CN106841270B - A kind of method for obtaining nuclear magnetic resonance two dimension phase sensitivity J spectrums - Google Patents
A kind of method for obtaining nuclear magnetic resonance two dimension phase sensitivity J spectrums Download PDFInfo
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- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
Abstract
A kind of method for obtaining nuclear magnetic resonance two dimension phase sensitivity J spectrums.Testing sample is loaded into nuclear magnetic tube, and the nuclear magnetic tube after dress sample is sent into the test chamber of nuclear magnetic resonance spectrometer；The one-dimensional hydrogen spectrum of the one-dimensional hydrogen spectrum pulse sequence acquisition of allocating conventional, obtains signal peak distribution and spectrum width information, and measure non-selective 90 ° of RF pulse widths；The two-dimentional phase sensitivity J spectrum pulse trains of compiling are imported on nuclear magnetic resonance chemical analyser device, open the weak slice selective gradient composite module of chirp pulses and two-dimentional phase sensitivity J spectrum pulse train J sampling modules of two-dimentional phase sensitivity J spectrums pulse train；Two-dimentional phase sensitivity J spectrums pulse train experiment parameter is set, after checking experiment parameter setting is errorless, performs data sampling；After the completion of data acquisition, corresponding data splicing and two-dimensional Fourier transform are carried out, obtains a two-dimensional frequency spectrum comprising J coupling information and chemical shift information；Two-dimentional phase sensitivity processing is carried out to obtained two-dimensional frequency spectrum, can obtain a two-dimentional phase sensitivity J spectrum.
Description
Technical field
The present invention relates to nuclear magnetic resonance (NMR, Nuclear Magnetic Resonance) Wave Spectrum detection method, especially
It is related to a kind of method that nuclear magnetic resonance two dimension phase sensitivity J spectrums are obtained by the design of simple pulse train and data post processing mode.
Background technology
The separation of J coupling information and chemical shift information can be achieved in nuclear magnetic resonance two dimension J spectrums (2D J spectroscopy)
And by both presentation of information in two spectrogram dimensions, contribute to the identification of the crowded compound of spectral peak and spectral peak in one-dimensional spectrogram
Ownership, simplify spectrum analysis.Conventional two-dimentional J spectral methods tie up by the indirect dimension evolution phase and directly sampling period phase due to its signal
The influence of position modulation so that the final two-dimentional J spectrums spectral peak of gained suffers from the phase twist in two dimension directions, and this phase is turned round
Triton Chang Wufa operates to obtain by simple phase modulation to be improved so as to realize the display of phase sensitive mode.Therefore conventional two-dimentional J spectrums
All it is to avoid being shown on spectrogram for spectral peak phase twist from influenceing with absolute value display pattern, but absolute value display pattern is brought
Spectral peak width broadening and the application that conventional two-dimentional J spectral methods are limited the problem of be coupled pseudo- peak by force.
The content of the invention
It is an object of the invention to provide can effectively solve spectral peak width broadening under conventional two-dimentional J spectrums absolute value display pattern
A kind of method of acquisition nuclear magnetic resonance two dimension phase sensitivity J spectrums of pseudo- peak problem is coupled by force.
A kind of method for obtaining nuclear magnetic resonance two dimension phase sensitivity J spectrums, comprises the following steps：
1) testing sample is loaded into nuclear magnetic tube, and the nuclear magnetic tube after dress sample is sent into the test chamber of nuclear magnetic resonance spectrometer；
2) the one-dimensional hydrogen spectrum of the one-dimensional hydrogen spectrum pulse sequence acquisition of allocating conventional, obtains signal peak distribution and spectrum width information, and survey
Measure non-selective 90 ° of RF pulse widths；
3) the two-dimentional phase sensitivity J spectrum pulse trains of compiling are imported on nuclear magnetic resonance chemical analyser device, open two-dimentional phase sensitivity J spectrums arteries and veins
Rush the weak slice selective gradient composite module of chirp pulses and two-dimentional phase sensitivity J spectrum pulse train J sampling modules of sequence；
4) set two-dimentional phase sensitivity J spectrums pulse train experiment parameter, after checking experiment parameter setting is errorless, perform data and adopt
Sample；
5) after the completion of data acquisition, corresponding data splicing and two-dimensional Fourier transform are carried out, one is obtained and includes J idols
Close information and the two-dimensional frequency spectrum of chemical shift information；
6) two-dimentional phase sensitivity processing is carried out to obtained two-dimensional frequency spectrum, can obtain a two-dimentional phase sensitivity J spectrum.
