, the outlet of multiport valve V6 is connected with detecting device D3, detecting device D3 outlet is connected with the entrance of the multiport valve V7 in Fraction collection system, the outlet of V7 and fraction collector S-phase connect, fraction collector S outlet is connected with counterbalance valve B2 entrance, B2 outlet is connected with induction system 2 again, form induction system 2 V3 C2(a, b, c, d, e, f) V4 V5 C3(I, II, III, IV) succession of V6 D3 V7 fraction collector S B2 induction system 2.
Above-mentioned supercritical fluid chromatograph, described supercritical carbon dioxide discharge pump P1, P3 can be the constant flow pumps that can provide steady pressure and flow velocity, may also be constant pressure pump etc.Carry fluid not only to comprise supercritical carbon dioxide, also comprise inorganic, the organic solvents such as water, methyl alcohol, ethanol, acetonitrile, sherwood oil, hexane, methylene chloride, ethyl acetate, chloroform.
Above-mentioned supercritical fluid chromatograph, described improver 1 discharge pump P2, improver 2 discharge pump P4 are the constant flow pumps that can provide steady pressure and flow velocity.Carry improver to comprise inorganic, the organic solvents such as water, methyl alcohol, ethanol, acetonitrile, sherwood oil, hexane, methylene chloride, ethyl acetate, chloroform.
Above-mentioned supercritical fluid chromatograph, described sampling system Cs can be sampling valve or sampling pump or the sample introduction post etc. of fixed volume.
Above-mentioned supercritical fluid chromatograph, described pre-separation post C1, trapping column C2, separating column C3 can be glass, stainless steel, PEEK etc.The filler loaded can be normal-phase chromatography filler, reverse-phase chromatography filler, gel filler etc., and the amount of filler can be analytic type, semi-preparative, preparative etc.
Above-mentioned supercritical fluid chromatograph, described multiport valve V1-V7 can be the multidigit multiport valve into having more, and also can be to enter a multidigit multiport valve out more.
Above-mentioned supercritical fluid chromatograph, described detecting device D1, D2, D3 can be the flow-through detector etc. such as UV-detector, fluorescence detector, differential refraction detector; The detection cell of detecting device is high pressure resistant detection cell.
Above-mentioned supercritical fluid chromatograph, described counterbalance valve B1, B2 can be the counterbalance valves that can provide systems stabilisation back pressure, also can be that other can provide the electronic valve device of stable back pressure.
Present invention also offers the described isolation and purification method preparing supercritical fluid chromatograph, step is as follows:
(1) blending ingredients carries out wash-out separation through pre-separating system: carbon dioxide is carried through supercritical carbon dioxide discharge pump P1, improver 1 is carried by improver discharge pump P2, the two converges after mixing through sampling system Cs, sample in carrier band Cs enters pre-separation post C1 and carries out pre-separation, the efflux of pre-separation post C1 enters detecting device D1 and detects, through multiport valve V1, be switched to each trapping column in trapping column system C2 respectively, respective components be caught clustered column trapping, efflux enters detecting device D2 through multiport valve V2, the switching of each trapping column is according to detecting device D1, the combined signal of D2 controls, the pre-separation and the component that complete blending ingredients trap.Now pre-separating system supercritical fluid flowing route is: induction system 1 Cs C1 D1 V1 C2(a, b, c, d, e, f) V2 D2 B1 induction system 1.The change of pre-separating system supercritical fluid composition is controlled by P1, P2 flow velocity or flow proportional.
(2) component be trapped in each trapping column carries out wash-out separation respectively by main piece-rate system: carbon dioxide is carried through supercritical carbon dioxide discharge pump P3, improver 2 is carried by improver discharge pump P4, respectively the component that is captured in each for trapping column system C2 trapping column is entered separating column system C3 through multiport valve V4 with V5 wash-out through multiport valve V3 switching after the two converges mixing to be separated, efflux enters after detecting device D3 detection through multiport valve V6, by the corresponding cut of Fraction collection systematic collection, carbon dioxide recycle uses.Now main piece-rate system supercritical fluid flowing route is: form induction system 2 V3 C2(a, b, c, d, e, f) V4 V5 C3(I, II, III, IV) V6 D3 V7 fraction collector B2 induction system 2.The change of main piece-rate system supercritical fluid composition is controlled by P3, P4 flow velocity or flow proportional.
The present invention is a kind of prepares supercritical fluid chromatograph and the method for the preparation of separation and purification with multiport valve, and Instrument Design is simple, and have superpower separating power, one time loading can obtain multiple monomer component; Supercritical fluid eluent recycles, and cost is low, and practicality is extremely strong.In addition, outstanding effect of the present invention is:
1. the sample of complexity is switched trapping by trapping after pre-separation post is separated, be now separated by main piece-rate system, there is superpower separating power, be suitable for the separation and purification of complex sample.
