CN101637665B - Method for combined use of accelerated solvent extraction and high speed countercurrent chromatogram and device thereof - Google Patents
Method for combined use of accelerated solvent extraction and high speed countercurrent chromatogram and device thereof Download PDFInfo
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- CN101637665B CN101637665B CN2009100365442A CN200910036544A CN101637665B CN 101637665 B CN101637665 B CN 101637665B CN 2009100365442 A CN2009100365442 A CN 2009100365442A CN 200910036544 A CN200910036544 A CN 200910036544A CN 101637665 B CN101637665 B CN 101637665B
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Abstract
The invention discloses a method for the combined use of accelerated solvent extraction and high speed countercurrent chromatogram and a device thereof. An accelerated solvent extraction device extracts a material so as to obtain an extraction liquid which is collected by a liquid storage bottle. The extraction liquid is pumped by a peristaltic pump into a dosing ring. Stationary phase in the liquid storage bottle is pumped by a plunger pump into a high speed countercurrent chromatography. The high speed countercurrent chromatography is started, and simultaneously the plunger pump is used for pumping flowing phase in the liquid storage bottle into the high speed countercurrent chromatography for purpose of solvent system balance. Sample solution in the dosing ring is pumped into the high speed countercurrent chromatography. A preparing-type high speed countercurrent chromatogram is used for purification and preparation so as to obtain a target component, or an analysis-type high speed countercurrent chromatogram is used for analyzing the target component in a natural product extract liquid. The above steps are integrated with the accelerated solvent extraction and the high speed countercurrent chromatogram by utilizing a switch valve, thereby realizing the online extraction, separation, purification and preparation of the natural product effective component and having the advantages of fastness, high efficiency and high automation. The method and the device have a wide application prospect in the fields such as food, medicine, biology and the like.
Description
Technical field
The present invention relates to a kind of accelerated solvent extraction-high speed adverse current chromatogram (ASE-HSCCC) method for combined use; And accelerated solvent extraction-high speed adverse current chromatograph joint used device of implementing this method, be applicable to extraction separation, purifying preparation or the analysis of field target components such as food, medicine, biology.
Background technology
It is loaded down with trivial details consuming time that the natural product extraction isolation and purification of tradition off-line prepares process, is prone to cause the loss of target components, and the recovery rate and the rate of recovery are low.Accelerated solvent extraction (ASE) is to increase material solubility and solute diffusion rate through improving temperature with enhancing pressure; Thereby improve a kind of abstraction technique of extraction efficiency; It has saving time, consume that solvent is few, recovery rate is high and be easy to advantage such as automation, and the extraction that is fit to active ingredient in the natural materials separates.
High speed adverse current chromatogram (HSCCC) is a kind of liquid luquid partition chromatography separation and preparation technology of continuous high-efficient; Realization separates according to the distribution coefficient of material in two mutual immiscible liquids is different for it; Do not need solid carrier; Avoided because of problems such as separated material loss that Irreversible Adsorption causes, inactivation, sex change sample all being reclaimed, the sample of recovery more can reflect its original characteristic; And, make the preparation amount of sample improve greatly owing to can fully contact between separated material and the stationary liquid phase.According to the effective difference of splitter volume, high performance countercurrent chromatography mainly comprises two kinds on analytic type and preparation type.Wherein, analytic type has the advantages that the target components separating rate is fast, separation purity is high; The preparation type then has advantages such as the purifying ability is strong, preparation amount is big, applied widely.
Although accelerated solvent extraction and high speed adverse current chromatogram are widely used in natural products, food, medicine and other fields respectively at present; But; The defective that accelerated solvent extraction exists is that the utilization rate of sample is low; And also there is certain defective in the independent application of high speed adverse current chromatogram, and both still are in the independent studies state.
Summary of the invention
The objective of the invention is to; Overcome the defective of the natural product extraction isolation and purification preparation existence of existing off-line, and a kind of novel accelerated solvent extraction-high speed adverse current chromatograph joint used method is provided, technical problem to be solved is to make it can effectively reduce operating procedure; Shorten extraction time; Reduce sample loss, improve product yield, thereby be suitable for practicality more.
Another object of the present invention provide a kind of rapidly and efficiently integrate extract to separate, purifying preparation or adding of analyzing
The object of the invention and solve its technical problem and adopt following technical scheme to realize.According to a kind of accelerated solvent extraction-high speed adverse current chromatograph joint used method that the present invention proposes, it may further comprise the steps: adopt accelerated solvent extraction to follow the example of the extract material and obtain extract; Adopt the countercurrent chromatography purifying to prepare extract and obtain target components, or adopt the analytic type high speed adverse current chromatogram to analyze the target components in the natural product extraction liquid.
