CN206876657U - A kind of Accelerate solvent extraction instrument LC-MS instrument combined apparatus - Google Patents
A kind of Accelerate solvent extraction instrument LC-MS instrument combined apparatus Download PDFInfo
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- CN206876657U CN206876657U CN201720520764.2U CN201720520764U CN206876657U CN 206876657 U CN206876657 U CN 206876657U CN 201720520764 U CN201720520764 U CN 201720520764U CN 206876657 U CN206876657 U CN 206876657U
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- instrument
- solvent extraction
- accelerate solvent
- combined apparatus
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Abstract
The utility model discloses Accelerate solvent extraction instrument LC-MS instrument combined apparatus, including Accelerate solvent extraction instrument, it is characterised in that the extract collecting tank of described Accelerate solvent extraction instrument is connected by peristaltic pump with switching valve 1；Switching valve 1 is connected with switching valve 2；Switching valve 2 is connected with LC-MS instrument.The utility model method integrates Accelerate solvent extraction instrument with LC-MS instrument in one by switching valve and on-line solid phase extraction, realize the On-line testing and qualitative and quantitative analysis of active ingredient of natural product, with rapidly and efficiently, automaticity is high the characteristics of, have wide practical use in fields such as food, medicine, biologies.
Description
Technical field
Technology of the present utility model is related to a kind of Accelerate solvent extraction instrument-LC-MS instrument（ASE-HPLC/MS）Combination dress
Put, extraction separation, qualitative or quantitative analysis suitable for the field target components such as medicine, biology, food.
Background technology
Accelerate solvent extraction technology（Accelerated Solvent Extraction, ASE）It is to grow up in recent years
One kind in high temperature（Room temperature~200 DEG C）, high pressure（Atmospheric pressure~20MPa）Under the conditions of rapid extraction solid or semi-solid sample
Sample-pretreating method, compared with the methods of conventional surname extraction, ultrasonic extraction, microwave-assisted extraction technique, it is substantially shorter extraction
The time is taken, improves extraction efficiency, reduces extractant dosage, significantly reduces the extraction expense of single sample, has saving molten
The advantages that agent, quick, health environment-friendly, high automaticity, U.S. EPA standard method has been confirmed to be it.
Although current Accelerate solvent extraction and LC-MS technology are widely used in natural products, food, medicine respectively
Deng field, still, the extraction liquid measure of Accelerate solvent extraction instrument extraction is big, it is necessary to be reclaimed, purified treatment more than impurity, so as to
Add the difficulty of experimental implementation；The technology of preparing of biological sample has turned into simultaneously hinders LC-MS technology quantitative analysis biology
The main bottleneck of medicine in sample, and both are still in independent studies state.
The content of the invention
Technology of the present utility model is aimed to overcome that existing for existing natural product extraction and qualitative and quantitative analysis
The defects of, and a kind of new Accelerate solvent extraction for integrating extraction separation and qualitative and quantitative analysis rapidly and efficiently is provided
Instrument-LC-MS instrument combined apparatus, operating procedure can be effectively reduced, reduce sample loss, improve analysis efficiency.
The technical solution of the utility model is：Accelerate solvent extraction instrument-LC-MS instrument combined apparatus, including fast solvent
Abstraction instrument, the extract collecting tank of described Accelerate solvent extraction instrument are connected by peristaltic pump with switching valve 1；Switching valve 1 with
Switching valve 2 is connected；Switching valve 2 is connected with LC-MS instrument.
It is 50~100mL that extract used in described Accelerate solvent extraction instrument, which collects tank volume,.
Described switching valve 1 and switching valve 2 is six-way valve.
Quantitative loop is connected with described switching valve 1, the quantitative loop volume is 0.5~5mL.
It is connected in described switching valve 1 by plunger pump with eluent liquid storage bottle.
Solid-phase extraction column is connected with described switching valve 2, the solid-phase extraction column is 2~5 × 10~100mm, and filler is
C18、C8, HILIC, silica gel, one or more of mixed fillers in multi-walled carbon nanotube.
Described LC-MS instrument includes chromatogram pump, chromatographic column, detector, mass spectrograph.
Described switching valve 2 is connected with the chromatogram pump and chromatographic column of LC-MS instrument.
Described chromatogram pump is connected with mobile phase liquid storage bottle.
Described chromatographic column is 1.5~5 × 10~100mm, filler C18、C8, HILIC, one kind in silica gel.
Described detector is one kind in UV-detector, PDAD, fluorescence detector.
Described mass spectrograph is one kind in triple quadrupole bar, ion trap, time of-flight mass spectrometer.