2. system is provided with 3 detecting devices, can ensure that component trapping switches with collection and accurately control, improve separating effect.
3. trapping column and main piece-rate system separating column can be reported to the leadship after accomplishing a task and be combinationally used, and are applicable to the separation and purification of the extensive polarity ranges of components of polar component from nonpolar to strong, are suitable for sample separation kind more.
4. system is simple, and good separating effect, be applicable to the separation and purification of all kinds of complex mixture, practicality is extremely strong.
Accompanying drawing explanation
Fig. 1 is the structural representation of embodiment of the present invention supercritical fluid chromatograph.
Fig. 2 is that embodiment detecting device D3 outputs signal schematic diagram.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in detail, but protection domain is not by this restriction.
embodimentas shown in Figure 1, a kind ofly prepare supercritical fluid chromatograph with multiport valve, be made up of pre-separating system and main piece-rate system.Pre-separating system is made up of induction system 1, sampling system Cs, pre-separation post C1, detecting device D1, multiport valve V1, trapping column system C2, multiport valve V2, detecting device D2, counterbalance valve B1; Main piece-rate system is made up of induction system 2, multiport valve V3, trapping column system C2, multiport valve V4, multiport valve V5, separating column system C3, multiport valve V6, detecting device D3, multiport valve V7, fraction collector S, counterbalance valve B2.Induction system 1 is made up of supercritical carbon dioxide discharge pump P1 and improver 1 discharge pump P2, and induction system 2 is made up of supercritical carbon dioxide discharge pump P3 and improver 2 discharge pump P4.
The isolation and purification method of supercritical fluid chromatograph is: (1) blending ingredients carries out wash-out separation through pre-separating system: carbon dioxide is carried through supercritical carbon dioxide discharge pump P1, improver 1 is carried by improver discharge pump P2, the two converges after mixing through sampling system Cs, sample in carrier band Cs enters pre-separation post C1 and carries out pre-separation, the efflux of pre-separation post C1 enters detecting device D1 and detects, through multiport valve V1, be switched to each trapping column in trapping column system C2 respectively, respective components be caught clustered column trapping, efflux enters detecting device D2 through multiport valve V2, the switching of each trapping column is according to detecting device D1, the combined signal of D2 controls, the pre-separation and the component that complete blending ingredients trap.Now pre-separating system supercritical fluid flowing route is: induction system 1 Cs C1 D1 V1 C2(a, b, c, d, e, f) V2 D2 B1 induction system 1.The change of pre-separating system supercritical fluid composition is controlled by P1, P2 flow velocity or flow proportional.
(2) component be trapped in each trapping column carries out wash-out separation respectively by main piece-rate system.Carbon dioxide is carried through supercritical carbon dioxide discharge pump P3, improver 2 is carried by improver discharge pump P4, respectively the component that is captured in each for trapping column system C2 trapping column is entered separating column system C3 through multiport valve V4 with V5 wash-out through multiport valve V3 switching after the two converges mixing to be separated, efflux enters after detecting device D3 detection through multiport valve V6, by the corresponding cut of Fraction collection systematic collection, carbon dioxide recycle uses.Now main piece-rate system supercritical fluid flowing route is: form induction system 2 V3 C2(a, b, c, d, e, f) V4 V5 C3(I, II, III, IV) V6 D3 V7 fraction collector S B2 induction system 2.The change of main piece-rate system supercritical fluid composition is controlled by P3, P4 flow velocity or flow proportional.
The present invention a kind of with multiport valve prepare trapping column system trapping column quantity in supercritical fluid chromatograph, separating column systematic position post quantity, multiport valve V port number be not limited only to above-mentioned fixing quantity, also comprises other quantity realizing situation of the present invention.