In step 2), the one-dimensional hydrogen spectrum pulse train of routine is the single pulse train that nuclear magnetic resonance spectrometer carries, only
It is made up of non-selective 90 ° of radio-frequency pulse.The one-dimensional hydrogen spectrum for sampling to obtain by the pulse train can directly obtain corresponding
Sample spectral peak is distributed and spectrum width information.Make magnetization vector pulse as corresponding to longitudinal direction is turned to transverse plane by measurement
Non-selective 90 ° of RF pulse widths can be measured with the time.
In step 3), the weak slice selective gradient composite module of chirp pulses of the two-dimentional phase sensitivity J spectrums pulse train is by one
Individual low-angle excites the weak slice selective gradient composition of chirp pulses collocation one, can be produced by this pulse and gradient combination module
Encourage echo mechanism, so as to realize the reunions of J coupling effects in directly dimension sampling period, by reunion J coupling effects letter
Pure chemistry displacement information can be obtained in indirect dimension by number carrying out data splicing, constitute the chemical shift information dimension of two-dimentional J spectrums；It is described
The J sampling modules of two-dimentional phase sensitivity J spectrums pulse train are by a series of sampling period t in short-term2Form, pass through with non-selection 180 ° of pulses
Constantly repeat upset magnetization vector and realize the reunion of chemical shift evolution information, finally obtain J coupling information, structure in directly dimension
Into the J coupling information dimensions of two-dimentional J spectrums.
In step 4), the two-dimentional phase sensitivity J spectrums pulse train experiment parameter includes non-selective 90 ° of RF pulse-to-pulse chong channels
Wide, directly dimension samples spectrum width SW, in short-term time sampling period t2, dimension spectrum width SW1, indirectly dimension sampling number ni, J sampling module indirectly
Sampling number np1, J adopt module repeat the weak slice selective gradient composite module of number N, chirp pulse in chirp pulse excitations angle [alpha],
Chirp pulse widths, chirp pulses scan width, weak slice selective gradient G2And its action time, phase dry separation gradient G1And its make
Use the time.The detailed process of the data sampling is：First non-selection 90 ° of pulse excitation magnetization vector is by longitudinal direction first
Transverse plane is gone to, the Mxy of the right non-selection 180 ° of Excited by Laser Pulses Pair in Two-Level System of the latter overturn in plane；Then, two
The weak slice selective gradient composite module of chirp pulses of dimension phase sensitivity J spectrum pulse trains develops to the Mxy；Finally,
The sampled signal in J sampling modules.Above-mentioned pulse train implementation procedure is to the once sampling of dimension points indirectly, for one
Full two-dimensional phase sensitivity J modal datas need to repeat above-mentioned sequence implementation procedure ni times.
In step 5), the process of the data splicing and two-dimensional Fourier transform is as follows：(a) to sampling obtained ni
× N number of echo data is ranked up, and extracts data points corresponding in the 1/SW1 times before each echo data；(b) according to ni
Order will count before corresponding echo data and be spliced in the 1/SW1 times, obtain new echo data of one group of points for np, and
N times are repeated, finally obtain new np × N 2-D data；(c) two-dimentional Fourier's change is carried out to new np × N 2-D datas
Get in return to a two-dimensional frequency spectrum comprising J coupling information and chemical shift information.
In step 6), the detailed process of the two-dimentional phase sensitivity processing is as follows：(a) two dimension frequency described in a step 5 is replicated
Rate is composed, and it is tieed up into spectrum center along F1 and does a mirror image operation, obtains the two-dimensional frequency spectrum of a F1 dimension reversion；(b) by institute
The two-dimensional frequency spectrum for obtaining F1 dimension reversions is added with original two-dimensional frequency spectrum, and it is zero to obtain a F1 dimension spectral peak phase recovery
New two-dimensional frequency spectrum；(c) F2 dimension phase phase modulation is carried out to obtained new two-dimensional frequency spectrum so that F2 dimension spectral peak phases also revert to
Zero, it is final to obtain a nuclear magnetic resonance two dimension phase sensitivity J spectrum without phase twist.
Compared with the two-dimentional J of routine decomposes spectral method, the present invention passes through pulse train design and corresponding Data Post
Technology, which proposes, a kind of can overcome J spectrum signals phase twist so as to realize the method for two-dimentional phase sensitivity J spectrums that phase sensitive mode shows.
This method can effectively improve the spectra resolution rate of two-dimentional J spectrum, overcome absolute value show caused by be coupled pseudo- peak by force to spectrogram
The spectra resolution rate of J spectrums is further improved while interfering, further improves the spectrogram quality of two-dimentional J spectrums, extending it should
With scope, it is favorably improved J and decomposes application of the spectral technology in practical systems.
