CN108459039A - A kind of nuclear magnetic resonance localization spectral method of Noninvasive observation emulsion forming process - Google Patents

A kind of nuclear magnetic resonance localization spectral method of Noninvasive observation emulsion forming process Download PDF

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CN108459039A
CN108459039A CN201810219108.8A CN201810219108A CN108459039A CN 108459039 A CN108459039 A CN 108459039A CN 201810219108 A CN201810219108 A CN 201810219108A CN 108459039 A CN108459039 A CN 108459039A
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CN108459039B (en
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崔晓红
游梦婷
韦芝良
杨健
陈忠
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Xiamen University
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    • G01N24/08Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N24/00Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
    • G01N24/08Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
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Abstract

The present invention provides a kind of nuclear magnetic resonance localization spectral method of Noninvasive observation emulsion forming process:It prepares emulsion and carries out fully shaking mixing with turbula shaker;Magnetic resonance localization is imported on nuclear magnetic resonance chemical analyser composes PRESS and GEMS pulse trains;Pulse train parameters and sampling parameter are set, carry out data acquisition, Data Post, obtain the GEMS pictures of high-resolution the MRS spectrum and sample entirety of different spatial, oily signal strength in MRS spectrograms is integrated, the stabilization that emulsion can be obtained in the Evolution by analyzing signal strength in different spatial forms the time and judges emulsification layer thickness.The advantages of this method is to sample using small voxel, and for non-uniform emulsion dynamic change system, the signal-to-noise ratio and resolution ratio of gained MRS spectrums are still very high, are appropriate for quantitative analysis.

Description

A kind of nuclear magnetic resonance localization spectral method of Noninvasive observation emulsion forming process
Technical field
The present invention relates to a kind of magnetic resonance localization spectrum detection methods, and emulsus is observed for Noninvasive more particularly, to one kind The magnetic resonance localization spectral method of liquid forming process material transport variation.
Background technology
Magnetic resonance imaging (Magnetic Resonance Imaging, MRI) technology has outstanding in terms of medical diagnosis Contribution, the 1970s NMR technology be used for medical diagnosis after, between short decades, MRI technique has been achieved for Quickly development.However the image information primary limitation obtained from MRI is in terms of institutional framework, actually mainly water and fat Spatial distribution image.Magnetic Resonance Spectrum (Magnetic Resonance Spectroscopy, MRS) be magnetic resonance imaging with A kind of method that conventional spectroscopy is combined, it is to obtain in vivo biochemical parameter quantitative information and unique non-intruding of diagnostic message Technology (Wang little Hong, Zhang Qinta, woods wild goose duty etc., 2011).
MRS is quantitatively divided specific atoms nuclei and its compound using the chemical shift of nuclear magnetic resonance and spin coupling effect The method of analysis.MRS localization spectrum utilizes gradient fields and pulse train, selectively excites the sample in a pocket (voxel), Spectrogram is generated by FID signal caused by observation, and using the FID signal for coming from selected voxel.This method be by Jackson and Langham was proposed and is developed first in nineteen sixty-eight.MRS can obtain sample interior structure with no damage Quantitative information judges whether its component ratio changes by observing the strong and weak variation of twocomponent signal in sample.And MRS Can on live body selectively, non-invasively chemical composition and structure, chemical environment variation and substance in quantitative measurment tissue Existence, this is that previous any imaging technique cannot achieve.MRS research in, in order to obtain it is significant as a result, I Need to generate the NMR signal region to be observed carry out stringent selection, so that NMR signal is resulted from desirable area of space, And allow experimental result by other regional effects minimum as far as possible.It is this that area-of-interest (Volume Of are selected from tissue Interest, VOI) technology, we are known as space orientation or localization (Keevil, 2006).Space orientation is MRS The first step (Chary&Govil, 2008).Magnetic resonance localization spectral method carries out localization, selective detection by pulsed field gradient The spectroscopic signal of substance in one fritter voxel.
