CN113805132B - Nuclear magnetic resonance method and device - Google Patents
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- 238000001225 nuclear magnetic resonance method Methods 0.000 title abstract description 9
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- 238000012546 transfer Methods 0.000 claims abstract description 58
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- 230000002441 reversible effect Effects 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 229940065287 selenium compound Drugs 0.000 claims abstract description 25
- 150000003343 selenium compounds Chemical class 0.000 claims abstract description 25
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- 238000011158 quantitative evaluation Methods 0.000 claims abstract description 10
- 238000011157 data evaluation Methods 0.000 claims abstract description 9
- 238000001208 nuclear magnetic resonance pulse sequence Methods 0.000 claims abstract description 9
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- 230000005284 excitation Effects 0.000 claims description 23
- 238000005070 sampling Methods 0.000 claims description 10
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 230000005415 magnetization Effects 0.000 description 4
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- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
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- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R33/00—Arrangements or instruments for measuring magnetic variables
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- G01R33/44—Arrangements or instruments for measuring magnetic variables involving magnetic resonance using nuclear magnetic resonance [NMR]
- G01R33/48—NMR imaging systems
- G01R33/54—Signal processing systems, e.g. using pulse sequences ; Generation or control of pulse sequences; Operator console
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Abstract
The application provides a nuclear magnetic resonance method and a device thereof, the method uses 1 H‑ 77 The quantitative detection of the organic selenium compound by the SeqHMBC pulse sequence comprises the following steps: polarization transfer stage: by means of polarization transfer 1 Conversion of H single quantum signals 77 A Se multiple quantum signal; evolution stage: by evolution means, produce 77 Se spectrogram, obtain 1 H and 77 the coupling relation of Se signals and inhibiting the evolution among homonuclear atoms in the organic matters; reverse polarization transfer stage: said transfer is performed by reverse polarization 77 Conversion of Se multiple quantum signals into the above 1 H single quantum signals; quantitative evaluation phase: quantitative data evaluation of the organic selenium compound was completed. The method and the device provided by the application can realize the effects of wide signal selection range, high resolution, less solvent consumption in the experimental process, less material consumption and accurate quantification.
Description
Technical Field
The application relates to the field of nuclear magnetic resonance, in particular to a method and a device for quantifying an organic selenium compound by a nuclear magnetic resonance method.
Background
Quantitative research of small organic molecules under the condition of complex matrixes is a research hotspot and difficulty in the field of organic analysis. The specific expression is as follows: in the agricultural field, attention is paid to the nature (qualitative study) and content (quantitative study) of nutrients and characteristic substances in agricultural products and foods; in the fields of chemistry and materials, the law of variation of compounds during the reaction (reaction mechanism research) is of interest; in the biological and medical fields, the metabolic laws of drug metabolites (metabolic studies) and the effects on metabolites (metabolome studies) are of interest. Compared with the conventional separation means such as liquid phase, gas phase and capillary electrophoresis, the quantitative nuclear magnetic resonance method has obvious advantages of simple pretreatment, little solvent and material consumption in the whole process, rich signals for quantification and the like. However, conventional quantitative hydrogen spectra suffer from a limited spectral width, only 20ppm, and particularly for those saturated hydrocarbons, separation of the hydrogen spectrum signal is very difficult. In recent years, although the application of deconvolution technology relieves the influence of signal superposition, the quantitative error is more than 10%, and the application prospect is very small. In the field of analysis of organic matters, the organic matters are rapidly quantified, and great convenience can be provided for further research on the properties of the organic matters in various aspects.
The HMBC (Heteronuclear multiple bond correlation) heteronuclear multiple bond correlation spectrum in nuclear magnetic resonance, which is a spectrum that can be used to describe the remote coupling relationship between a high-sensitivity core and a low-sensitivity core, is mostly used for qualitative research of organic compounds by using the coupling relationship between hydrogen and carbon. In the aspect of quantitative research on organic matters, the signal frequencies of hydrogen elements and carbon elements are more likely to overlap with signals of other elements, so that quantitative analysis with high accuracy on the organic matters is difficult to perform by utilizing the coupling relation between the hydrogen elements and the carbon elements.