Connecting tube between described Accelerate solvent extraction instrument and LC-MS instrument is polyfluortetraethylene pipe or PA tube,
A diameter of 0.8~3.0mm of described connecting tube.
By above-mentioned technical proposal, Accelerate solvent extraction instrument of the present invention-LC-MS instrument combined apparatus at least has following
Advantage：With reference to Accelerate solvent extraction solvent load is few, extraction advantage rapidly and efficiently；Simple, effective spy of on-line solid phase extraction
Point and the efficient qualitative and quantitative of LC-MS instrument, highly sensitive advantage, research and development Accelerate solvent extraction instrument-LC-MS instrument connection
With device, the full-automatic or semi-automatic operation of complete machine is realized；Target components extraction point in the materials such as natural products can effectively be reduced
From the loss of sample in, qualitative or quantitative analysis overall process, shorten extraction time, simplify operating procedure, improve analysis efficiency.
Brief description of the drawings
Fig. 1 is ASE-HPLC/MS combined apparatus schematic diagram of the present invention；
Fig. 2 is the high-efficient liquid phase chromatogram of great Hua rough gentian extract solutions；
A:Accelerate solvent extraction instrument, B:Peristaltic pump, C:Switching valve 1, D:Quantitative loop, E:Waste liquid bottle, F:Switching valve 2, G:
Solid-phase extraction column, H:Chromatogram pump, I:Mobile phase liquid storage bottle, J:Chromatographic column, K:Detector, L:Mass spectrograph, M:Plunger pump, N:Wash
De- liquid liquid storage bottle
1:Isorhamnetin-3-O-neohesperidoside, 2:Oleoside methylester, 3:Sweroside, 4:Different Polygonum orientale
Element -6'-O- glucosides, 5:Homo-orientin -4'-O- glucosides, 6:Different scoparin -2 "-O- glucopyranosides, 7:
Homo-orientin, 8:Urnu gentian herb glycosides E, 9:Isovitexin, 10:Different scoparin, 11:Apigenin-7-O-beta-D-glucopyranose
Glycosides, 12:Great Hua gentiins A, 13:Depressine, 14:Urnu gentian herb glycosides B, 15:3"-glucosyl
Depresteroside, 16:Urnu gentian herb glycosides A, 17:Great Hua gentiins B
Embodiment
The Accelerate solvent extraction of active component-LC-MS analysis in the great Hua rough gentian of embodiment 1
The purpose great Hua rough gentian samples of 2.0g 40 are weighed in 22mL ASE extraction kettles, use 75% methanol as extract solution,
10min is extracted under 70 DEG C and 100bar of pressure, circulation extraction twice, collects extract solution in extract collecting tank；Will extraction
Liquid is pumped into switching valve 1 by peristaltic pump, and it is 2mL that switching valve 1, which matches somebody with somebody quantitative loop,；Then with plunger pump by 20% acetonitrile eluent
It is pumped into switching valve 1 so that sample is flowed into switching valve 2 in solid-phase extraction column in quantitative loop, solid-phase extraction column model 2.1 ×
10mm, filler C18；Elute 2 minutes in solid-phase extraction column, then Vavle switching is injected a sample into LC-MS instrument and carried out
Separation and qualitative analysis, chromatographic column 4.6 × 250mm of model, filler C18, detector is PDAD, mass spectrum
Instrument is ion trap mass spectrometer.Active component has obtained preferable separation in great Hua rough gentian, altogether it is qualitative go out active component 17, Fig. 2
It is the high-efficient liquid phase chromatogram of great Hua rough gentian extract solutions.
Claims (12)
1. a kind of Accelerate solvent extraction instrument-LC-MS instrument combined apparatus, including Accelerate solvent extraction instrument, it is characterised in that institute
The extract collecting tank for the Accelerate solvent extraction instrument stated is connected by peristaltic pump with switching valve 1；Switching valve 1 and the phase of switching valve 2
Connection；Switching valve 2 is connected with LC-MS instrument.
2. Accelerate solvent extraction instrument-LC-MS instrument combined apparatus as described in claim 1, it is characterised in that described is fast
It is 50~100mL that extract used in quick-dissolving agent abstraction instrument, which collects tank volume,.
3. Accelerate solvent extraction instrument-LC-MS instrument combined apparatus as described in claim 1, it is characterised in that described cuts
It is six-way valve to change valve 1 and switching valve 2.
4. Accelerate solvent extraction instrument-LC-MS instrument combined apparatus as described in claim 1, it is characterised in that described cuts
Change on valve 1 and be connected with quantitative loop, the quantitative loop volume is 0.5~5mL.
