CN100504396C - High performance liquid chromatography and magnetic resonance imaging analyzer - Google Patents
High performance liquid chromatography and magnetic resonance imaging analyzer Download PDFInfo
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- CN100504396C CN100504396C CNB200510026402XA CN200510026402A CN100504396C CN 100504396 C CN100504396 C CN 100504396C CN B200510026402X A CNB200510026402X A CN B200510026402XA CN 200510026402 A CN200510026402 A CN 200510026402A CN 100504396 C CN100504396 C CN 100504396C
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- magnet
- chromatographic column
- gradient coil
- magnetic resonance
- measuring sonde
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Abstract
An image and spectrum analyzer is composed of high efficient liquid phase chromatograph system and nuclear magnetic resonance system. It is featured as setting chromatographic column in central hole of measuring probe placed between two gradient coils set between two cylindrical magnetic poles if normal magnet is applied or setting chromatographic column in central hole of measuring probe placed in gradient coil set in cylindrical superconductive magnet if superconductive magnet is applied.
Description
Technical field
The invention belongs to the chemical analysis technology field, be specifically related to a kind of high performance spectrmeter for liquid chromatography and magnetic resonance imaging.
Background technology
At present, nuclear magnetic resonance chemical analysis instrument, efficient liquid phase chromatographic analysis instrument all separate independent.
The nuclear magnetic resonance chemical analysis instrument has: Switzerland Bruker company, Japanese JEO company and U.S. Varian company.
The efficient liquid phase chromatographic analysis instrument abroad has: U.S. Aglient (Agilent), Waters company etc.The domestic product that the above-mentioned company of import is arranged.
The weak point of present technology: nuclear magnetic resonance and chromatogram are difficult to combination.Its reason is that prior art is to utilize chromatogram to separate the back to collect, and the material after will collecting is again put into nuclear magnetic resonance respectively and measured.Like this can cause material to lose in a large number in collection process, especially nuclear magnetic resonance itself is the low analytical instrument of muting sensitivity, effective rate of utilization, lacks the stage that can't measure substantially through the material after the chromatographic resolution like this.Chromatogram that Here it is-nuclear magnetic resonance coupling is difficult to the effectively reason of realization.
Summary of the invention
The objective of the invention is to propose the high performance spectrmeter for liquid chromatography and magnetic resonance imaging that a kind of liquid chromatography and nuclear magnetic resonance can couplings.
The high performance spectrmeter for liquid chromatography and magnetic resonance imaging that the present invention proposes, be the different mechanism of utilizing in the high performance liquid chromatography because of different material rate of propagation in the look post, make to mix object and in the look post, have the function of separation, utilize the chemical shift of NMR spectrum and the J-J coupling of different position of fault in nuclear mangetic resonance-CT technology and the high resolving power spectrometer commercial measurement look post to compose simultaneously.
Instrument is made up of common highly effective liquid phase chromatographic system and NMR system two parts.Wherein, the chromatographic column of liquid chromatographic system is installed in the magnet and measuring sonde of NMR system, to replace the sample position in the nuclear magnetic resonance.
Advantage of the present invention
1. with chromatogram and the complete organic integration one of nuclear magnetic resonance,, improve the effective rate of utilization of Nuclear Magnetic Resonance Measurement simultaneously, eliminate the measuring error of a series of high performance liquid chromatography such as dead space again so there is not material damage.
2. can study the basic mechanism of chromatogram by Magnetic resonance imaging.
3. the solid phase spectral line and the contrast of liquid phase spectral line that utilize the interaction of fluid to be measured and look post filling powder to produce obtain more chemical substance information.
4. can realize measuring in real time and on-line measurement.
Description of drawings
Fig. 1 is the instrument general diagram under the conventional magnet.
Fig. 2 is the installation graph of a relation (transverse section diagram) of the chromatographic column of the instrument under the conventional magnet.
Fig. 3 is the instrument general diagram under the superconducting magnet.
Fig. 4 is the installation graph of a relation (transverse section diagram) of the chromatographic column of the instrument under the superconducting magnet.
Fig. 5 is Zeitigung displacement study figure.
Fig. 6 is the space chemistry displacement diagram.
