CN204989118U - Online activity detection's liquid chromatogram - mass spectrometry appearance - Google Patents
Online activity detection's liquid chromatogram - mass spectrometry appearance Download PDFInfo
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- CN204989118U CN204989118U CN201520580280.8U CN201520580280U CN204989118U CN 204989118 U CN204989118 U CN 204989118U CN 201520580280 U CN201520580280 U CN 201520580280U CN 204989118 U CN204989118 U CN 204989118U
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- mass spectrometer
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- pump
- online activity
- fluid reservoir
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Abstract
The utility model discloses an online activity detection's liquid chromatogram - mass spectrometry appearance. Including one set of high performance liquid chromatography tandom mass spectrometer, a plurality of reaction liquid are in order to correspond control pump and ultraviolet detector. The sample gets into liquid chromatograph process after -separating, and through the reposition of redundant personnel of first three -way valve, partly mass spectrum that gets into carries out qualitative analysis such as structural identification, and enzyme solution and substrate the solution partly and output of pump control system mix in the cross valve in advance, get into spiral helicine reacting chamber, get into the detector with the color development liquid that has the pump control system to export after the reaction liquid that the reacting chamber flows out mixes in the second three -way valve. Simple structure, equipment are convenient, controlled strong, activity that can direct on -line measuring compound of temperature control and time, can improve the efficiency of natural products active ingredient development greatly.
Description
Technical field
The utility model relates to a kind of liquid chromatograph-mass spectrometer, especially a kind of can the liquid chromatograph-mass spectrometer of Activity determination online.
Background technology
Natural products resource has huge economic worth and using value, compound containing medical active in many natural productss, native compound is one of important directions of drug discovery, at present many active ingredients still all deriving from natural products at the medicine used and health products.The importance of Natural products research to health is also more and more paid close attention to.But natural products wide variety, complicated component are an important directions of its research to the separation and purification of natural products and screening bioactive compounds always.Liquid chromatograph-mass spectrometer has the good separating property of liquid chromatography and mass spectrum qualitative function accurately because of it, has become modern analysis and has commonly used and one of important analytical instrument.Also be an important means of current Separation of Natural Products purifying, Structural Identification.But for the selective mechanisms of active component in the complicated ingredients such as natural products, being the important directions of Natural products research, is also a difficult problem always.Traditional compound activity evaluation, after being through loaded down with trivial details separation and purification and Structural Identification, setting up Determination of biological activity model and carries out activity rating.And the complicated ingredients such as natural products contain tens, an even hundreds of compound, needs human and material resources and the time cost of at substantial, just can complete the activity rating work to multiple compounds in a kind of natural products.If can while the complicated ingredients such as natural products be separated, realize the online Activity determination to wherein compound and evaluation, just can carry out separation and purification and Structural Identification for activated composition, greatly can reduce the cost of traditional natural product active ingredient exploitation.
Utility model content
Technical problem to be solved in the utility model is, provides a kind of liquid chromatograph-mass spectrometer of online Activity determination, can realize completing the separation of reactive compound in the complicated ingredients such as natural products, activity rating and Structural Identification simultaneously.
In order to solve the problems of the technologies described above, the technical solution adopted in the utility model is: a kind of liquid chromatograph-mass spectrometer of online Activity determination, comprise a set of by liquid chromatography pump, the using high performance liquid chromatography tandem mass spectrum instrument of chromatographic column and mass spectrometer composition, pipeline between chromatographic column and mass spectrometer is set up the first T-valve, first T-valve is connected with a four-way valve, two streams of four-way valve are connected to the first fluid reservoir controlling the reactant liquor exported by the first pump and the second fluid reservoir exported by the second pump control, four-way valve is connected with a spiral helicine reaction chamber, the outflow end of spiral helicine reaction chamber is connected on the second T-valve, a stream of the second T-valve connects the 3rd fluid reservoir being controlled output by the 3rd pump, another stream of second T-valve connects UV-detector.
Described first fluid reservoir is for filling enzyme solutions, and the second fluid reservoir is for filling substrate solution, and the 3rd fluid reservoir is for filling nitrite ion.
The arranged outside of described reaction chamber has heating and thermal insulation layer.
Described reaction chamber is the helical duct of polytetrafluoroethylmaterial material or stainless steel material.
The length of the helical duct of described reaction chamber is 100-500cm, and diameter is 0.05-1mm.
The beneficial effects of the utility model are: the advantages such as structure is simple, easy to assembly, temperature controls and time controlling is strong, favorable reproducibility, minimizing manual operation, can the activity of direct-on-line detection compound, greatly can improve the efficiency of natural product active ingredient exploitation.