Brief description of the drawings
Fig. 1 is the pulse sequence diagram for being used to obtain nuclear magnetic resonance two dimension phase sensitivity J spectrums proposed by the invention.
Fig. 2 is the echo data schematic diagram that a full experiment collects.Wherein black dotted lines frame represents first echo
Along longitudinal spliced order, spliced new echo data points are np.
Fig. 3 is the np × N two-dimensional frequency modal datas reconstructed after data are spliced.
Fig. 4 is that the two-dimentional phase sensitivity J tested using methacrylic acid fourth fat sample composes result.
Fig. 5 is dotted line frame regional enlarged drawing in Fig. 4.
Embodiment
Below in conjunction with drawings and examples, the present invention will be further described：
The instrument that the present embodiment uses is discussed for Varian 500MHz NMR spectrums, and sample is butyl methacrylate.
Used pulse train is as shown in Figure 1.Its operating procedure is as follows：
1) sample introduction：A certain amount of butyl methacrylate sample (about 0.55mL) is put into NMR spectrum view.
2) RF pulse width measures：The one-dimensional hydrogen spectral sequence (SPULS) for calling spectrometer to carry measures the non-selection of sample
Property 90 ° of frequency pulse widths be 14.35 μ s, obtain formant distribution and spectrum width information, set the spectrogram center to be according to obtained information
Pulse excitation center.
4) test of pulse sequence is imported：The two-dimentional phase sensitivity J spectrum arteries and veins of designed compiling is imported on nuclear magnetic resonance chemical analyser device
Sequence (as shown in Figure 1) is rushed, opens the weak slice selective gradient composite module of chirp pulses and J sampling modules of this pulse train.
5) pulse train parameters and sampling are set：
It is 10000Hz that parameter setting, which includes directly tieing up spectrum width SW, in short-term sampling period t2For 10.75ms, spectrum width SW1 is tieed up indirectly
For 100Hz, it be that 70, J sampling module sampling numbers np1 is that to adopt module repetition number N be 90 to 215, J to tie up sampling number ni indirectly,
Chirp pulse excitations angle [alpha] is 18 °, chirp pulse widths 30ms, chirp pulse scan width 10000Hz, weak slice selective gradient
G2For 0.8G/cm, its action time is 30ms, phase dry separation gradient intensity value G1For 24.0G/cm, its action time is 1.5ms.
After pulse train parameters are set, data sampling is performed.A sequential sampling is often performed, can obtain once what dimension indirectly was counted
Sampled data, 70 dimension evolutions indirectly are repeated to the sample.Whole experiment process data acquisition time is about 2min.
6) Data Post：
Data Post includes data splicing and two-dimensional Fourier transform processing and the processing of two-dimentional phase sensitivity.Wherein data are spliced
And two-dimensional Fourier transform processing is specific as follows：(a) 70 × 90 echo datas for sampling to obtain are ranked up along longitudinal direction,
Extract corresponding data points (as shown in Figure 2) in the preceding 1/SW1 times of each echo data；(b) order according to longitudinal ni
Spliced being counted in the 1/SW1 times before corresponding echo data, obtain the new echo data that one group of points is np, and repeat N
It is secondary, finally obtain new np × N 2-D data (as shown in Figure 3)；(c) two-dimentional Fu is carried out to new np × N 2-D datas
In leaf transformation obtain one comprising J coupling information and chemical shift information two-dimensional frequency spectrum.Two-dimentional phase sensitivity processing is specific as follows：
(a) a above-mentioned two-dimensional frequency spectrum is replicated, and it is tieed up into spectrum center along F1 and does a mirror image operation, obtains a F1 dimension reversion
Two-dimensional frequency spectrum；(b) the two-dimensional frequency spectrum that obtained F1 is tieed up to reversion is added with original two-dimensional frequency spectrum, obtains one, ground
The new two-dimensional frequency spectrum that F1 dimension spectral peak phase recoveries are zero；(c) it is phase phase modulation to carry out F2 to obtained new two-dimensional frequency spectrum so that
F2 dimension spectral peak phases also revert to zero, and the final nuclear magnetic resonance two dimension phase sensitivity J spectrums for obtaining a methacrylic acid fourth fat sample are (such as
Shown in Fig. 4).From two-dimentional phase sensitivity J spectrums shown in Fig. 4 as can be seen that the two-dimentional spectrogram is shown with High-Resolution Spectral with phase sensitive mode
Figure information, chemical shift and J are coupled on two dimension directions the influence without phase-modulation and are coupled the interference at pseudo- peak by force.Simultaneously
In the two-dimentional phase sensitivity J spectrums, the multiplet comprising small J couplings that dotted line frame is marked is amplified (as shown in Figure 5), can
To obtain accurate J couplings information, as spectral peak splits merotype and J coupling constants.