Number in the figure: 1 is the circuit control section of nuclear magnetic resonance, and 2 is magnet, and 3 is gradient coil, and 4 is measuring sonde, and 5 is chromatographic column, and 6 is high-pressure pump, and 7 is retaining valve, and 8 is the molten device of cleaning fluid, and 9 is valve, and 10 is sample injector, and 11 is superconducting magnet.
Embodiment
Through connecting to form, liquid chromatographic system is connected to form by chromatographic column, high-pressure pump, valve, the molten device of sample injector cleaning fluid common NMR system by the road by magnet, gradient coil, probe, computing machine and circuit control section.Wherein,
1, magnet: the critical piece of nuclear magnetic resonance, divide conventional magnet and superconducting magnet two big classes.Conventional magnet is to utilize common magnet steel or electric current to form the loop through ferromagnetic material to obtain higher magnetic field (＜2.3T) magnet.Superconducting magnet is that hollow superconducting coil utilizes superconductor zero resistance at low temperatures, has the magnet of the supramaximal current ability that flows through, generation superelevation high-intensity magnetic field (5-20T).It can and utilize zero resistance to form the stable electric current of shut height under power free situation.
2, gradient coil: the critical piece of Magnetic resonance imaging.When the gradient coil inflow current, produce gradient magnetic, utilize gradient magnetic to carry out selective excitation, thereby obtain the spatial positional information of measured matter different spaces.
3, probe: the vitals of nuclear magnetic resonance.Be used for emitting radio wave (nuclear magnetic resonance term " radio-frequency (RF) magnetic field "), the excited nucleus magnetic resonance energy, and measure the radiowave of nuclear magnetic resonance radiation.Its effect is the material of surveying in chromatographic column, can obtain the chemical shift and the J-J coupling information of material according to the radio frequency difference of chemical substance emission.
4, computing machine and automatically controlled part: the vitals of nuclear magnetic resonance.Excite and measure by the radiowave of computer control gradient coil current, probe, carry out data analysis by computer software again and handle.
5, chromatographic column: being the vitals of high performance liquid chromatography, is a pipeline of being made by materials non-conductive, non magnetic, no NMR signal such as quartz or polyetheretherketones, and the attritive powder that corundum, silica gel etc. have separating property is filled up in the inside.Thereby its effect is to make different material have different flowing velocities material is spatially separated.Can measure particular location in the chromatographic column of different material place by probe and gradient coil.
6, high-pressure pump: the power that the vitals of high performance liquid chromatography, its sampling flow in chromatographic column.
7, valve: the parts of high performance liquid chromatography.It is used for sample, cleaning fluid switches.
8, retaining valve, sample injector: the accessory of high performance liquid chromatography.
9, soda liquor container: deposit cleaning fluid.
Dissimilar according to two kinds of magnet, chromatographic column 2 kinds of different forms are installed, specifically be described below:
1. corresponding to the installation of the chromatographic column of conventional magnet:
Conventional magnet is made up of two flat cylindrical magnetic irons, in the middle of two blocks of magnet certain interval is arranged, and is commonly referred to as magnetic gap, serve as reasons two thin plates that turn to of common coil of gradient coil, and measuring sonde is that thin-walled shape is cylindrical, chromatographic column is an elongate cylinder." measuring sonde " is arranged in " gradient coil " two thin plates, and " gradient coil " is arranged in the gap of two blocks of magnet." chromatographic column " diameter minimum is installed in the right cylinder " measuring sonde ".
2. corresponding to the installation of the chromatographic column of superconducting magnet:
The centre porose right cylinder of superconducting magnet for making by the superconducting line pitch of the laps, the gradient coil thin wall cylindrical body that common coil winding becomes of serving as reasons, measuring sonde is similarly the thin wall cylindrical body, and chromatographic column is a slender cylinder.
" measuring sonde " is positioned at " gradient coil ", and " gradient coil " is arranged in the interstitial hole of " superconducting magnet "." chromatographic column " diameter minimum is installed in the thin wall cylindrical body " measuring sonde ".See Fig. 3 and shown in Figure 4.
Annexation:
The gradient current output of circuit control section is connected with gradient coil, and the RF detection system of circuit control section and measuring sonde are formed NMR system.