The object of the invention and solve its technical problem and also can adopt following technical measures further to realize.
According to the method for combined use of the embodiment of the invention, it also comprises step: 1) accelerated solvent extraction is followed the example of the extract employing liquid storage bottle collection that the extract material obtains; 2) through peristaltic pump the extract in the liquid storage bottle is pumped into quantifying ring; 3) adopt plunger displacement pump with the fixing high-speed counter-current chromatograph that pumps into mutually in the liquid storage bottle, start high-speed counter-current chromatograph, with plunger displacement pump the flowing phase in the liquid storage bottle is pumped into high-speed counter-current chromatograph simultaneously, carry out the dicyandiamide solution balance; 4) after high speed adverse current chromatogram dicyandiamide solution balance is set up, the sample solution in the quantifying ring is pumped into high speed adverse current chromatogram carry out separation and purification preparation or analysis; Above-mentioned steps through the integrated accelerated solvent extraction of transfer valve and high speed adverse current chromatogram in one, realize active ingredient of natural product in preparation of line drawing isolation and purification or analysis.
According to the method for combined use of the embodiment of the invention, wherein to adopt volume ratio be 1: 2: 1 to the dicyandiamide solution of high speed adverse current chromatogram: 2 n-hexane: ethyl acetate: methyl alcohol: water, more than be fixing phase mutually, time is flowing phase mutually.
Method for combined use according to the embodiment of the invention; Wherein the extraction conditions in the accelerated solvent extraction process is: adopting the flowing phase of high speed adverse current chromatogram is extract; Under the pressure of 90～120 ℃ and 85～120bar, extract 10～20min, twice of circulation extraction or more than, obtain extract.
According to the method for combined use of the embodiment of the invention, wherein said transfer valve is a six-way valve; After high speed adverse current chromatogram dicyandiamide solution balance was set up, the rotation six-way valve made that a position of six-way valve communicates with the f position, the b position communicates with the c position and the d position communicates with the e position.
The object of the invention and solve its technical problem and also adopt following technical scheme to realize.A kind of accelerated solvent extraction-high speed adverse current chromatograph joint used device according to the present invention proposes comprises: the accelerated solvent extraction device is used to extract material to obtain extract; High-speed counter-current chromatograph is used for the target components that purifying prepares or analyze extract; Solvent pump, the extract that is used to will speed up solvent extraction plant pumps into high-speed counter-current chromatograph; Transfer valve is used to connect accelerated solvent extraction device and high-speed counter-current chromatograph, to realize the switching between sample introduction state and released state.
The object of the invention and solve its technical problem and also can adopt following technical measures further to realize.
According to the combined apparatus of the embodiment of the invention, the used extractor volume of wherein said accelerated solvent extraction device is 1-100mL.
According to the combined apparatus of the embodiment of the invention, wherein said high-speed counter-current chromatograph is countercurrent chromatography appearance or analytic type high-speed counter-current chromatograph.
According to the combined apparatus of the embodiment of the invention, wherein said transfer valve is a six-way valve.
According to the combined apparatus of the embodiment of the invention, the tube connector between wherein said accelerated solvent extraction device and the high-speed counter-current chromatograph is polyfluortetraethylene pipe or PA tube, and the diameter of described tube connector is 0.8-3.0mm.
By technique scheme, accelerated solvent extraction-high speed adverse current chromatograph joint used method of the present invention and device have the following advantages at least:
, rapidly and efficiently extraction advantage few in conjunction with the accelerated solvent extraction solvent load and the purifying that the high speed adverse current chromatogram preparation amount is big, purity is high prepare advantage; Develop a kind of method for combined use of accelerated solvent extraction-high speed adverse current chromatogram; Can effectively reduce target components in the material such as natural products extract separate, purifying preparation or analyze the loss of sample in the overall process, shorten extraction time, the step that simplifies the operation, improve product yield.
Above-mentioned explanation only is the general introduction of technical scheme of the present invention; Understand technological means of the present invention in order can more to know; And can implement according to the content of specification, and for let of the present invention above-mentioned with other purposes, feature and advantage can be more obviously understandable, existing special act preferred embodiment; And conjunction with figs., specify as follows.