The present invention a kind of with multiport valve to prepare supercritical fluid chromatograph separating power strong, can complete the separation task that common chromatograph has been difficult to, simultaneously because circulation of supercritical fluid uses, separation costs is low.By above-mentioned connection and mode of operation, composition in the separation and purification red sage root: by above-mentioned connection and mode of operation, pre-separation post C1 diameter 25mm, the stainless steel column of long 200mm, 10mm amino bonded silica filler is loaded in post, 6 trapping column load C-18, C-8, C-4, benzene, CN, amino, glycol bonding silica filler respectively, load C-18, benzene, CN, glycol bonding silica filler in 4 separating columns respectively.Induction system pump 1 transport of carbon dioxide, methyl alcohol carried by pump 2, and carbon dioxide and methyl alcohol adopt graded, and Gradient methods is as follows: 0-30min, and carbon dioxide flow ratio becomes 70% from 100%, and methanol flow ratio becomes 30% from 0.According to detecting device D1 detection signal, eluting fraction is trapped in different trapping column.Induction system pump 3 transport of carbon dioxide, ethanol carried by pump 4, carbon dioxide and ethanol adopt graded, Gradient methods is as follows: 0-60min, and carbon dioxide flow ratio becomes 20% from 100%, and ethanol flow proportional becomes 20% from 0, respectively the composition in trapping column is eluted to separating column to be separated, detecting device D3 detects separating column efflux, collects each cut according to D3 signal, obtains each component.Fig. 2 is for be separated red sage root ethyl acetate extract, and detecting device D3 recording of output signals in detachment process, according to signal collection, first separation can obtain 12 compositions, and its purity measures all higher than 98% through HPLC.Determine that these 12 compositions are: tanshinone IIA, miltionone, new przewaquinone A, salvia miltiorrhiza bge I through Modern spectroscopy analysis, dihydrotanshinone Ⅰ, Dihydroisotanshinone Ⅰ, Cryptotanshinone, hydroxy tanshinone IIA, methylene red sage root quinone, methyl tanshinonate, red sage root quinone B, removes first tanshinone.
Finally it should be noted that, embodiment is the embodiment of optimum of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in previous embodiment, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. prepare supercritical fluid chromatograph with multiport valve for one kind, be made up of pre-separating system and main piece-rate system, it is characterized in that, pre-separating system is made up of induction system 1, sampling system Cs, pre-separation post C1, detecting device D1, multiport valve V1, trapping column system C2, multiport valve V2, detecting device D2, counterbalance valve B1; Main piece-rate system is made up of induction system 2, multiport valve V3, trapping column system C2, multiport valve V4, multiport valve V5, separating column system C3, multiport valve V6, detecting device D3, multiport valve V7, fraction collector S, counterbalance valve B2; Induction system 1 is made up of supercritical carbon dioxide discharge pump P1 and improver 1 discharge pump P2, and induction system 2 is made up of supercritical carbon dioxide discharge pump P3 and improver 2 discharge pump P4; The outlet of induction system 1 is connected with Cs C1 D1 pipeline, the entrance of multiport valve V1 exports with D1 and is connected, the multiple exit of V1 is connected with the trapping column a in trapping column system C2, b, c, d, e, f respectively, trapping column a, b, c, d, e, f are connected with multiple imports of multiport valve V2 more respectively, the outlet of multiport valve V2 is connected with D2 entrance, D2 outlet is connected with counterbalance valve B1, B1 is connected with induction system 1, forms the connected mode of induction system 1 Cs C1 D1 V1 C2(a, b, c, d, e, f) V2 D2 B1 induction system 1.
2. the outlet of induction system 2 is connected with the entrance of multiport valve V3, the multiple exit of V3 respectively with the trapping column a in trapping column system C2, b, c, d, e, f is connected, trapping column a, b, c, d, e, f is connected with multiple imports of multiport valve V4 more respectively, the outlet of multiport valve V4 is connected with the entrance of multiport valve V5, multiple outlets of multiport valve V5 respectively with the separating column I in separating column system C3, II, III, the entrance of IV is connected, separating column I, II, III, the outlet of IV is connected with the multiple entry of multiport valve V6 respectively, the outlet of multiport valve V6 is connected with detecting device D3, detecting device D3 outlet is connected with the entrance of the multiport valve V7 in Fraction collection system, the outlet of V7 and fraction collector S-phase connect, fraction collector S outlet is connected with counterbalance valve B2 entrance, B2 outlet is connected with induction system 2 again, form induction system 2 V3 C2(a, b, c, d, e, f) V4 V5 C3(I, II, III, IV) succession of V6 D3 V7 fraction collector S B2 induction system 2.
3. a kind ofly prepare supercritical fluid chromatograph with multiport valve as claimed in claim 1, it is characterized in that, described supercritical carbon dioxide discharge pump P1, P3 can be the constant flow pumps that can provide steady pressure and flow velocity, may also be constant pressure pump etc.; Carry fluid not only to comprise supercritical carbon dioxide, also comprise inorganic, the organic solvents such as water, methyl alcohol, ethanol, acetonitrile, sherwood oil, hexane, methylene chloride, ethyl acetate, chloroform.