The dispersion that emulsion is made of two kinds of immiscible liquid phases, emulsion generally can simply be divided into oil-in-water Type (O/W) and water-in-oil type (W/O) (Lobato-Calleros et al., 2008;Tan Y Y et al., 2016).Study emulsion Right solution surface tension, surface aggregation, kinetics and research biological film model are of great significance, and emulsion is in food (Gonz á lez-P é rez et al., 2005), medical (Relkin P et al., 2014), cosmetics (Nagelreiter et al., 2013;Onuki Y et al., 2016) and oil exploitation (Cherney et al., 2015;Carneiro et al., 2015) etc. It is more and more widely used.In recent years, NMR technology is mainly used for the self-diffusion by measuring water oil component in emulsion Coefficient obtain emulsion droplet size (Denkova et al., 2004) and particle diameter distribution (Slavka et al., 2003;Tuuk etc. People, 2016), and still about the achievement in research of the migration of substance during emulsion formation mechenism and phase transition and changing rule It is few.Therefore, this patent uses magnetic resonance localization spectral method and has carried out dynamic monitoring and research to water oil emulsion process.Magnetic resonance Localization spectrum can obtain the one-dimensional hydrogen spectrum information of different level sample by the voxel of selection different location, and then obtain water oil Different time different level component and changes of contents in emulsion process.
Garcia-Aparicio et al. the diffusions of application MRS three kinds of small molecules of technique study in hydrogel in 2012 (Garcia-Aparicio et al., 2012).By expanding molecule chitosan concentration in drug solubility, molecular weight and gel The feasibility of the influence research and inquirement MRS technique study dispersal behaviors for the behavior of dissipating.Research is by several different fixed positions It is detected, the behavior of solutes accumulation is studied, obtained the spatial homing and temporal regularity of solutes accumulation.With proton arteries and veins Rush the measured value of diffusion coefficient and the measured value very one obtained by MRS methods in the propagation measurement of gradient field method progress It causes.
Onuki in 2014 et al. uses MRI method as a kind of lossless monitoring method, divides oil-in-water emulsion Layer process is studied (Onuki, Y et al., 2014).The research accelerates point of emulsion sample by the methods of centrifugation Then layer carries out MRI monitorings.
Therefore, in the present invention, we by MRS localization spectral method and MRI pictures for the formation of emulsion and with it is excessive The process of oil and aqueous phase separation carries out quantitative analysis, to depict by obtained MRS spectrums to water oil content at different zones The migration and variation process of substance in emulsion forming process.
Invention content
The purpose of the present invention is to provide a kind of emulsus is observed by acquiring the method for high-resolution MRS spectrums and MRI pictures The research method of liquid forming process, and migration of this method suitable for detecting the substance changed with room and time chemical system And changes of contents.
In order to solve the above-mentioned technical problem, the present invention is achieved by the following technical solutions:
A kind of nuclear magnetic resonance localization spectral method of Noninvasive observation emulsion forming process, includes the following steps:
(1) emulsion sample to be measured is prepared, emulsion is prepared by miscella and emulsifier aqueous solution, by fully shaking The emulsion crossed is transferred in NMR pipes, is placed in nuclear magnetic resonance spectrometer;
(2) stable reference sample is placed in nuclear magnetic resonance spectrometer, sample is referred to conventional one-dimensional pulse sequence acquisition The one-dimensional hydrogen of product is composed, and obtains its signal peak distributed areas and line width, reference, while line width values are provided for spectrum width parameter setting Size reflects field homogeneity implementations;
(3) it uses nuclear magnetic resonance spectrometer to apply GEMS pulse trains to emulsion sample to be measured, GEMS pulse sequences is set The parameter of row acquires the gtadient echo picture of emulsion sample to be measured, was denoted as 0 moment;The parameter of the GEMS pulse trains includes: Pulse-recurrence time TR, echo time TE, flip angle, sky sweep number, accumulative frequency nt, imaging array, visual field FO, layer The thick, sampling time;
(4) while using nuclear magnetic resonance spectrometer to emulsion sample to be measured apply PRESS pulse trains, PRESS is set The parameter of pulse train, acquire emulsion sample to be measured 0 moment a certain spatial position localization spectrogram;The PRESS pulses The parameter of sequence includes that spectrum width SW, sampling number NP, pulse-recurrence time TR, echo time TE, sky sweep number, accumulative frequency Nt, voxel size, sampling time;
(5) change the voxel location parameter in PRESS pulse trains, keep other parameters and voxel size constant, successively Acquire emulsion sample to be measured 0 moment other spatial positions localization spectrogram;
(6) every 10 minutes, step (3) is repeated;
(7) at regular intervals, step (4), (5) are repeated, until emulsion sample delaminating process to be measured is substantially steady It is fixed;
(8) collected localization spectrum FID is subjected to Fourier transformation, obtains high-resolution one-dimensional localization spectrogram;To every Signal peak in one-dimensional spectrum is integrated, and will be obtained integration data and is imported Origin softwares, according to time and space rule to data Carry out taxonomic revision;
(9) integrated intensity of different spaces level and time are mapped, the oil concentration of different level can be obtained at any time Variation relation, analyze different spatial on signal strength Evolution can be obtained emulsion formation stabilization time and breast Change layer thickness, wherein stabilization time can intuitively be read out by tendency chart.