Disclosure of Invention
The embodiment of the application aims to provide a method and a device for quantifying an organic selenium compound by a nuclear magnetic resonance method, which are used for solving the problem of quantifying organic matters in the prior art. 77 Se is used as a rare nuclear quantum, the frequency range is larger, and the distribution range of organic selenium is-50-350 ppm, so that 1 H and 77 the coupling relation between Se can be used for quantitative analysis and research with higher accuracy, and the scheme provides a method by utilizing the property, so that the defects in the technology are overcome.
In a first aspect, embodiments of the present application identify a method for quantifying an organic selenium compound by a nuclear magnetic resonance method.
The embodiment of the application provides a nuclear magnetic resonance method by utilizing 1 H- 77 The Se qHMBC pulse sequence quantitatively detects the organic selenium compound, and comprises the following steps: polarization transfer stage: by means of polarization transfer 1 Conversion of single quantum signals of H 77 A Se multiple quantum signal; evolution stage: by evolution mode, obtain 1 H and 77 the coupling relation of Se signals and inhibiting the evolution among homonuclear atoms in the organic matters; reverse polarization transfer stage: said transfer is performed by reverse polarization 77 Conversion of Se multiple quantum signals into the above 1 H single quantum signals; quantitative evaluation phase: quantitative data evaluation of the organic selenium compound was completed.
In the embodiment of the application, the implementation process of the method is divided into four stages, wherein the first stage is that 1 H single quantum signal to 77 The process of Se multiple quantum signal transfer, the second stage is 77 The Se signal evolvement stage, and establishes an indirect dimension through evolution to form a reflection 77 Se signal 1 Spectrum of remote coupling relationship between H signals. The third stage is to obtain the coupling relation between two element signals in the previous stage and then to obtain multiple quantum signals 77 Se transfer to 1 Single quantum signal of H channel. The quantitative evaluation stage of the fourth stage comprises a sampling stage, and the effects of wide signal selection range, high resolution, less solvent consumption, less material consumption and accurate quantification are finally achieved after the four stages are passed through in order to finally realize the quantitative evaluation of the organic selenium compound.
Further, the polarization transfer mode is adopted 1 Conversion of H single quantum signals 77 Se multiple quantum signal, comprising: by remote coupling partyPolarization transfer is realized; wherein, 1 the first excitation pulse of the H channel is a 90-degree rectangular pulse; wherein the first one 77 90 ° pulse realizations of Se employ 90 ° selective excitation pulses.
The embodiment of the application takes a remote coupling mode as a carrier and takes 1 Conversion of single quantum signals of H 77 The multiple quantum signal of Se, remote coupling is here taken as a way of implementing the present embodiment. At the same time, an excitation pulse of 90 ° is given to start this polarization transfer process.
Further, in the remote coupling mode, the time interval of remote coupling evolution is specifically 0.5 to 0.02s.
In the embodiment of the application, the time interval for the remote coupling is set to be 0.5 to 0.02s, which is set according to the characteristics of the two-key and three-key coupling, and in the scheme, the remote coupling is suitable for the two-key or the three-key, so that the polarization transfer effect is best. Accordingly, when the time interval is set to 0.5 to 0.02s, the distribution range of the remote coupling reaches 2 to 50Hz, and the distribution range of the time interval is the inverse of the remote coupling time.
Further, a wide range of spectral widths is selected when the selective pulse is set to a frequency; and the selected pulse is any one of the selective pulses that can achieve a 90 deg. flip effect.
In the embodiment of the application, a wide spectrum width is selected when the frequency is set by the selective pulse, and is generally in the range of 300ppm, thus improving the resolution of the signal and being easy to obtain 77 Se signal, while other uncorrelated signals are filtered out. In addition, the excitation pulse type selected here only needs to achieve the effect of 90 ° inversion, so that more types of pulses capable of achieving 90 ° inversion can be selected.