In summary, the invention provides a kind of method of the two-dimentional phase sensitivity J spectrums of new acquisition, low-angle chirp arteries and veins is utilized
The weak slice selective gradient of punching collocation produces excitation echo mechanism and realizes that J couplings are met again in direct sampling period, passes through the J couplings to being obtained
Reunion free induction decay signal, which carries out data splicing, to obtain pure chemistry displacement information in dimension acquisition indirectly.Meanwhile by adopting
J sampling modules used in the sample phase can obtain J coupling information in directly dimension.Further using two-dimentional phase sensitivity treatment technology to this two
Tie up frequency spectrum and carry out Data Post, it is final to obtain a nuclear magnetic resonance two dimension phase sensitivity J spectrum.
The present invention produces excitation echo mechanism using the weak slice selective gradient of single chirp pulses collocation and realized in direct sampling period
J couplings are met again, and data splicing is carried out by being coupled reunion free induction decay signal to the J obtained, can be obtained in indirect dimension
Pure chemistry displacement information.Meanwhile J can be obtained in directly dimension by J sampling modules used in sampling period and be coupled information.By two
Tieing up Fourier transformation can be associated this two dimensions of information and obtain a two-dimensional frequency spectrum.Dimension letter indirectly is composed according to the two-dimensional frequency
The symmetry of breath, the two-dimensional frequency is composed using a kind of new two-dimentional phase sensitivity treatment technology and carries out Data Post, it is final to obtain
One nuclear magnetic resonance two dimension phase sensitivity J spectrum.Compared with the two-dimentional J spectral methods of routine, institute's extracting method of the present invention can make spectra resolution rate
Improve twice, while can avoid being coupled influence of the pseudo- peak to spectrogram by force, be favorably improved J and decompose spectral technology in practical systems
Using.
Claims (6)
- A kind of 1. method for obtaining nuclear magnetic resonance two dimension phase sensitivity J spectrums, it is characterised in that comprise the following steps：1) testing sample is loaded into nuclear magnetic tube, and the nuclear magnetic tube after dress sample is sent into the test chamber of nuclear magnetic resonance spectrometer；2) the one-dimensional hydrogen spectrum of the one-dimensional hydrogen spectrum pulse sequence acquisition of allocating conventional, obtains signal peak distribution and spectrum width information, and measure non- 90 ° of RF pulse widths of selectivity；3) the two-dimentional phase sensitivity J spectrum pulse trains of compiling are imported on nuclear magnetic resonance chemical analyser device, open two-dimentional phase sensitivity J spectrums pulse sequence The weak slice selective gradient composite module of chirp pulses of row and two-dimentional phase sensitivity J spectrum pulse train J sampling modules；The weak slice selective gradient composite module of chirp pulses of the two-dimentional phase sensitivity J spectrums pulse train is excited by a low-angle The weak slice selective gradient composition of chirp pulses collocation one, excitation echo mechanism can be produced by this pulse and gradient combination module, So as to realize the reunions of J coupling effects in directly dimension sampling period, by the signals of reunion J coupling effects carry out data splicing Pure chemistry displacement information can be obtained in indirect dimension, constitute the chemical shift information dimension of two-dimentional J spectrums；The two-dimentional phase sensitivity J spectrums arteries and veins The J sampling modules for rushing sequence are by a series of sampling period t in short-term2Formed with non-selection 180 ° of pulses, by constantly repeating to overturn Magnetization vector and the reunion for realizing chemical shift evolution information, J coupling information finally is obtained in directly dimension, constitute two-dimentional J spectrums J coupling information dimension；4) two-dimentional phase sensitivity J spectrums pulse train experiment parameter is set, after checking experiment parameter setting is errorless, performs data sampling；5) after the completion of data acquisition, corresponding data splicing and two-dimensional Fourier transform are carried out, one is obtained and includes J coupling letters The two-dimensional frequency of breath and chemical shift information is composed；6) two-dimentional phase sensitivity processing is carried out to obtained two-dimensional frequency spectrum, can obtain a two-dimentional phase sensitivity J spectrum.