In a preferred embodiment:Water oil volume ratio is 1 in the emulsion sample to be measured described in step (1):1.
In a preferred embodiment:In step (2), the routine one-dimensional pulse sequence be nuclear magnetic resonance spectrometer from The one-dimensional pulse sequence of band is made of a non-selective pi/2 radio-frequency pulse and signal sampling phase, and the non-selective pi/2 is penetrated Followed by signal sampling phase after frequency impulse action.
In a preferred embodiment:The PRESS pulse trains are a double spin-echo sequences, which is selected by piece Pi/2 excitation pulse and two pieces select π reunion pulses to form.
Compared to the prior art, technical scheme of the present invention has following advantageous effect:
(1) compared with the method for traditional research emulsion property, NMR methods have repeatability, Noninvasive etc. excellent Point.The result that this method obtains illustrates metastable emulsion and forms time and the substance variation in different spaces level Trend.The advantages of MRS is composed is to possess higher spectral resolution and signal-to-noise ratio.
(2) nuclear magnetic resonance pulse sequence used by this experiment is PRESS sequences, the different spaces layer obtained by PRESS The localization spectrum in face can capture the migration and variation process of dynamic system substance in change procedure, and GEMS pictures can be used for macroscopically seeing The variation for examining system is compareed with facilitating with localization spectrum result.
(3) by carrying out contrast experiment to the sample of different emulsifiers content, we can obtain emulsifier concentration for The influence of emulsion process.By carrying out contrast experiment to different water oil systems samples, we can obtain different types of oil and exist The similarities and differences on emulsifying property.
Description of the drawings
Fig. 1 is the edge arrow that the emulsion sample that emulsifier content is 0.35g/L changes over time in entire delaminating process The GEMS pictures in shape face.
Fig. 2 is the sample edge arrow that the emulsion sample that emulsifier content is 0.35g/L was layered at 120 minutes after stablizing relatively The localization spectrogram of each layer of the GEMS pictures in shape face and space.
The emulsion sample that Fig. 3 emulsifier contents are 0.35g/L oil substances signal of different level during monitoring is strong Spend the curve changed over time.
Fig. 4 be emulsifier content be 0.35g/L emulsion sample during monitoring under Each point in time oil substances believe The distribution situation of number intensity in different location.
Specific implementation mode
It elaborates below to the embodiment of the present invention, the present embodiment is carried out lower based on the technical solution of the present invention Implement, gives detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation Example.
A kind of nuclear magnetic resonance localization spectral method of Noninvasive observation emulsion forming process is present embodiments provided, including Following steps:
(1) emulsion sample to be measured is prepared, emulsion is prepared by miscella and emulsifier aqueous solution, wherein oil and water Volume ratio is 1:1.It is transferred in NMR pipes, is placed in nuclear magnetic resonance spectrometer by the emulsion that fully shaking is crossed;
(2) stable reference sample is placed in nuclear magnetic resonance spectrometer, sample is referred to conventional one-dimensional pulse sequence acquisition The one-dimensional hydrogen of product is composed, and obtains its signal peak distributed areas and line width, reference, while line width values are provided for spectrum width parameter setting Size reflects field homogeneity implementations;The routine one-dimensional pulse sequence is the included one-dimensional pulse of nuclear magnetic resonance spectrometer Sequence is made of a non-selective pi/2 radio-frequency pulse and signal sampling phase, after the non-selective pi/2 radio-frequency pulse effect The followed by signal sampling phase.