Further, the over-evolution method generates 77 Se spectrogram, obtain 1 H and 77 coupling relationship of Se signals and suppressing evolution between homonuclear atoms in the substance, comprising: let the 77 Se multiple quantum signal evolution generation energy embodiment 1 H and 77 spectrogram of remote coupling relation between Se; suppressing the said by adopting constant time evolution methodEvolution between homonuclear atoms in a substance.
In the embodiment of the application, the main purpose of evolution is to make 77 The Se signal evolves, thereby establishing an indirect dimension. The aforementioned stage of plan transfer is from 1 Single quantum signal to H 77 Conversion of the multiple quantum signal of Se, the evolution here being mainly 77 The properties of the Se signal itself change inside.
Further, the reverse polarization transfer mode is adopted 77 Re-conversion of Se multiple quantum signals 1 A single quantum signal of H comprising: using only rectangular pulses in the reverse polarisation stage to remove the material 77 Conversion of multiple quantum signals of Se 1 H single quantum signal.
In the embodiment of the application, the effect of the reverse polarization is to 7 Multiple quantum signal transfer to Se 1 Single quantum signal of H due to 1 The H signal has high sensitivity, and is more convenient for signal sampling. Unlike polarization transfer, the pulses used here must be rectangular pulses, not other pulses that can produce a 90 ° flip effect, in order to convert the multiple quantum signal produced in the evolution stage into a single quantum signal.
Further, the reverse polarization transfer mode is adopted to transfer the components 77 Conversion of the multiple quantum signal of Se into the above 1 A single quantum signal of H comprising: the said 77 Direct conversion of the multiple quantum signal of Se into the said 1 H single quantum signal.
In the embodiment of the application, the direct detection of the signal in the reverse polarization stage means that no redundant time interval is added and the reverse single quantum signal is not converted into the in-phase single quantum signal. The problem of signal attenuation is considered here, and in the prior art, the use of 1 H and 13 the relation between C is qualitatively researched, and the requirement of the qualitative process on the sensitivity is low, so that the attenuation of the signal in a long time interval does not need to be considered.Similarly, the conversion of the inverted signal into the single quantum signal requires a long time interval to convert, and the signal is attenuated in the process, so that in the implementation of the scheme, the inverted signal is not converted into the in-phase single quantum signal, thereby achieving the effect of improving the accuracy of the result.
Further, the performing of quantitative data evaluation of the organic selenium compound comprises: quantitative data evaluation of the organic selenium compound is completed by a sampling mode.
In the embodiment of the application, the reverse polarization stage does not convert the anti-phase single-quantum signal into the in-phase single-quantum signal for the purpose of reducing signal attenuation, so that in the sampling stage, if 77 The Se signal adopts decoupling pulse, and the signal obtained in the last stage is in phase opposition, so that the decoupling pulse counteracts the positive value and the negative value of the phase opposition signal, and finally, the signal loss is caused, and the sampling result is difficult to obtain.
Further, the polarization transfer includes a gradient field, which gradient field is denoted as GPZ1; the evolution stage includes a gradient field, which gradient field is denoted as GPZ2; the reverse polarization phase includes a gradient field, which gradient field is denoted as GPZ3; the amplitude ratio of the three gradient fields is: GPZ1 GPZ2 gpz3=70.00: 30.00:59.07.
in the embodiment of the application, the gradient field is used as a magnetic field, and the magnetic field has the function of dispersing signals and then refocusing the signals, so as to improve the resolution and the sensitivity of the signals.
In a second aspect, embodiments of the present application provide a method of quantifying 1 H- 77 The Se qHMBC pulse sequence detection device comprises: the device completes the quantification of the organic selenium compound according to the phase sequence of polarization transfer, constant time evolution, reverse polarization transfer and quantitative evaluation; the dosing process of the device is performed according to the method provided by the first aspect of the application.
In a third aspect, an embodiment of the present application provides an electronic device, including: the device comprises a processor, a memory and a bus, wherein the processor and the memory complete communication with each other through the bus; the memory stores program instructions executable by the processor, the processor invoking the program instructions to perform the method of the first aspect.