Soda liquor container is connected with the input port of retaining valve, the delivery outlet of retaining valve is connected with the input port of high-pressure pump, the delivery outlet of high-pressure pump is connected with the input port of valve 1, sample injector is connected with the input port 2 of valve, the delivery outlet of valve is connected with the input port of chromatographic column, forms liquid chromatographic system.
Concrete using method is as follows:
The sample of being made up of the number of chemical material (material behind the chemical reaction or the natural materials of multiple mixing) is injected into the bottom of chromatographic column by sample injector by the valve of opening, and valve-off starts high-pressure pump cleaning fluid is slowly injected chromatographic column.Sample flows in chromatographic column under the promotion of cleaning fluid.The flow velocity difference of different material in the sample in chromatographic column separated gradually.Utilize the nuclear magnetic resonance gradient coil to the different spatial in the chromatographic column successively scanning property excite, observe the radiowave of different aspects nuclear magnetic resonance emission again, obtain chromatogram nuclear magnetic resonance two dimension spectrogram by computing machine spectrum analysis software.The chromatogram nmr spectrum is divided into two kinds of mode of operations:
1, time-chemical shift figure: only repeatedly one deck is excited the material information of distinguishing chromatographic resolution by the time.As Fig. 5.
2, space-chemical shift figure: the multilayer space scanned excite, directly obtain chromatographic resolution information.As Fig. 6.
Claims (1)
1, a kind of high performance liquid chromatography nuclear magnetic resonance formula imaging spectrometer is characterized in that being made up of highly effective liquid phase chromatographic system and NMR system two parts, and wherein, the chromatographic column of liquid chromatographic system is installed in the magnet and measuring sonde of NMR system; Wherein:
When described magnet is conventional magnet, magnet is made up of two plain block formula cylindrical magnetic irons, gradient coil turns to two thin plates, measuring sonde is a thin walled cylindrical, chromatographic column is an elongate cylinder, measuring sonde is arranged in two thin plates of gradient coil, and gradient coil is arranged in the gap of two blocks of magnet, and chromatographic column is installed in the measuring sonde;
When described magnet is superconducting magnet, the centre porose right cylinder of magnet for turning to by superconducting coil, gradient coil turns to the thin wall cylindrical body, and measuring sonde is the thin wall cylindrical body, and chromatographic column is a slender cylinder; Measuring sonde is arranged in the interstitial hole of gradient coil, and gradient coil is arranged in the interstitial hole of cylindrical superconducting magnet, and chromatographic column is installed in the interstitial hole of measuring sonde.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510026402XA CN100504396C (en) | 2005-06-02 | 2005-06-02 | High performance liquid chromatography and magnetic resonance imaging analyzer |
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|---|---|---|---|
| CNB200510026402XA CN100504396C (en) | 2005-06-02 | 2005-06-02 | High performance liquid chromatography and magnetic resonance imaging analyzer |
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| Publication Number | Publication Date |
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| CN1696705A CN1696705A (en) | 2005-11-16 |
| CN100504396C true CN100504396C (en) | 2009-06-24 |
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| CNB200510026402XA Expired - Fee Related CN100504396C (en) | 2005-06-02 | 2005-06-02 | High performance liquid chromatography and magnetic resonance imaging analyzer |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105004832A (en) * | 2015-08-11 | 2015-10-28 | 苏州优谱德精密仪器科技有限公司 | Four-spectrometer combined analytical instrument suitable for complex chemical samples |
| CN106525890B (en) * | 2016-11-29 | 2017-10-10 | 中国地质调查局油气资源调查中心 | A kind of experimental provision synthesized with decomposing mixed gas hydrate |
| CN107607894B (en) * | 2017-11-06 | 2019-06-04 | 厦门大学 | It is applicable in miniature malcoils and its preparation associated with HPLC-NMR |
| CN108896946B (en) * | 2018-07-04 | 2020-05-19 | 中国原子能科学研究院 | Calibration method for calibrating area of induction coil probe |
| CN117130297B (en) * | 2023-10-25 | 2023-12-29 | 北京豪思生物科技股份有限公司 | Upper computer control method, device and equipment of liquid chromatograph |
| CN117783017A (en) * | 2024-02-26 | 2024-03-29 | 中国科学院武汉岩土力学研究所 | Rock and soil detection device and method combining nuclear magnetic resonance and hyperspectral imaging |
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