(3) it uses nuclear magnetic resonance spectrometer to apply GEMS pulse trains to emulsion sample to be measured, GEMS pulse sequences is set The parameter of row acquires the gtadient echo picture of emulsion sample to be measured, was denoted as 0 moment;The parameter of the GEMS pulse trains includes: Pulse-recurrence time TR, echo time TE, flip angle, sky sweep number, accumulative frequency nt, imaging array, visual field FOV, layer The thick, sampling time;
(4) while using nuclear magnetic resonance spectrometer to emulsion sample to be measured apply PRESS pulse trains, PRESS is set The parameter of pulse train, acquire emulsion sample to be measured 0 moment a certain spatial position localization spectrogram;The PRESS pulses The parameter of sequence includes that spectrum width SW, sampling number NP, pulse-recurrence time TR, echo time TE, sky sweep number, accumulative frequency Nt, voxel size, sampling time;The PRESS pulse trains are a double spin-echo sequences, which selects pi/2 by piece Excitation pulse and two pieces select π reunion pulses to form.
(5) change the voxel location parameter in PRESS pulse trains, keep other parameters and voxel size constant, successively Acquire emulsion sample to be measured 0 moment other spatial positions localization spectrogram;
(6) every 10 minutes, step (3) is repeated;
(7) at regular intervals, step (4), (5) are repeated, until emulsion sample delaminating process to be measured is substantially steady It is fixed;
(8) collected localization spectrum FID data are subjected to Fourier transformation, obtain high-resolution one-dimensional localization spectrogram;It is right Signal peak in every one-dimensional spectrum is integrated, and will be obtained integration data and is imported Origin softwares, according to time and space rule pair Data carry out taxonomic revision;
(9) integrated intensity of different spaces level and time are mapped, the oil concentration of different level can be obtained at any time Variation relation, analyze different spatial on signal strength Evolution can be obtained emulsion formation stabilization time and breast Change layer thickness, wherein stabilization time can intuitively be read out by tendency chart.
The nuclear-magnetism for hereafter observing emulsion forming process to verify above-mentioned Noninvasive by a specific experiment is total to Localization of shaking spectral method.
The present embodiment be suitable for using magnetic resonance localization compose and MRI method monitoring oil-water system emulsion formed to oil, The process of water and emulsion layer layering stabilization, detects the variation of substance during this:
(1) this experiment sesame oil used is purchased from local supermarket and directly uses without any pretreatment.It is husky to moor Lip river Nurse 188 and acetone (99.5% purity) are purchased from local chemical products retailer (Jilin GmbH, Xiamen, China) and directly It is employed without and is further purified.D2O (99.8%) is the product of Norell (USA).D2O and distilled water prepare lotion.1200μL D2The distilled water of O and 800 μ L are configured as water phase, by PLURONICS F87 be dispersed in water phase in the ratio of 0.35g/L and At room temperature with vortex rotation to ensure to be completely dissolved.2000 μ L sesame oil are taken, it is mixed with water, at room temperature with the rotation 5 that is vortexed Minute, so that sample fully shaking is become emulsion.Take 550 μ L fully shakings, after be transferred in the standard NMR pipes of 5mm, be put into It is vibrated again before H NMR spectroscopy instrument.
(2) sample detection
The instrument that this experiment uses is the micro- imaging account of 500MHz Varian nuclear magnetic resonance spectrometers, pulse train For PRESS sequences and GEMS imaging sequences, sample temperature 298K.
Before formal experiment, shimming is carried out to provide relatively uniform field using stable reference sample.It will make The solution example nuclear magnetic tube got ready is placed in 500MHz Varian nuclear magnetic resonances spectrometer routine one-dimensional pulse sequence acquisition one Zhang Yiwei is composed, and is obtained the line width of spectral line, is provided foundation for spectrum width parameter setting, while line width values reflect magnetic field environment uniformity Situation.