In a fourth aspect, embodiments of the present application provide a non-transitory computer readable storage medium comprising: the non-transitory computer-readable storage medium stores computer instructions that cause the computer to perform the method of the first aspect.
Additional features and advantages of the application will be set forth in the description which follows, and in part will be apparent from the description, or may be learned by practice of the embodiments of the application. The objectives and other advantages of the application will be realized and attained by the structure particularly pointed out in the written description and claims thereof as well as the appended drawings.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments of the present application will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present application and should not be considered as limiting the scope, and other related drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow chart of each stage of the embodiment of the application;
FIG. 2 is a pulse sequence design of the present application;
FIG. 3 is a schematic diagram of a nuclear magnetic resonance apparatus according to the present application;
fig. 4 is a schematic diagram of an entity structure of an electronic device according to an embodiment of the present application.
Detailed Description
The technical solutions in the embodiments of the present application will be described below with reference to the accompanying drawings in the embodiments of the present application.
The method can be applied to quantitative research of organic small molecules under the condition of complex matrixes, and the quantitative two-dimensional nuclear magnetic method can solve the problem of signal overlapping in quantitative detection of the organic small molecules under the condition of complex matrixesThe questions are given. 1 H- 77 SeqHMBC spectrum can convert one-dimensional hydrogen signal into two-dimensional plane, and the signal distribution range of indirect dimension is along with 77 The signal distribution range of Se is correspondingly enlarged, so that the problem of spectrum peak overlapping in nuclear magnetic resonance hydrogen spectrum is effectively solved. In the high energy process, after the nuclei are magnetically resonated to a stable high energy state under the action of an applied radio frequency pulse RF (B1), the relaxation effect (the relaxation process is called a relaxation process, that is, a physical state recovery process) and a longer pulse sequence can cause an influence factor of sensitivity reduction from the moment of disappearance of the applied radio frequency to the moment of restoring to the moment before the magnetic resonance, and a corresponding solution is provided and a novel pulse sequence is developed.
FIG. 1 is a schematic flow chart of each stage of the embodiment of the present application, as shown in FIG. 1, the method includes:
step 101: polarization transfer stage: by means of polarization transfer 1 Conversion of H single quantum signals 77 Se multiple quantum signals.
In a specific implementation of step 101, magnetization from the nuclei is achieved at this stage by using excitation pulses to induce polarization transfer 1 Single quantum signal to rare nucleus of H 77 Conversion between Se multiple quantum signals, wherein nuclei and rare nuclei refer to the rarity of the corresponding isotopes in nature, the rare isotopes in nature are called rare nuclei, and the rich isotopes in nature are called nuclei signals 1 Conversion of H single quantum signals 77 Se multiple quantum signals. The stage starts to carry out polarization transfer under the action of excitation pulse, and when the stage is finished, single quantum signals are transferred to 77 Multiple quantum signals of Se.
Step 102: in the evolution stage, through an evolution mode, the method comprises the following steps of 1 H and 77 and the coupling relation of Se signals and inhibiting the evolution among homonuclear atoms in the organic matters.
In a specific implementation, when the signal is concentrated 77 After Se, an indirect dimension is established,generating energy to embody 1 H and 77 two-dimensional map of remote coupling relationship between Se. In the polarization transfer phase only the signal is concentrated 77 Se, evolution stage is 77 The Se signal itself changes in nature.
Step 103: a reverse polarization stage for transferring the light beam by reverse polarization 77 Conversion of the multiple quantum signal of Se into the above 1 H single quantum signals.
In a specific implementation process, magnetization from rare nuclei is realized at the stage through polarization transfer 77 Multiple quantum to plump core of Se 1 The conversion between the inverted single quanta of H can be understood as the signal vibration frequency of the quanta is defined by 77 Conversion of Se frequency to 1 Frequency of H. Only at 77 The Se multi-quantum signal is added with 90-degree pulse, thereby achieving the effect of reverse polarization.