Description of drawings
Fig. 1 is an ASE-HSCCC combined apparatus sample introduction process sketch map of the present invention;
Fig. 2 is an ASE-HSCCC combined apparatus separation process sketch map of the present invention;
Fig. 3 is the high-efficient liquid phase chromatogram of Glabrous Sarcandra Herb extract;
Fig. 4 is that ASE-of the present invention prepares the high speed adverse current chromatogram figure that type HSCCC separates Glabrous Sarcandra Herb;
Fig. 5 is that ASE-of the present invention prepares the high-efficient liquid phase chromatogram that type HSCCC separates the isofraxidin that obtains;
Fig. 6 is the high speed adverse current chromatogram figure that ASE-analytic type HSCCC of the present invention separates Glabrous Sarcandra Herb;
Fig. 7 is the high-efficient liquid phase chromatogram that ASE-analytic type HSCCC of the present invention separates the isofraxidin that obtains.
1: accelerated solvent extraction device 2: liquid storage bottle
3: peristaltic pump 4: quantifying ring
5: six-way valve 6: triple valve
7: liquid storage bottle 8: liquid storage bottle
9: plunger displacement pump 10: high-speed counter-current chromatograph
11: waste liquid bottle I: isofraxidin.
A, b, c, d, e, f: switch the position
The specific embodiment
For further setting forth the present invention to reach technological means and the effect that predetermined goal of the invention is taked; Below in conjunction with accompanying drawing and preferred embodiment; To accelerated solvent extraction-high speed adverse current chromatograph joint used method of proposing according to the present invention and install its specific embodiment, structure, characteristic and effect thereof, specify as after.
Please refer to illustrated in figures 1 and 2ly, accelerated solvent extraction-high speed adverse current chromatograph joint used method of the present invention and device thereof are further detailed.Accelerated solvent extraction of the present invention-high speed adverse current chromatograph joint used method extraction isolation and purification prepares process and comprises: accelerated solvent extraction device 1 is used to extract material; High speed adverse current chromatogram dicyandiamide solution equilibrium process is used to set up high speed adverse current chromatogram fluid dynamic equilibrium system; High-speed counter-current chromatograph 10 is used for the separation and purification of material.The condition (like sample size, different solvents system) of extraction conditions of accelerated solvent extraction (as extracting temperature, pressure, extraction time and cycle-index etc.) and high speed adverse current chromatogram can be confirmed according to the different target thing, does not limit at this.Accelerated solvent extraction of the present invention-high speed adverse current chromatograph joint used device is through polytetrafluoroethylene (PTFE) or polypropylene tube connector (not shown), and the diameter of tube connector can be realized the full-automatic or semi-automatic operation of complete machine for 0.8-3.0mm, transfer valve (being six-way valve 5 in the present embodiment), solvent pump (being peristaltic pump 3 and plunger displacement pump 9 in the present embodiment) etc.
Please with reference to shown in Figure 1, in the process, a position of six-way valve 5 communicates with the b position, the c position communicates with the d position, the e position communicates with the f position.At first extract material through accelerated solvent extraction device 1, this accelerated solvent extraction device 1 used extractor volume can be 1-100mL; Extract and finish 2 collections of back employing liquid storage bottle; Adopt plunger displacement pump 9 with the fixing high-speed counter-current chromatograph 10 that pumps into mutually in the liquid storage bottle 8; Start high-speed counter-current chromatograph 10, with plunger displacement pump 9 flowing phase in the liquid storage bottle 7 is pumped into high-speed counter-current chromatograph simultaneously, carry out the dicyandiamide solution balance.
Extract in the liquid storage bottle 2 is pumped into quantifying ring 4 through peristaltic pump 3; After high speed adverse current chromatogram dicyandiamide solution balance was set up, please with reference to shown in Figure 2, rotation six-way valve 5 made that a position of six-way valve 5 communicates with the f position, the b position communicates with the c position and the d position communicates with the e position; Sample solution in the quantifying ring 4 is pumped into high speed adverse current chromatogram 10, sample solution is carried out purifying preparation or analysis.
(adopting ASE-to prepare the isofraxidin in the type HSCCC coupling separation and purification Glabrous Sarcandra Herb)
Its concrete operations are: the Glabrous Sarcandra Herb sample that takes by weighing 2.0g 20-40mesh is in 22mL ASE extractor; Adopting HSCCC flowing phase is extract; Extract 10min at 100 ℃ down with the pressure of 100bar, circulation extraction twice, collection extract (high-efficient liquid phase chromatogram of Glabrous Sarcandra Herb extract sees also shown in Figure 3); Extract is directly pumped into preparation type HSCCC carry out the purifying preparation, the waste collection in the sample introduction process is in waste liquid bottle 11.The condition of preparation type HSCCC: sampling volume 10mL, dicyandiamide solution are n-hexane: ethyl acetate: methyl alcohol: water=1: 2: 1: 2 (volume ratios), column volume are 240mL; Rotating speed 800rpm; Above phase n-hexane/ethyl acetate is fixing phase, and following phase methanol is a flowing phase, flow velocity 2.0mL/min; Fixedly the phase retention rate is about 54%, and ultraviolet detects wavelength 344nm.Fig. 4 is that ASE-prepares the adverse current chromatogram figure that type HSCCC separation Glabrous Sarcandra Herb obtains; Fig. 5 is that ASE-prepares the high-efficient liquid phase chromatogram that type HSCCC separates the isofraxidin that obtains, and the liquid chromatographic detection purity of isofraxidin is greater than 99%.