According to step 3, the GEMS pulse trains, sampling parameter is called to be:Pulse-recurrence time TR (repetition time) =20ms, echo time TE (echo time)=4ms, flip angle (flip angle)=20 °, sky sweep (Dummy Scans)= 0, accumulative frequency nt=1, imaging array=128 × 128, visual field FOV (field of view)=25 × 25mm, thickness 2mm, sampling time 7.7s.
According to step 4 and 5, PRESS sequences are called, according to experiment needs, experiment parameter is set.It is real for this experiment It includes spectrum width SW=8013Hz, sampling number (NP)=4096, pulse-recurrence time TR=2.2s, echo time TE=to test parameter 15ms, sky sweep (Dummy Scans)=0, add up nt=1 times secondary, and voxel size is 5.0 × 5.0 × 0.2mm3, the sampling time= 2.2s。
Execute step 6,7.
(3) Data Processing in Experiment
Collected initial data carries out Fourier transformation to PRESS spectrograms with VNMR J and obtains high-resolution one-dimensional MRS The one-dimensional spectrum signal of all voxels from different spatial is stacked up by spectrogram, and such as Fig. 2, every one-dimensional spectrum contains Thickness is the material information in the voxel of Δ z.By selecting suitable parameter to the methylene group from oil (at 1.30ppm) Spectral peak carry out integral obtain quantitative analysis data.Import data to Origin softwares (Version Pro8), to data into Row taxonomic revision, it is in the reference axis of signal strength (i.e. integrated value) that by data point, to be drawn in abscissa, which be time (min) ordinate,. The point of different time in same level is connected into a curve, such as Fig. 3, you can obtain in the level oil substances at any time The rule of variation.Simultaneously as these curves represent different level, the variation rule of oil substances spatially also can be obtained in we Rule.It is in the reference axis of signal strength (i.e. integrated value) that by data point, to be drawn in abscissa, which be position (position) ordinate,.It will Point in same time different level connects into a curve, such as Fig. 4, you can obtains oil substances in same time difference position The changing rule set.
(4) analysis of experimental results
Fig. 1 be sample 0 to 120 minutes every 10 minutes collected GEMS pictures, therefrom we are it can be found that 0 moment When entire sample be uniform state, be in bright signal, at 10 minutes, the top of image be bright signal remaining be dark signal, show Bright signal is presented in separation to moieties from mixing sample.Hereafter, separation continues, and the upper area of bright signal is more next It is bigger, and lower part signal strength also gradually increases.Image is that the bright centre in both ends is dark at about 40 minutes, and sample reaches after 50 minutes Basicly stable until 120 minutes, part was most bright in presentation, and lower part is slightly dark, most dark centered on middle section+dark mixing of surrounding Region.Since MRI pictures show only the macroscopic view variation in emulsion forming process, in order to obtain in change procedure each component in sky Between and the time variation, we acquire the localization spectrogram of different moments different spaces level.Stacking spectrogram in Fig. 2 is The high-resolution localization spectrum of different spaces level at 120 minutes, it can be seen that the peak intensity of oil substances is in spatially from top to down The trend of reduction, and water peak intensity is in incremental trend.
Oily signal in being composed by all localization acquired to different moments integrates (at 1.30ppm) can analyze difference On spatial position the Evolution of signal strength can be obtained emulsion stabilization formed the time and emulsification layer thickness.Fig. 3 is difference The curve that the oil substances signal strength of level changes over time, when 0 moment, nuclear magnetic tube Nei Shui, oil and emulsifier are in uniformly mixed Conjunction state, water, oil and emulsion are each to be mutually not yet layered, and the oily signal strength of every aspect is not much different in NMR pipes, and curve rises Initial point is concentrated.As time goes by, sample starts to be layered, and the oily signal strength of inclined water phase is lower and lower, and the oil letter of oil phase partially Number intensity is increasing.The growth of the intensity of the oily signal positioned at different level at any time is shown as in figure in polarization to become Gesture reached stable state at 50 minutes or so.
