CN102269721B - Sample broadband detection method applied to nuclear magnetic resonance chemical analyzer - Google Patents
Sample broadband detection method applied to nuclear magnetic resonance chemical analyzer Download PDFInfo
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- CN102269721B CN102269721B CN201110125353.0A CN201110125353A CN102269721B CN 102269721 B CN102269721 B CN 102269721B CN 201110125353 A CN201110125353 A CN 201110125353A CN 102269721 B CN102269721 B CN 102269721B
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- 238000005481 NMR spectroscopy Methods 0.000 title claims abstract description 22
- 238000001514 detection method Methods 0.000 title claims abstract description 22
- 238000012360 testing method Methods 0.000 claims abstract description 12
- 238000001228 spectrum Methods 0.000 claims abstract description 9
- 230000005311 nuclear magnetism Effects 0.000 claims description 7
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Abstract
The invention discloses a sample broadband detection method applied to a nuclear magnetic resonance chemical analyzer. The method provided by the invention comprises the following steps of: collecting a bandwidth range of a signal generated by testing the sample by the nuclear magnetic resonance chemical analyzer; selecting corresponding standard nuclear magnetic frequency spectrum parameters according to the bandwidth range of the signal; receiving a primary reference pulse and dispersing the reference pulse into a plurality of rectangular pulses by time intervals; testing the sample by the driving of the plurality of rectangular pulses to obtain signal parameters of the sample; carrying out a time inversion operation on the signal parameters according to the plurality of rectangular pulses; comparing the signal parameters with time inversion signal parameters to obtain a pulse gradient value; modulating phase and amplitude of the primary reference pulse to obtain a secondary reference pulse according to the pulse gradient value; and comparing the signal parameters with the standard nuclear magnetic frequency spectrum parameters. The method provided by the invention has the advantages of higher flexibility and wider frequency spectrum range.
Description
Technical field
The present invention relates to a kind of sample detection method, be specifically related to a kind of sample wide band detection method that is applied to nuclear magnetic resonance spectrometer.
Background technology
Nuclear magnetic resonance (NMR) is as one of biology sample detection and the most frequently used technology of medical diagnosis on disease, can be within molecular level reflects biosome or in human body the information of pathology, obviously improve the specificity of diagnosis, the early diagnosis of enhancing to dangerous disease (senile dementia, epilepsy, brain tumor, prostate cancer etc.) and the ability of curative effect monitoring.Therefore, nuclear magnetic resonance technique is that the biomedical research of 21st century enters one of important testing tool of molecular level, is one of the first-selected monitoring technique in the medical science such as molecular medicine, gene therapy forward position.
Say technically, magnetic field intensity and uniformity coefficient improve constantly, and composite pulse technology is constantly used, and miniaturization and movable type are progressively universal, are several visible trends of commercial NMR system development.
The exploitation of optimizing pulse is one of forward position of the most active research in nuclear magnetic resonance field in recent years.Along with nuclear magnetic resonance technique application more and more widely in biomacromolecule, complicated organic molecule system, the drawback of tradition pulse progressively displays, as: excite bandwidth inhomogeneous, the relaxation of sample is larger to the influence of fading of signal, and signal sensitivity is on the low side etc.And the optimization pulse of developing and designing for above problem will be expected to overcome the above problems.Traditional pulse is generally made up of rect.p., and shape is comparatively single, and effect is not satisfactory.Optimize pulse and be made up of amplitude several pulse units different with phase place, there is no fixing shape, effect can design according to different experiment purposes.
Along with the continuous expansion in nuclear magnetic resonance research field, at present for the nuclear-magnetism research of biomolecule and sample main exist be with roomy, the feature such as relaxation rate is strong, traditional pulse is difficult to solve the above problems.Optimize the exploitation of pulse, not only can solve the signals collecting problem of special system, and can be according to different experiment demands, the pulse of design specific purposes, the degree of freedom of intensifier pulse exploitation and the control ability to Nuclear Spin Systems.
Summary of the invention
The invention provides a kind of sample wide band detection method that is applied to nuclear magnetic resonance spectrometer, this sample wide band detection method sensitivity is higher; Spectral range is wider.