5. Accelerate solvent extraction instrument-LC-MS instrument combined apparatus as described in claim 1, it is characterised in that described cuts
Change on valve 1 and be connected by plunger pump with eluent liquid storage bottle.
6. Accelerate solvent extraction instrument-LC-MS instrument combined apparatus as described in claim 1, it is characterised in that described cuts
Change on valve 2 and be connected with solid-phase extraction column, the solid-phase extraction column is 2~5 × 10~100mm, filler C18、C8, HILIC, silica gel,
One or more of mixed fillers in multi-walled carbon nanotube.
7. Accelerate solvent extraction instrument-LC-MS instrument combined apparatus as described in claim 1, it is characterised in that described liquid
Matter combined instrument includes chromatogram pump, chromatographic column, detector, mass spectrograph.
8. Accelerate solvent extraction instrument as claimed in claim 7-LC-MS instrument combined apparatus, it is characterised in that described color
Spectrum pump is connected with mobile phase liquid storage bottle.
9. Accelerate solvent extraction instrument as claimed in claim 7-LC-MS instrument combined apparatus, it is characterised in that described color
Spectrum post is 1.5~5 × 10~250mm, filler C18、C8, HILIC, one kind in silica gel.
10. Accelerate solvent extraction instrument-LC-MS instrument combined apparatus as described in claim 7, it is characterised in that described
Detector is one kind in UV-detector, PDAD, fluorescence detector.
11. Accelerate solvent extraction instrument-LC-MS instrument combined apparatus as described in claim 7, it is characterised in that described
Mass spectrograph is one kind in triple quadrupole bar, ion trap, time of-flight mass spectrometer.
12. Accelerate solvent extraction instrument-LC-MS instrument combined apparatus as described in claim 1, it is characterised in that described
Connecting tube between Accelerate solvent extraction instrument and peristaltic pump, switching valve 1, switching valve 2 is polyfluortetraethylene pipe or PA tube, institute
A diameter of 0.8~the 3.0mm for the connecting tube stated.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720520764.2U CN206876657U (en) | 2017-05-11 | 2017-05-11 | A kind of Accelerate solvent extraction instrument LC-MS instrument combined apparatus |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720520764.2U CN206876657U (en) | 2017-05-11 | 2017-05-11 | A kind of Accelerate solvent extraction instrument LC-MS instrument combined apparatus |
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| CN206876657U true CN206876657U (en) | 2018-01-12 |
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| CN201720520764.2U Expired - Fee Related CN206876657U (en) | 2017-05-11 | 2017-05-11 | A kind of Accelerate solvent extraction instrument LC-MS instrument combined apparatus |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108535368A (en) * | 2018-03-13 | 2018-09-14 | 宇妥藏药股份有限公司 | A kind of method of quality control of three tastes rough gentian flower piece |
| CN108802224A (en) * | 2018-06-14 | 2018-11-13 | 潍坊学院 | A kind of high-precision traditional Chinese medicine ingredients liquid chromatography system |
| CN108845056A (en) * | 2018-08-02 | 2018-11-20 | 山东省农业科学院农业质量标准与检测技术研究所 | A kind of on-line automatic pretreating device of aflatoxin based on flow path switching |
| CN109932448A (en) * | 2019-03-29 | 2019-06-25 | 完美（广东）日用品有限公司 | The content assaying method of effective component in a kind of line leaf broom top and its product |
-
2017
- 2017-05-11 CN CN201720520764.2U patent/CN206876657U/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108535368A (en) * | 2018-03-13 | 2018-09-14 | 宇妥藏药股份有限公司 | A kind of method of quality control of three tastes rough gentian flower piece |
| CN108802224A (en) * | 2018-06-14 | 2018-11-13 | 潍坊学院 | A kind of high-precision traditional Chinese medicine ingredients liquid chromatography system |
| CN108802224B (en) * | 2018-06-14 | 2021-07-02 | 肖飞 | High accuracy traditional chinese medicine composition liquid chromatography analytical equipment |
| CN108845056A (en) * | 2018-08-02 | 2018-11-20 | 山东省农业科学院农业质量标准与检测技术研究所 | A kind of on-line automatic pretreating device of aflatoxin based on flow path switching |
| CN109932448A (en) * | 2019-03-29 | 2019-06-25 | 完美（广东）日用品有限公司 | The content assaying method of effective component in a kind of line leaf broom top and its product |
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Granted publication date: 20180112 Termination date: 20200511 |