- A kind of 2. method for obtaining nuclear magnetic resonance two dimension phase sensitivity J spectrums as claimed in claim 1, it is characterised in that in step 2), The one-dimensional hydrogen spectrum pulse train of routine is the single pulse train that nuclear magnetic resonance spectrometer carries, and is only penetrated by one non-selective 90 ° Frequency pulse is formed；The one-dimensional hydrogen spectrum for sampling to obtain by the pulse train can directly obtain corresponding sample spectral peak distribution and spectrum width letter Breath；Magnetization vector pulse operating time as corresponding to longitudinal direction is turned to transverse plane is set to measure by measurement non-selective 90 ° of RF pulse widths.
- A kind of 3. method for obtaining nuclear magnetic resonance two dimension phase sensitivity J spectrums as claimed in claim 1, it is characterised in that in step 4), The two-dimentional phase sensitivity J spectrum pulse train experiment parameter include non-selective 90 ° of radio-frequency pulse pulsewidths, directly dimension sample spectrum width SW, Time sampling period t in short-term2, indirectly dimension spectrum width SW1, dimension sampling number ni, J sampling module sampling number np1, J adopts module indirectly Repeat chirp pulse excitations angle [alpha], chirp pulse widths, chirp in the weak slice selective gradient composite module of number N, chirp pulse Pulse scan width, weak slice selective gradient G2And its action time, phase dry separation gradient G1And its action time.
- A kind of 4. method for obtaining nuclear magnetic resonance two dimension phase sensitivity J spectrums as claimed in claim 1, it is characterised in that in step 4), The detailed process of the data sampling is：(1) first non-selection 90 ° of pulse excitation magnetization vector goes to transverse plane by longitudinal direction, and right the latter is non-selection The Mxy of 180 ° of Excited by Laser Pulses Pair in Two-Level System overturn in plane；(2) the weak slice selective gradient composite module of chirp pulses of two-dimentional phase sensitivity J spectrums pulse train is drilled the Mxy Change；(3) sampled signal in J sampling modules, two-dimentional phase sensitivity J spectrum pulse trains implementation procedure is simply to once dimension is counted indirectly Sampling, need to compose pulse train implementation procedure to two-dimentional phase sensitivity J for full two-dimensional phase sensitivity J modal data and repeat ni times.
- A kind of 5. method for obtaining nuclear magnetic resonance two dimension phase sensitivity J spectrums as claimed in claim 1, it is characterised in that in step 5), The process of the data splicing and two-dimensional Fourier transform is as follows：(1) ni × N number of echo data for sampling to obtain is ranked up, extracts before each echo data institute in the 1/SW1 times Corresponding data points；(2) order according to ni will count in the 1/SW1 times before corresponding echo data is spliced, and it is np's to obtain one group of points New echo data, and n times are repeated, finally obtain new np × N 2-D data；(3) one is obtained to new np × N 2-D datas progress two-dimensional Fourier transform comprising J coupling information and chemical shift to believe The two-dimensional frequency spectrum of breath.
- A kind of 6. method for obtaining nuclear magnetic resonance two dimension phase sensitivity J spectrums as claimed in claim 1, it is characterised in that in step 6), The detailed process of the two-dimentional phase sensitivity processing is as follows：(1) two-dimensional frequency spectrum described in a step 5 is replicated, and it is tieed up into spectrum center along F1 and does a mirror image operation, obtains one Open the two-dimensional frequency spectrum of F1 dimension reversions；(2) the two-dimensional frequency spectrum that obtained F1 is tieed up to reversion is added with original two-dimensional frequency spectrum, obtains a F1 dimension spectral peak The new two-dimensional frequency spectrum that phase recovery is zero；(3) F2 dimension phase phase modulation is carried out to obtained new two-dimensional frequency spectrum so that F2 dimension spectral peak phases also revert to zero, final to obtain One nuclear magnetic resonance two dimension phase sensitivity J spectrum without phase twist.
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| CN107144591B (en) * | 2017-06-23 | 2018-11-30 | 厦门大学 | A method of measurement is independently with nuclear spin to indirect coupling mode |
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| CN110361680A (en) * | 2019-06-21 | 2019-10-22 | 厦门大学 | A kind of super-resolution nuclear magnetic resonance two dimension J decomposition spectral method |
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| CN113281366B (en) | 2021-04-02 | 2022-04-05 | 厦门大学 | Nuclear magnetic resonance phase-sensitive two-dimensional J decomposition spectrum method for inhibiting strong coupling pseudo peak |
| CN114487954B (en) * | 2022-04-14 | 2022-07-01 | 中国科学院精密测量科学与技术创新研究院 | Multichannel transmitting-receiving NMR method for accurately measuring field intensity and distribution of electromagnet |
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