Step 104: and a quantitative evaluation stage, wherein quantitative data evaluation of the organic selenium compound is completed.
In a specific implementation process, the phase is obtained by using polarization transfer, evolution and reverse polarization transfer in the steps 1 H and 77 and (3) carrying out sampling treatment on the reversed-phase single quantum signal according to a remote coupling relation between Se, so as to finish the quantification of the organic selenium compound.
In step 101, an excitation pulse is used, the purpose of which is to achieve a 90 ° flip effect, thus in the first 77 In the 90 ° pulse implementation of Se, as long as the selective excitation pulse capable of achieving the 90 ° flip effect can be used, it is possible to use a combination pulse and an adiabatic pulse (a combination pulse refers to a system of providing a plurality of different coded signals by a specified pulse or tone, the determining factor of the coding is two or more pulse counts, and the classification of the adiabatic pulse and the non-adiabatic pulse is divided according to the uniform attribute of the radio frequency pulse), which includes: eburp2, G4, gauss1-90, pc9-4-90, Q5, service, sinc1, squa100, squaramp.20.
Also in step 101 above, the signal is transmitted from 1 Conversion of H single quantum signals 77 The method used in the Se channel process can adopt a remote coupling method, according to the scheme 1 H atoms 77 The remote coupling time is suitable for the coupling constant of the two and three bonds because of the characteristic of Se atoms, the time interval is set to be 0.5-0.02s, and correspondingly, the distribution range of remote coupling is the inverse of the remote coupling time interval, so that the distribution range of remote coupling is set to be 2-50Hz.
In step 102, a constant time evolution method may be used to suppress homonuclear evolution in the indirect dimension, where homonuclear evolution refers to evolution between homonuclear atoms, such as H-H, se-Se.
In the above step 103, it should be noted that, during the implementation of this step, no extra time interval is added, but a very short time interval is used, because HMBC is used in the prior art for qualitative analysis using the coupling relationship between H-cs, and in this process, the requirement for time interval is not made because the qualitative study has a low requirement for sensitivity. In this scheme, quantitative studies are performed, and in consideration of the sensitivity requirement of the low concentration signal, an extremely short time interval is used, thereby eliminating the influence of attenuation of the signal during a long time interval. Similarly, because the signal attenuation can occur in the process of converting the inverted single-quantum signal into the in-phase single-quantum signal, the inverted single-quantum signal is not converted into the in-phase single-quantum signal in the reverse polarization stage, so that the effect of improving the measurement sensitivity of the scheme is achieved.
In step 104, since the inverted single quantum signal is not converted in step 103, a non-decoupling pulse signal is selected here to prevent the decoupling pulse from counteracting the inverted single quantum signal, so that the signal is lost after being counteracted.
In the processes of steps 101-103, namely, the polarization transfer stage, the evolution stage and the reverse polarization transfer stage, gradient fields are added in each stage, and the gradient fields have the effects of dispersing signals in organic matters and then refocusing, so that noise signals are suppressed by using the method, and the resolution and sensitivity of the signals are improved. In this scheme, the gradient ratio that can achieve the best effect of signal selection is set as GPZ 1:gpz2:gpz3=70.00: 30.00:59.07, wherein GPZ1 represents the gradient field of the polarization transfer phase, GPZ2 represents the gradient field of the evolution phase, and GPZ3 represents the gradient field of the reverse polarization phase.
Fig. 2 is a pulse sequence design diagram of the present embodiment:
wherein T is ct Is the time interval adopted by the constant time evolution stage, d 0 Is an incremental time interval, time interval T ct Time domain point number of evolution x time interval of increment, G 1 ,G 2 ,G 3 The gradient field of the polarization transfer stage, the gradient field of the evolution stage and the gradient field of the reverse polarization stage are respectively corresponding. The concept of gradient field is popular knowledge in nuclear magnetic resonance field, in this scheme, the ratio of the three gradients is set as follows: g 1 :G 2 :G 3 =70.00: 30.00:59.07, which can suppress noise signals and improve sensitivity, and the noise source is mainly thermal noise in the instrument.