4. a kind ofly prepare supercritical fluid chromatograph with multiport valve as claimed in claim 1, it is characterized in that, described improver 1 discharge pump P2, improver 2 discharge pump P4 are the constant flow pumps that can provide steady pressure and flow velocity; Carry improver to comprise inorganic, the organic solvents such as water, methyl alcohol, ethanol, acetonitrile, sherwood oil, hexane, methylene chloride, ethyl acetate, chloroform.
5. a kind ofly prepare supercritical fluid chromatograph with multiport valve as claimed in claim 1, it is characterized in that, described sampling system Cs can be sampling valve or sampling pump or the sample introduction post etc. of fixed volume.
6. a kind ofly prepare supercritical fluid chromatograph with multiport valve as claimed in claim 1, it is characterized in that, described pre-separation post C1, trapping column C2, separating column C3 can be glass, stainless steel, PEEK etc.; The filler loaded can be normal-phase chromatography filler, reverse-phase chromatography filler, gel filler etc., and the amount of filler can be analytic type, semi-preparative, preparative etc.
7. a kind ofly prepare supercritical fluid chromatograph with multiport valve as claimed in claim 1, it is characterized in that, described multiport valve V1-V7 can be the multidigit multiport valve into having more, and also can be enter a multidigit multiport valve out more.
8. a kind ofly prepare supercritical fluid chromatograph with multiport valve as claimed in claim 1, it is characterized in that, described detecting device D1, D2, D3 can be the flow-through detector etc. such as UV-detector, fluorescence detector, differential refraction detector; The detection cell of detecting device is high pressure resistant detection cell.
9. a kind ofly prepare supercritical fluid chromatograph with multiport valve as claimed in claim 1, it is characterized in that, described counterbalance valve B1, B2 can be the counterbalance valves that can provide systems stabilisation back pressure, also can be that other can provide the electronic valve device of stable back pressure.
10. a kind of isolation and purification method preparing supercritical fluid chromatograph with multiport valve as claimed in claim 1, it is characterized in that, step is as follows:
(1) blending ingredients carries out wash-out separation through pre-separating system: carbon dioxide is carried through supercritical carbon dioxide discharge pump P1, improver 1 is carried by improver discharge pump P2, the two converges after mixing through sampling system Cs, sample in carrier band Cs enters pre-separation post C1 and carries out pre-separation, the efflux of pre-separation post C1 enters detecting device D1 and detects, through multiport valve V1, be switched to each trapping column in trapping column system C2 respectively, respective components be caught clustered column trapping, efflux enters detecting device D2 through multiport valve V2, the switching of each trapping column is according to detecting device D1, the combined signal of D2 controls, the pre-separation and the component that complete blending ingredients trap, now pre-separating system supercritical fluid flowing route is: induction system 1 Cs C1 D1 V1 C2(a, b, c, d, e, f) V2 D2 B1 induction system 1, the change of pre-separating system supercritical fluid composition is controlled by P1, P2 flow velocity or flow proportional,
(2) component be trapped in each trapping column carries out wash-out separation respectively by main piece-rate system: carbon dioxide is carried through supercritical carbon dioxide discharge pump P3, improver 2 is carried by improver discharge pump P4, respectively the component that is captured in each for trapping column system C2 trapping column is entered separating column system C3 through multiport valve V4 with V5 wash-out through multiport valve V3 switching after the two converges mixing to be separated, efflux enters after detecting device D3 detection through multiport valve V6, by the corresponding cut of Fraction collection systematic collection, carbon dioxide recycle uses; Now main piece-rate system supercritical fluid flowing route is: form induction system 2 V3 C2(a, b, c, d, e, f) V4 V5 C3(I, II, III, IV) V6 D3 V7 fraction collector S B2 induction system 2; The change of main piece-rate system supercritical fluid composition is controlled by P3, P4 flow velocity or flow proportional.
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| CN109416349A (en) * | 2016-07-06 | 2019-03-01 | 株式会社岛津制作所 | Preparative liquid chromatography instrument |
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| CN107121504A (en) * | 2017-04-12 | 2017-09-01 | 岛津企业管理（中国）有限公司 | Multi-functional temperature-pressure extraction trapping chromatographic isolation on-line coupling equipment |
| WO2018188184A1 (en) * | 2017-04-12 | 2018-10-18 | 岛津企业管理（中国）有限公司 | Multifunctional on-line combination device for temperature and pressue increase-assisted extraction, trapping, and chromatographic separation |
| CN107121504B (en) * | 2017-04-12 | 2019-08-20 | 岛津企业管理（中国）有限公司 | Multi-functional temperature-pressure extraction-trapping-chromatographic isolation on-line coupling equipment |
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