Accompanying drawing explanation
Fig. 1 is the structural representation of the liquid chromatograph-mass spectrometer of the online Activity determination of the utility model.
Fig. 2 is that embodiment utilizes the liquid chromatograph-mass spectrometer of online Activity determination complicated ingredient to be detected to the liquid chromatogram and active figure that obtain.
Embodiment
Below in conjunction with the drawings and specific embodiments, the utility model is described in further detail:
As shown in Figure 1, the liquid chromatograph-mass spectrometer of online Activity determination of the present utility model, comprise a set of by liquid chromatography pump 1, the using high performance liquid chromatography tandem mass spectrum instrument that chromatographic column 2 and mass spectrometer 4 form, pipeline between chromatographic column 2 and mass spectrometer 4 is set up the first T-valve 3, first T-valve 3 is connected with a four-way valve 9, two streams of four-way valve 9 are connected to the first fluid reservoir 5 controlling the reactant liquor exported by the first pump 6 and the second fluid reservoir 7 exported by the second pump 8 control, four-way valve 9 is connected with a spiral helicine reaction chamber 10, the outflow end of spiral helicine reaction chamber 10 is connected on the second T-valve 13, a stream of the second T-valve 13 connects the 3rd fluid reservoir 11 being controlled output by the 3rd pump 12, another stream of second T-valve 13 connects UV-detector 14.
Described first fluid reservoir 5 is for filling enzyme solutions, and the second fluid reservoir 7 is for filling substrate solution, and the 3rd fluid reservoir 11 is for filling nitrite ion.
The arranged outside of described reaction chamber 10 has heating and thermal insulation layer.
Described reaction chamber 10 is helical ducts of polytetrafluoroethylmaterial material or stainless steel material.
The length of the helical duct of described reaction chamber 10 is 100-500cm, and diameter is 0.05-1mm.
Specifically, sample enters liquid chromatography pump 1, chromatographic column 2 after being separated, shunt through the first T-valve 3, a part enters mass spectrometer 4 and carries out the qualitative analyses such as Structural Identification, a part and the first pump 6 control substrate solution premix in four-way valve 9 of enzyme solutions and the second pump 8 control output exported, enter spiral helicine reaction chamber 10, after the reactant liquor that reaction chamber flows out and the nitrite ion controlling to export by the 3rd pump 12 mix in the second T-valve 13, enter UV-detector 14.
The efflux be separated to make liquid chromatography and enzyme solutions and substrate solution fully react, and can keep temperature constant and be placed in keeping warm mode, there is heating and thermal insulation layer in the outside of described reaction chamber 10.
The helical duct that described reaction chamber 10 is made up of polyfluortetraethylene pipe or stainless-steel tube, to ensure the abundant hybrid reaction of solution, the derivatization reaction time can be controlled according to solution flow velocity in the channel, usually, the length that room 10 is led in described reaction is 100-500cm, and diameter is 0.05-1mm.
Pump 1,6,8,12 described in the utility model can the absorption of Quality control solution, enzyme solutions, substrate solution and nitrite ion and flow velocity; Design the length of reaction channel (spiral helicine reaction chamber 9) according to the length of derivatization reaction time, material can use teflon, stainless steel or other materials.Pump is liquid chromatography pump or constant flow pump.
Such as, the liquid chromatograph-mass spectrometer of the online Activity determination of the utility model is utilized to measure in a complex sample each compound to the inhibit activities of AMS.Liquid chromatograph tandem mass spectrometer is started shooting, and be 0.4mL/min by liquid chromatograph flow rate set, be 0.1mL/min, 0.2mL/min, 0.1mL/min by pump 6,8,12 flow rate set controlling AMS solution, substrate 0.1% starch solution and nitrite ion 0.5% iodine solution respectively; Reaction chamber temperature is set to the optimal reactive temperature 37 DEG C of AMS; A whole set of instrument is made to be in equilibrium state, equilibration time 10-30min.After instrument balance, by liquid chromatograph, sample is separated, different component compound in time length elutes in chromatographic column 2, shunted by the first T-valve 3 and enter mass spectrometer 4 and four-way valve 9 respectively, mass spectrometer 4 carries out Structural Identification to entering mass spectrometer part compound, enter four-way valve 9 part and AMS solution, substrate 0.1% starch solution mixes, entering by heating and thermal insulation layer and length after mixing is 200cm, the reaction chamber 10 of the polyfluortetraethylene pipe composition of internal diameter 0.1mm, by to AMS solution, the impact of substrate 0.1% starch solution reaction velocity in the reaction chamber, namely remaining starch solution is how many, reflect the inhibit activities of compound to AMS, reacted reactant liquor enters the second T-valve 13 and nitrite ion 0.5% iodine solution hybrid reaction, by be set as the UV-detector 14 of 610nm carry out assaying reaction after the content of remaining starch, UV-detector signal is stronger, show to react remaining starch more, namely the inhibit activities of compound to AMS is stronger.As can be seen from result (Fig. 2): A figure is after liquid chromatography is separated, the total ion current figure of Mass Spectrometer Method, can see in this complex sample having five compounds, B figure is after liquid chromatography shunting, the activity figure that online activity monitor system measures, as can be seen from the figure, there is stronger signal at compound 2,4 place, show that compound 2,4 pairs of AMSs have stronger inhibit activities, and compound 1,3,5 pairs of AMSs do not have inhibit activities, mass spectrum, to compound 2,4 Structural Identification, confirms that compound 2,4 is respectively acarbose and voglibose.Prove that the liquid chromatography mass instrument of this online Activity determination can realize detection to the activity of compound in complicated ingredient and Structural Identification.