In fig. 2, first, give 1 The H signal emits an excitation pulse, which is a 90 deg. rectangular pulse 201, under excitation of which a single quantum signal (not shown) is generated. Then at 77 The Se channel gives an excitation pulse 203, here a 90 ° selective pulse, comprising: eburp2, G4, gauss1-90, pc9-4-90, Q5, service, sinc1, squa100, squaramp.20. Under the influence of the excitation pulse 203, a multi-quantum signal (not shown) is generated, which then enters the evolution stage. Wherein T is represented in FIG. 2 ct -d 0 It is understood that a constant buffer time is a dependent variable, and the independent variable is d 0 ，T ct -d 0 The effect of (c) can be regarded as being on d 0 The buffer of the change ensures that the total time of the whole evolution process is a constant value. In the course of the evolution process, 1 the H signal will have a second excitation pulse, which is a rectangular pulse 205 of 180 deg., which is then passed through 2d after evolution has begun 0 At time 210 of (1) 77 The Se signal uses the next excitation pulse207, which is a 90 deg. rectangular pulse, is counter polarized by the action of the pulse 207, producing an inverted single quantum signal (not shown). Line graph 220 after the evolution stage of fig. 2 reflects the process of signal sampling.
Referring to fig. 3, fig. 3 illustrates a schematic structure of a nmr apparatus 300 according to an embodiment of the application; the apparatus 300 may be a module, a program segment, or code on an electronic device. It should be understood that the apparatus 300 corresponds to the above embodiment of the method of fig. 1, and is capable of executing the steps involved in the embodiment of the method of fig. 1, and specific functions of the apparatus 300 may be referred to in the description of the related embodiments of the present application above, and are omitted here as appropriate to avoid repetition.
The nuclear magnetic resonance apparatus 300 includes a polarization transfer module 301 for transferring 1 Conversion of H single quantum signals 77 A multiple quantum signal of Se signal; under the specific action process of the module 301, the magnetization secondary nucleus enlargement is realized 1 Single quantum signal to rare nucleus of H 77 Conversion between multiple quantum signals of Se, the signals being derived from 1 Conversion of H single quantum signals 77 Se multiple quantum signals.
An evolution module 302 for acquiring 1 H and 77 and the coupling relation of Se signals and inhibiting evolution among homonuclear atoms in the organic matters. Module 302 concentrates the signals to 77 After Se multiple quantum signal, let 77 Se evolves to establish an indirect dimension, the evolution of which can be reflected 1 H and 77 two-dimensional map of remote coupling relationship between Se. Polarization transfer means simply concentrate the signal to 77 Se channel, evolution device is to 77 Se signal itself properties are changed.
Reverse polarization transfer module 303 for transferring 77 Conversion of multiple quantum signals of Se 1 H single quantum signal. Module 303 implements polarization transfer to achieve magnetization from rare nuclei 77 Multiple quantum to plump core of Se 1 Conversion between inverted single quanta of H, so that the signal vibration frequency of quanta is determined by 77 Conversion of Se frequency to 1 Frequency of H. The module 303 is only 77 90-degree pulse is added into the Se channel, so that the effect of reverse polarization is achieved.
A quantitative evaluation module 304 for use in 1 The H channel completes the quantification of the organic selenium compound. The module 304 uses the polarization transfer, evolution, and reverse polarization transfer obtained in the above module 1 H and 77 and (3) carrying out sampling treatment on the reversed single quantum signal according to the coupling relation between Se, and completing quantification of the organic selenium compound.
Optionally, in an embodiment of the present application, the polarization transfer module includes:
and the coupling module realizes polarization transfer in a remote coupling mode.
1 An H signal excitation pulse module for generating a pulse signal in the following way 1 The H single quantum signal produces a 90 ° rectangular excitation pulse.
77 Se signal excitation pulse module for at 77 The Se multiple quantum signal produces a 90 DEG selective excitation pulse.
The coupling module is also used for providing a time interval of 0.5-0.02 and a distribution range of 2-50Hz when remotely coupled.