Fig. 4 is that oil substances signal strength intuitively illustrates each in the distribution situation of different location under Each point in time Under time point in the sample of different location oil concentration content.At 0 moment, oil concentration becomes without significantly variation on each position Gesture, in one than more uniform state, curve is more straight.As time goes by, curve gradually becomes precipitous, after 50 minutes Curve essentially coincide, illustrate after 50 minutes, the phase separation of emulsion is basicly stable.With Fig. 3 conclusions one It causes.
In figure 3, can judge to correspond to oil phase and water phase respectively respectively according to the oil concentration height at the places 8mm and -8mm, and As emulsus liquid phase of the oil concentration between oil phase and water phase.Since the spatial positional information representated by every curve comes from one In a voxel, it is therefore assumed that the voxel of acquisition is enough, according to the variation tendency of each space aspects oil concentration, meter can be passed through Calculation obtains emulsification layer thickness.The present invention is method introduction, does not acquire enough voxels.In Fig. 4, at the positions observation 8mm Point, the size of oil concentration gradually rises as the time increases.Point at the positions -8mm, the size of oil concentration increase with the time It is gradually reduced.The changing rule of oil concentration in oil phase and water phase can be respectively represented by analyzing the oil concentration on the two positions.
In conclusion using localization spectral method and MRI pictures can be to emulsion stabilization forming process and excessive water Mutually and the disconnected process of oil phase carries out both macro and micro monitoring respectively.It can be from from obtained high-resolution magnetic resonance localization spectrum Substance is analyzed on molecular level at any time with the changing rule in space, the stabilization that emulsion can be obtained forms time and its thickness. MRI pictures can prove the conclusion of localization spectrum as compensation process.By examples detailed above, this method is to study non-uniform emulsion Quick variation system provides technical support, can be used for studying different preparation methods and component ratio to emulsion formation and property Influence.
The above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be to the present invention Embodiment restriction.It is all the present invention design and technical solution within made by all any modification, equivalent and improvement Deng should all be included in the scope of protection of the claims of the present invention.

Claims (4)

1. a kind of nuclear magnetic resonance localization spectral method of Noninvasive observation emulsion forming process, it is characterised in that including following step Suddenly:
(1) emulsion sample to be measured is prepared, emulsion is prepared by miscella and emulsifier aqueous solution, is crossed by fully shaking Emulsion is transferred in NMR pipes, is placed in nuclear magnetic resonance spectrometer;
(2) stable reference sample is placed in nuclear magnetic resonance spectrometer, with conventional one-dimensional pulse sequence acquisition reference sample One-dimensional hydrogen spectrum, obtains its signal peak distributed areas and line width, reference, while line width values size is provided for spectrum width parameter setting Reflect field homogeneity implementations;
(3) nuclear magnetic resonance spectrometer is used to apply GEMS pulse trains to emulsion sample to be measured, setting GEMS pulse trains Parameter acquires the gtadient echo picture of emulsion sample to be measured, was denoted as 0 moment;The parameter of the GEMS pulse trains includes:Pulse Repetition time TR, echo time TE, flip angle, sky are swept number, accumulative frequency nt, imaging array, visual field FO, thickness, are adopted The sample time;
(4) while using nuclear magnetic resonance spectrometer to emulsion sample to be measured apply PRESS pulse trains, PRESS pulses are set The parameter of sequence, acquire emulsion sample to be measured 0 moment a certain spatial position localization spectrogram;The PRESS pulse trains Parameter include that spectrum width SW, sampling number NP, pulse-recurrence time TR, echo time TE, sky sweep number, accumulative frequency nt, body Plain size, sampling time;
(5) change the localization voxel location parameter in PRESS pulse trains, keep other parameters and voxel size constant, successively Acquire emulsion sample to be measured 0 moment other spatial positions localization spectrogram;
(6) every 10 minutes, step (3) is repeated;
(7) at regular intervals, step (4), (5) are repeated, until emulsion sample delaminating process to be measured is basicly stable;
(8) collected localization spectrum FID is subjected to Fourier transformation, obtains high-resolution one-dimensional localization spectrogram;It is one-dimensional to every Signal peak in spectrum is integrated, by obtained integration data import Origin softwares, according to time and space rule to data into Row taxonomic revision;
(9) integrated intensity of different spaces level and time are mapped, the change of the oil concentration of different level at any time can be obtained Change relationship;Stabilization time and the emulsion layer of emulsion formation can be obtained in the Evolution of signal strength in analysis different spatial Thickness, wherein stabilization time can intuitively be read out by tendency chart.