For achieving the above object, the technical solution used in the present invention is: a kind of sample wide band detection method that is applied to nuclear magnetic resonance spectrometer, comprising:
The bandwidth range of step 1, collection nuclear magnetic resonance spectrometer test signal that sample produces;
Step 2, select corresponding standard nuclear-magnetism frequency spectrum parameter according to the bandwidth range of described signal;
Step 3, acceptance one elementary reference pulse, and this reference pulse is discrete as some rect.p.s taking the time interval;
Step 4, sample test is obtained the signal parameter of this sample under described some rect.p.s drive;
Step 5, according to described some rect.p.s, described signal parameter is carried out to time reverse operation and obtain time reversal signal parameter;
Step 6, more described signal parameter and time reversal signal parameter obtain pulsed gradient value;
Step 7, obtain secondary reference pulse according to phase place and the amplitude of the described elementary reference pulse of described pulsed gradient value modulation; Described amplitude modulation(PAM) is operating as:
A2?=?A1?+?d?*?grad
Wherein, the amplitude that A2 is secondary reference pulse, the amplitude that A1 is elementary reference pulse, d is an a small amount of (being generally 1e-10), grad is pulsed gradient value.
Described phase-modulation is operating as:
Phi?=?arctg(Ay/Ax)
Wherein, the phase place that Phi is pulse, the y component value that Ay is amplitude, the x component value that Ax is amplitude;
Step 8, more described signal parameter and standard nuclear-magnetism frequency spectrum parameter; In the time of coupling, finish; Otherwise repeating step three is to step 8;
Thereby step 9, record and the corresponding phase place of each rect.p. and amplitude form phase amplitude list, and according to this phase amplitude list output detections pulse;
Step 10, the form that becomes nuclear magnetic resonance spectrometer to identify described detection pulses switch, and input programming radio-frequency signal generator, can apply this detection pulse, tests uniformly sample parameter signal thereby obtain amplitude.
Because technique scheme is used, the present invention compared with prior art has following advantages and effect:
1, the present invention has utilized the Optimal Control Theory of engineering mathematics field widespread use, and integrate various external parameters, as: detection bandwidth, magnetic interference size, on the basis of cross relaxation intensity, further combine with numerical computation technology, the solution that is optimized in the hyperspace of pulse parameter, and with fine parameters recording impulses such as amplitude, phase place and switching times.
2, detection method of the present invention has versatility and compatibility widely, the parameters of optimizing pulse can be rewritten according to the form of the operating system using on instrument.
3, the sensitivity of pulse of the present invention improves 10%-100%, and spectral response width improves 2-5 doubly: the spectral range that traditional technology can cover is thousands of hertz, and our technology can cover ten thousand hertz of 1-2.
4, the present invention is general easy, exists in the database of shaped pulse according to certain format, later can recycled in user's use procedure, and do not need the detail of the parameter of knowing pulse.
Brief description of the drawings
Accompanying drawing 1 is process flow diagram of the present invention;
Accompanying drawing 2 is implementation result figure of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described:
Embodiment: a kind of sample wide band detection method that is applied to nuclear magnetic resonance spectrometer, is characterized in that: comprising:
The bandwidth range of step 1, collection nuclear magnetic resonance spectrometer test signal that sample produces;
Step 2, select corresponding standard nuclear-magnetism frequency spectrum parameter according to the bandwidth range of described signal;
Step 3, acceptance one elementary reference pulse, and this reference pulse is discrete as some rect.p.s taking the time interval;
Step 4, sample test is obtained the signal parameter of this sample under described some rect.p.s drive;
Step 5, according to described some rect.p.s, described signal parameter is carried out to time reverse operation and obtain time reversal signal parameter;
Step 6, more described signal parameter and time reversal signal parameter obtain pulsed gradient value;
Step 7, obtain secondary reference pulse according to phase place and the amplitude of the described elementary reference pulse of described pulsed gradient value modulation; Described amplitude modulation(PAM) is operating as:
A2?=?A1?+?d?*?grad
Wherein, the amplitude that A2 is secondary reference pulse, the amplitude that A1 is elementary reference pulse, d is an a small amount of (being generally 1e-10), grad is pulsed gradient value.