Optionally, in an embodiment of the present application, the evolution module includes:
a map generation module for controlling 77 The Se multiple quantum signal evolves from one point to produce a spectrum.
And the homonuclear evolution suppression module is used for suppressing homonuclear evolution in the evolution stage.
Optionally, in an embodiment of the present application, the reverse polarization transfer module includes:
77 se channel excitation pulse module for at 77 The Se multiple quantum signal generates a 90-degree rectangular excitation pulse, and reverse polarization occurs to generate an inverted single quantum signal.
And the signal attenuation suppression module is used for preventing the signal from being attenuated in a long time interval.
Optionally, in an embodiment of the present application, the quantitative evaluation module includes:
and the sampling module is used for collecting the inverted single quantum signal for evaluation.
Optionally, in the stages corresponding to the modules 301 to 303, that is, the polarization transfer stage, the evolution stage and the reverse polarization transfer stage, a gradient field needs to be added in each stage, and the gradient field has the function of dispersing signals in an organic matter and then refocusing the signals, so as to improve the resolution and the sensitivity of the signals. In the present apparatus, the gradient ratio capable of achieving the optimum effect of signal selection is set as GPZ 1:gpz2:gpz3=70.00: 30.00:59.07, wherein GPZ1 represents the gradient field of the polarization transfer phase, GPZ2 represents the gradient field of the evolution phase, and GPZ3 represents the gradient field of the reverse polarization phase.
It should be understood that the apparatus corresponds to the above embodiment of the nuclear magnetic resonance method, and is capable of performing the steps involved in the above embodiment of the method, and specific functions of the apparatus may be referred to in the above description, and detailed descriptions thereof are omitted herein as appropriate to avoid redundancy. The device includes at least one software functional module that can be stored in memory in the form of software or firmware (firmware) or cured in an Operating System (OS) of the device.
Referring to fig. 4, fig. 4 shows a schematic structural diagram of an electronic device according to an embodiment of the present application.
An electronic device 400 provided in an embodiment of the present application includes: a processor 401 and a memory 402, the memory 402 storing machine-readable instructions executable by the processor 401, which when executed by the processor 401 perform the method as described above.
The embodiment of the application also provides a storage medium, wherein a computer program is stored on the storage medium, and the computer program is executed by a processor to execute the method.
The storage medium may be implemented by any type of volatile or nonvolatile Memory device or combination thereof, such as static random access Memory (Static Random Access Memory, SRAM), electrically erasable Programmable Read-Only Memory (Electrically Erasable Programmable Read-Only Memory, EEPROM), erasable Programmable Read-Only Memory (Erasable Programmable Read Only Memory, EPROM), programmable Read-Only Memory (PROM), read-Only Memory (ROM), magnetic Memory, flash Memory, magnetic disk, or optical disk. In the embodiments of the present application, it should be understood that the disclosed apparatus and method may be implemented in other manners. The apparatus embodiments described above are merely illustrative, for example, of the flowcharts and block diagrams in the figures that illustrate the architecture, functionality, and operation of possible implementations of apparatus, methods and computer program products according to various embodiments of the present application. In this regard, each block in the flowchart or block diagrams may represent a module, segment, or portion of code, which comprises one or more executable instructions for implementing the specified logical function(s). It should also be noted that, in some alternative implementations, the functions noted in the block may occur out of the order noted in the figures. For example, two blocks shown in succession may, in fact, be executed substantially concurrently, or the blocks may sometimes be executed in the reverse order, depending upon the functionality involved. It will also be noted that each block of the block diagrams and/or flowchart illustration, and combinations of blocks in the block diagrams and/or flowchart illustration, can be implemented by special purpose hardware-based systems which perform the specified functions or acts, or combinations of special purpose hardware and computer instructions.
In addition, the functional modules of the embodiments of the present application may be integrated together to form a single part, or the modules may exist separately, or two or more modules may be integrated to form a single part.
In this document, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions.