2. a kind of nuclear magnetic resonance localization spectral method of Noninvasive observation emulsion forming process as described in claim 1, special Sign is:Water oil volume ratio is 1 in the emulsion sample to be measured described in step (1):1.
3. a kind of nuclear magnetic resonance localization spectral method of Noninvasive observation emulsion forming process as described in claim 1, special Sign is:In step (2), the routine one-dimensional pulse sequence is the included one-dimensional pulse sequence of nuclear magnetic resonance spectrometer, by One non-selective pi/2 radio-frequency pulse and signal sampling phase are constituted, and are followed by believed after the non-selective pi/2 radio-frequency pulse effect Number sampling period.
4. a kind of nuclear magnetic resonance localization spectral method of Noninvasive observation emulsion forming process as described in claim 1, special Sign is:The PRESS pulse trains are a double spin-echo sequences, which selects pi/2 excitation pulse and two by piece Piece selects π reunion pulses to form.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110441345A (en) * 2019-09-06 2019-11-12 苏州大学 Method based on the aqueous printing ink formula of low-field nuclear magnetic resonance Technology design
CN110940944A (en) * 2019-12-04 2020-03-31 厦门大学 J coupling removing method for magnetic resonance signals based on deep learning

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1374427A (en) * 1972-03-08 1974-11-20 Newport Instr Ltd Measurement of water content
US20030009297A1 (en) * 2001-03-26 2003-01-09 Konstantin Mirotchnik Determination of oil and water compositions of oil/water emulsions using low field NMR Relaxometry
CN106050225A (en) * 2016-06-06 2016-10-26 中国石油天然气集团公司 Method for determining 100% pure water spectrum through nuclear magnetic resonance logging spectrum T2
US20160320323A1 (en) * 2015-04-29 2016-11-03 Colorado School Of Mines Water/oil/gas emulsions/foams characterization using low field nuclear magnetic resonance
CN106645255A (en) * 2017-01-21 2017-05-10 厦门大学 NMR (nuclear magnetic resonance) single voxel localization and one-dimensional pure chemical shift spectroscopy method
CN106970102A (en) * 2017-03-10 2017-07-21 厦门大学 The nuclear magnetic resonance spatial discrimination spectral method of emulsus liquid phases separation is monitored in real time

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1374427A (en) * 1972-03-08 1974-11-20 Newport Instr Ltd Measurement of water content
US20030009297A1 (en) * 2001-03-26 2003-01-09 Konstantin Mirotchnik Determination of oil and water compositions of oil/water emulsions using low field NMR Relaxometry
US20160320323A1 (en) * 2015-04-29 2016-11-03 Colorado School Of Mines Water/oil/gas emulsions/foams characterization using low field nuclear magnetic resonance
CN106050225A (en) * 2016-06-06 2016-10-26 中国石油天然气集团公司 Method for determining 100% pure water spectrum through nuclear magnetic resonance logging spectrum T2
CN106645255A (en) * 2017-01-21 2017-05-10 厦门大学 NMR (nuclear magnetic resonance) single voxel localization and one-dimensional pure chemical shift spectroscopy method
CN106970102A (en) * 2017-03-10 2017-07-21 厦门大学 The nuclear magnetic resonance spatial discrimination spectral method of emulsus liquid phases separation is monitored in real time

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110441345A (en) * 2019-09-06 2019-11-12 苏州大学 Method based on the aqueous printing ink formula of low-field nuclear magnetic resonance Technology design
CN110940944A (en) * 2019-12-04 2020-03-31 厦门大学 J coupling removing method for magnetic resonance signals based on deep learning

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