Described phase-modulation is operating as:
Phi?=?arctg（Ay/Ax）
Wherein, the phase place that Phi is pulse, the y component value that Ay is amplitude, the x component value that Ax is amplitude;
Step 8, more described signal parameter and standard nuclear-magnetism frequency spectrum parameter; In the time of coupling, finish; Otherwise repeating step three is to step 8;
Thereby step 9, record and the corresponding phase place of each rect.p. and amplitude form phase amplitude list, and according to this phase amplitude list output detections pulse;
Step 10, the form that becomes nuclear magnetic resonance spectrometer to identify described detection pulses switch, and input programming radio-frequency signal generator, can apply this detection pulse, tests uniformly sample parameter signal thereby obtain amplitude
.
The design sketch that accompanying drawing 2 is pulse, the design sketch that accompanying drawing 2B is pulse of the present invention.Horizontal ordinate is bandwidth range (Hz), the relative intensity (without numerical value unit) that ordinate is signal.The signal relative intensity of accompanying drawing 2A skewness in bandwidth range as shown in the figure, the effect of accompanying drawing 2B is greatly improved.
Above-described embodiment is only explanation technical conceive of the present invention and feature, and its object is to allow person skilled in the art can understand content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences that Spirit Essence is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.
Claims (1)
1. a sample wide band detection method that is applied to nuclear magnetic resonance spectrometer, is characterized in that: comprising:
The bandwidth range of step 1, collection nuclear magnetic resonance spectrometer test signal that sample produces;
Step 2, select corresponding standard nuclear-magnetism frequency spectrum parameter according to the bandwidth range of described signal;
Step 3, acceptance one elementary reference pulse, and this reference pulse is discrete as some rect.p.s taking the time interval;
Step 4, sample test is obtained the signal parameter of this sample under described some rect.p.s drive;
Step 5, according to described some rect.p.s, described signal parameter is carried out to time reverse operation and obtain time reversal signal parameter;
Step 6, more described signal parameter and time reversal signal parameter obtain pulsed gradient value;
Step 7, obtain secondary reference pulse according to phase place and the amplitude of the described elementary reference pulse of described pulsed gradient value modulation; Described amplitude modulation(PAM) is operating as:
A2?=?A1?+?d?*?grad
Wherein, the amplitude that A2 is secondary reference pulse, the amplitude that A1 is elementary reference pulse, d is an a small amount of, and d is specially 1e-10, and grad is pulsed gradient value;
Described phase-modulation is operating as:
Phi?=?arctg(Ay/Ax)
Wherein, the phase place that Phi is secondary reference pulse, Ay is the y component value of elementary reference pulse amplitude, Ax is the x component value of elementary reference pulse amplitude;
Step 8, more described signal parameter and standard nuclear-magnetism frequency spectrum parameter; In the time of coupling, finish; Otherwise repeating step three is to step 8;
Thereby step 9, record and the corresponding phase place of each rect.p. and amplitude form phase amplitude list, and according to this phase amplitude list output detections pulse;
Step 10, the form that becomes nuclear magnetic resonance spectrometer to identify described detection pulses switch, and input programming radio-frequency signal generator, can apply this detection pulse, tests uniformly sample parameter signal thereby obtain amplitude.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3111419B2 (en) * | 1994-08-31 | 2000-11-20 | 株式会社島津製作所 | Nuclear magnetic resonance inspection system |
| CN2896299Y (en) * | 2005-07-18 | 2007-05-02 | 北京海思威科技有限公司 | Novel digital spectrum instrument for nuclear magnetic resonance imaging system |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3111419B2 (en) * | 1994-08-31 | 2000-11-20 | 株式会社島津製作所 | Nuclear magnetic resonance inspection system |
| CN2896299Y (en) * | 2005-07-18 | 2007-05-02 | 北京海思威科技有限公司 | Novel digital spectrum instrument for nuclear magnetic resonance imaging system |
Non-Patent Citations (3)
| Title |
|---|
| "宽带脉冲DC SQUID核磁共振谱仪的研制";丁克俭等;《低温与超导》;20010831;第29卷(第3期);第39-42页 * |
| JP特许第3111419号B2 2000.09.22 |
| 丁克俭等."宽带脉冲DC SQUID核磁共振谱仪的研制".《低温与超导》.2001,第29卷(第3期),第39-42页. |
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