The above description is only an example of the present application and is not intended to limit the scope of the present application, and various modifications and variations will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (12)
1. A method of nuclear magnetic resonance, characterized by using 1 H- 77 The Se qHMBC pulse sequence is used for quantitatively detecting the organic selenium compound, and the method comprises the following steps:
polarization transfer stage: by means of polarization transfer 1 Conversion of H single quantum signals 77 A Se multiple quantum signal;
evolution stage: by evolution mode, obtain 1 H and 77 coupling relation of Se signals and inhibiting evolution among homonuclear atoms of the organic selenium compound;
reverse polarization transfer stage: said transfer is performed by reverse polarization 77 Conversion of Se multiple quantum signals into the above 1 H single quantum signals; and
quantitative evaluation phase: quantitative data evaluation of the organic selenium compound was completed.
2. The method according to claim 1, wherein the polarization transfer is performed by 1 Conversion of H single quantum signals 77 Se multiple quantum signal, comprising:
polarization transfer is realized through a remote coupling mode;
wherein, 1 the first excitation pulse of the H signal is a 90-degree rectangular pulse;
wherein the first one 77 90 ° pulse realizations of Se employ 90 ° selective excitation pulses.
3. The method according to claim 2, characterized in that in the remote coupling mode, the time interval for remote coupling evolution is 0.5 to 0.02s.
4. The method of claim 2, wherein the selective excitation pulse is set to a frequency that selects a spectral width in the range of 300 ppm; and the selected pulse is any selectively activated pulse that achieves a 90 deg. flip effect.
5. The method according to claim 1, wherein the transfer of the reverse polarization is performed by 77 Conversion of Se multiple quantum signals 1 A single quantum signal of H comprising:
using only rectangular pulses in the reverse polarisation phase, the method will 77 Conversion of Se multiple quantum signals 1 H single quantum signal.
6. The method according to claim 1, wherein said transferring said reverse polarization is performed by 77 Conversion of Se multiple quantum signals into the above 1 A single quantum signal of H comprising:
the said 77 Direct conversion of Se multiple quantum signals into the said 1 H single quantum signal.
7. The method according to claim 1, wherein the acquisition is performed by evolution means 1 H and 77 coupling relationship of Se signals and inhibiting evolution among homonuclear atoms of the organic selenium compound, comprising:
let the 77 Se channel multi-quantum signal evolution generation energy embodiment 1 H and 77 a two-dimensional spectrogram of a remote coupling relation between Se;
and adopting a constant time evolution method to inhibit evolution among homonuclear atoms in the organic selenium compound.
8. The method of claim 1, wherein said performing quantitative data evaluation of said organic selenium compound comprises:
quantitative data evaluation of the organic selenium compound is completed by a sampling mode.
9. The method according to any one of claims 1 to 8, wherein,
polarization transfer includes a gradient field, denoted as GPZ1;
the evolution stage includes a gradient field, which gradient field is denoted as GPZ2;
the reverse polarization phase includes a gradient field, which gradient field is denoted as GPZ3;
the amplitude ratio of the three gradient fields is as follows: GPZ1 GPZ2 gpz3=70.00: 30.00:59.07.
10. a nuclear magnetic resonance apparatus, characterized by using 1 H- 77 Quantitative detection of organic selenium compounds by Se qHMBC pulse sequence, the device comprising:
a polarization transfer module for transferring the polarization of the light to the light source by a polarization transfer mode 1 Conversion of H single quantum signals 77 A Se multiple quantum signal;
the evolution module is used for obtaining through an evolution mode 1 H and 77 coupling relation of Se signals and inhibiting evolution among homonuclear atoms of the organic selenium compound;
a reverse polarization transfer module for transferring the light beam in reverse polarization mode 77 Conversion of Se multiple quantum signals into the above 1 H single quantum signals; and
quantitative evaluation module: for performing quantitative data evaluation of the organic selenium compound.
11. An electronic device, comprising: a processor and a memory storing machine-readable instructions executable by the processor to perform the method of any one of claims 1 to 9 when executed by the processor.
12. A storage medium having stored thereon a computer program which, when executed by a processor, performs the method of any of claims 1 to 9.
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