(adopting the isofraxidin in the ASE-analytic type HSCCC coupling separation and purification Glabrous Sarcandra Herb)
Its concrete operations are: the Glabrous Sarcandra Herb sample that takes by weighing 2.0g 20-40mesh is in the 22mL extractor; Adopting HSCCC flowing phase is extract; Extract 10min at 100 ℃ down with the pressure of 100bar, circulation extraction twice, collection extract (high-efficient liquid phase chromatogram of Glabrous Sarcandra Herb extract sees also shown in Figure 3); Extract is directly pumped into analytic type HSCCC carry out purifies and separates, the waste collection in the sample introduction process is in waste liquid bottle 11.Analytic type high speed adverse current chromatogram condition: sampling volume 2mL; Dicyandiamide solution is a n-hexane: ethyl acetate: methyl alcohol: water=1: 2: 1: 2 (volume ratios); Column volume is 43mL, rotating speed 1600rpm, and above phase n-hexane/ethyl acetate is fixing phase; Following phase methanol is a flowing phase, flow velocity 2.0mL/min; Fixedly the phase retention rate is about 51%, and ultraviolet detects wavelength 344nm.Fig. 6 is that ASE-analytic type HSCCC separates the adverse current chromatogram figure that Glabrous Sarcandra Herb obtains; Fig. 7 is the high-efficient liquid phase chromatogram that ASE-analytic type HSCCC separates the isofraxidin that obtains; The liquid chromatographic detection purity of isofraxidin is greater than 99%.
Clearly; Adopt accelerated solvent extraction-high speed adverse current chromatograph joint used method of the present invention and device; Can directly from Glabrous Sarcandra Herb, obtain purity greater than 99% active ingredient isofraxidin, the rapid extraction of isofraxidin is separated with purifying and is prepared in the canbe used on line Glabrous Sarcandra Herb.This combined apparatus has combined the accelerated solvent extraction device can rapidly and efficiently extract the advantage of the efficiently purifying preparation of separation and high speed adverse current chromatogram; Effectively reduce target components extraction in the sample such as natural products, separation, purifying and preparation or analyze the sample loss in the overall process; Shorten extraction time; Cut down the number of intermediate links, improve separative efficiency.
In addition; In above-mentioned instance; Isofraxidin is explained as object in the employing Glabrous Sarcandra Herb; But the present invention is not only applicable to extraction separation, the purifying preparation of active ingredient in the natural products or analyzes, and can be applied to the separating at line drawing fast of target components in other complex objects such as food, medicine, biology, purifying preparation yet or analyzes.
Can know according to above explanation; Accelerated solvent extraction of the present invention-high speed adverse current chromatograph joint used appearance have adapt to wide, rapidly and efficiently, rate of recovery advantages of higher, the extraction that can be widely used in target components in the complex objects such as food, medicine and biology separates, purifying, preparation and analysis.
The above only is preferred embodiment of the present invention, is not the present invention is done any pro forma restriction; Though the present invention discloses as above with preferred embodiment; Yet be not in order to limiting the present invention, anyly be familiar with the professional and technical personnel, in not breaking away from technical scheme scope of the present invention; Make the equivalent embodiment that changes or be modified to equivalent variations when the technology contents of above-mentioned announcement capable of using; In every case be the content that does not break away from technical scheme of the present invention, to any simple modification, equivalent variations and modification that above embodiment did, all still belong in the scope of technical scheme of the present invention according to technical spirit of the present invention.
Claims (9)
1. accelerated solvent extraction-high speed adverse current chromatograph joint used method is characterized in that it comprises step:
1) accelerated solvent extraction is followed the example of the extract employing liquid storage bottle collection that the extract material obtains;
2) through peristaltic pump the extract in the liquid storage bottle is pumped into quantifying ring;
3) adopt plunger displacement pump with fixing preparation type or the analytic type high-speed counter-current chromatograph of pumping into mutually in the liquid storage bottle; Start high-speed counter-current chromatograph; With plunger displacement pump the flowing phase in the liquid storage bottle is pumped into preparation type or analytic type high-speed counter-current chromatograph simultaneously, carry out the dicyandiamide solution balance;
4) after high speed adverse current chromatogram dicyandiamide solution balance is set up, the sample solution in the quantifying ring is pumped into preparation type or analytic type high speed adverse current chromatogram carry out the separation and purification preparation or analyze;
Above-mentioned steps through the integrated accelerated solvent extraction of transfer valve and high speed adverse current chromatogram in one, realize active ingredient of natural product in preparation of line drawing isolation and purification or analysis.