Above-described embodiment is only for illustration of technological thought of the present utility model and feature, its object is to enable those skilled in the art understand content of the present utility model and implement according to this, only can not limit the scope of the claims of the present utility model with the present embodiment, namely the equal change that the spirit that all the utility model disclose is done or modification, still drop in the scope of the claims of the present utility model.
Claims (5)
1. the liquid chromatograph-mass spectrometer of an online Activity determination, comprise a set of by liquid chromatography pump (1), the using high performance liquid chromatography tandem mass spectrum instrument that chromatographic column (2) and mass spectrometer (4) form, it is characterized in that, pipeline between chromatographic column (2) and mass spectrometer (4) is set up the first T-valve (3), first T-valve (3) is connected with a four-way valve (9), two streams of four-way valve (9) are connected to the first fluid reservoir (5) controlling the reactant liquor exported by the first pump (6) and the second fluid reservoir (7) exported by the second pump (8) control, four-way valve (9) is connected with a spiral helicine reaction chamber (10), the outflow end of spiral helicine reaction chamber (10) is connected on the second T-valve (13), a stream of the second T-valve (13) connects the 3rd fluid reservoir (11) being controlled output by the 3rd pump (12), another stream of second T-valve (13) connects UV-detector (14).
2. the liquid chromatograph-mass spectrometer of online Activity determination according to claim 1, it is characterized in that, described first fluid reservoir (5) is for filling enzyme solutions, and the second fluid reservoir (7) is for filling substrate solution, and the 3rd fluid reservoir (11) is for filling nitrite ion.
3. the liquid chromatograph-mass spectrometer of online Activity determination according to claim 1, is characterized in that, the arranged outside of described reaction chamber (10) has heating and thermal insulation layer.
4. the liquid chromatograph-mass spectrometer of online Activity determination according to claim 1, is characterized in that, described reaction chamber (10) is the helical duct of polytetrafluoroethylmaterial material or stainless steel material.
5. the liquid chromatograph-mass spectrometer of online Activity determination according to claim 4, is characterized in that, the length of the helical duct of described reaction chamber (10) is 100-500cm, and diameter is 0.05-1mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520580280.8U CN204989118U (en) | 2015-08-04 | 2015-08-04 | Online activity detection's liquid chromatogram - mass spectrometry appearance |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520580280.8U CN204989118U (en) | 2015-08-04 | 2015-08-04 | Online activity detection's liquid chromatogram - mass spectrometry appearance |
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| CN204989118U true CN204989118U (en) | 2016-01-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201520580280.8U Expired - Fee Related CN204989118U (en) | 2015-08-04 | 2015-08-04 | Online activity detection's liquid chromatogram - mass spectrometry appearance |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106018596A (en) * | 2016-05-17 | 2016-10-12 | 华南理工大学 | Online microwave-assisted chiral derivatization-LC/MS (liquid chromatography/mass spectrometry) analysis system and method |
| CN107525870A (en) * | 2017-09-07 | 2017-12-29 | 吴建发 | A kind of on-line chromatograph detects tubular reactor system |
-
2015
- 2015-08-04 CN CN201520580280.8U patent/CN204989118U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106018596A (en) * | 2016-05-17 | 2016-10-12 | 华南理工大学 | Online microwave-assisted chiral derivatization-LC/MS (liquid chromatography/mass spectrometry) analysis system and method |
| CN106018596B (en) * | 2016-05-17 | 2018-09-14 | 华南理工大学 | A kind of online microwave radiation technology chiral derivatization-LC-MS analysis system and method |
| CN107525870A (en) * | 2017-09-07 | 2017-12-29 | 吴建发 | A kind of on-line chromatograph detects tubular reactor system |
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Legal Events
| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160120 Termination date: 20160804 |