2. accelerated solvent extraction-high speed adverse current chromatograph joint used method according to claim 1; It is characterized in that; It is 1: 2: 1 that the dicyandiamide solution of high speed adverse current chromatogram adopts volume ratio: 2 n-hexane: ethyl acetate: methyl alcohol: water, more than be fixing phase mutually, time is flowing phase mutually.
3. accelerated solvent extraction-high speed adverse current chromatograph joint used method according to claim 1; It is characterized in that; The extraction conditions of accelerated solvent extraction is: adopting the flowing phase of high speed adverse current chromatogram is extract; Under the pressure of 90～120 ℃ and 85～120bar, extract 10～20min, twice of circulation extraction or more than, obtain extract.
4. accelerated solvent extraction-high speed adverse current chromatograph joint used method according to claim 1 is characterized in that: said transfer valve is a six-way valve; After high speed adverse current chromatogram dicyandiamide solution balance was set up, the rotation six-way valve made that a position of six-way valve communicates with the f position, the b position communicates with the c position and the d position communicates with the e position.
5. accelerated solvent extraction-high speed adverse current chromatograph joint used device is characterized in that it comprises:
The accelerated solvent extraction device is used to extract material to obtain extract;
High-speed counter-current chromatograph is used for the target components that purifying prepares or analyze extract;
Solvent pump, the extract that is used to will speed up solvent extraction plant pumps into high-speed counter-current chromatograph;
Transfer valve is used to connect accelerated solvent extraction device and high-speed counter-current chromatograph, to realize the switching between sample introduction state and released state.
6. accelerated solvent extraction according to claim 5-high speed adverse current chromatograph joint used device is characterized in that: the used extractor volume of described accelerated solvent extraction device is 1-100mL.
7. accelerated solvent extraction according to claim 5-high speed adverse current chromatograph joint used device is characterized in that: described high-speed counter-current chromatograph is countercurrent chromatography appearance or analytic type high-speed counter-current chromatograph.
8. the extract-high speed adverse current chromatograph joint used device of accelerated solvent according to claim 5 is characterized in that: described transfer valve is a six-way valve.
9. accelerated solvent extraction according to claim 5-high speed adverse current chromatograph joint used device; It is characterized in that: the tube connector between described accelerated solvent extraction device and the high-speed counter-current chromatograph is polyfluortetraethylene pipe or PA tube, and the diameter of described tube connector is 0.8-3.0mm.
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| CN103913533B (en) * | 2013-01-09 | 2016-08-24 | 丽珠集团利民制药厂 | For evaluating method and the application thereof of ginseng and astragalus injection for strengthening body chemical composition |
| CN103278595B (en) * | 2013-05-07 | 2015-08-19 | 大连依利特分析仪器有限公司 | Special automatic detection equipment for benzopyrene |
| CN104645667B (en) * | 2013-11-18 | 2017-02-08 | 华东理工大学 | Expanded bed chromatography and counter-current chromatography on-line combination method, application and apparatus thereof |
| CN107151203A (en) * | 2016-03-03 | 2017-09-12 | 复旦大学 | Separate the method for preparing natural naphthoquinone compound |
| CN106053870A (en) * | 2016-08-02 | 2016-10-26 | 国网山东省电力公司枣庄供电公司 | Automatic sample introduction device for insulating oil slug test |
| CN107227413A (en) * | 2017-05-27 | 2017-10-03 | 润华实业有限公司 | A kind of method of use counter-current chromatograph extracting and separating zirconium and hafnium |
| CN108254475A (en) * | 2018-03-09 | 2018-07-06 | 山东省分析测试中心 | A kind of high-speed counter-current chromatograph and method of work for complex sample multi-cycle separation |
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| CN101073595A (en) * | 2007-06-18 | 2007-11-21 | 石任兵 | Glycyrrhiza total flavonoid and total saponin extract and its production |
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| CN101073595A (en) * | 2007-06-18 | 2007-11-21 | 石任兵 | Glycyrrhiza total flavonoid and total saponin extract and its production |
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| 胡江涌.天然产物中有效成分的高压均质提取和高速逆流色谱分离技术研究.《华南师范大学硕士学位论文（2007）》.2007,第32-34，41-46页. * |
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