CN108982644A - Method based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS - Google Patents
Method based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS Download PDFInfo
- Publication number
- CN108982644A CN108982644A CN201810724111.5A CN201810724111A CN108982644A CN 108982644 A CN108982644 A CN 108982644A CN 201810724111 A CN201810724111 A CN 201810724111A CN 108982644 A CN108982644 A CN 108982644A
- Authority
- CN
- China
- Prior art keywords
- south pole
- mass
- canine tooth
- iipidomic
- fish
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
- G01N33/483—Physical analysis of biological material
- G01N33/487—Physical analysis of biological material of liquid biological material
- G01N33/48707—Physical analysis of biological material of liquid biological material by electrical means
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Biomedical Technology (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Pathology (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Biophysics (AREA)
- Medicinal Chemistry (AREA)
- Food Science & Technology (AREA)
- Urology & Nephrology (AREA)
- Molecular Biology (AREA)
- Hematology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses the methods based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS, the following steps are included: A, use iKnife electric knife cut South Pole canine tooth fish tissues slice surface, form aerosol, aerosol is introduced into mass spectrograph and is detected by mass analyzer, is obtained mass spectrum profile diagram (South Pole canine tooth fish tallow matter mass spectrum profile diagram)；B, mass spectrum profile diagram is made an uproar, the processing of centralization and mass calibration through MassLynx progress peak match, filter, mass spectrometric data and lipid molecular database is compared to the iipidomic profile of determining South Pole canine tooth fish.The present invention detects fast speed, sensitivity and high resolution, result is stablized, and provides new detection means for iipidomic research and piscine organism infomation detection.The present invention can meet the needs of quick, high-throughput, real-time detection.
Description
Technical field
The present invention relates to the detections of iipidomic profile, especially a kind of to be based on the direct sample detecting South Pole canine tooth of REIMS
The method of fish iipidomic profile.
Background technique
South Pole canine tooth fish (Dissostichus eleginoides), also known as U.S. dew cod, Notothenia Coriiceps of Antarctica, category spoke fin net-rope,
Perciformes, Nototheniidae, South Pole canine tooth fish category are mainly distributed on South America, Australia and secondary Antarctic archipelagic sea, waters of surviving
It is deep and 2500 meters.Canine tooth fish is delicate glittering and translucent and well-known with few bone and meat in the South Pole.The economic value ratio that canine tooth Antarctic Fish belongs to
Higher, current market average price is higher than the market average price of tuna, referred to as " platinum fishery ".To South Pole canine tooth fish
The business development and utilization of resource have about 40 years history since mid-term the 1970s so far in the world.China is by each
Kind condition limitation, does not carry out actual fishery fishing also, and the country also has no that its fishery resources is related in terms of processing and utilization
Report.
Lipid is a kind of biological organic molecule for being insoluble in water and being soluble in nonpolar solvent, mainly include fatty acid and its
The derivative naturally occurred, and compound relevant to its biosynthesis and function.Lipoid substance is in energy conversion, substance
Be in transport, information identification and transmitting, cell development and differentiation, disease and many life processes such as immune it is indispensable,
Abnormal metabolism and diabetes, arteriosclerosis, Alzheimer disease, fetus metabolic deficiency etc. are all closely related.Due to lipid point
The diversity and complexity of minor structure and the lag of corresponding analysis means hinder people to the whole lipid of life entity and its
Complicated metabolism network and function controlling carries out the system research of scale, globality.With 20th century genomics, protein
Group, the rise of the systematicness such as metabolism group " group is learned " concept, Han in 2003 et al. formally propose iipidomic this newly
Research frontier.Iipidomic identifies crucial rouge by lipids and its metabolins such as network analysis cell, body fluid, tissues
Biomarker reflects the overall variation of lipid under biological interspecific difference or specified conditions.With to iipidomic study by
Gradually deeply, the foundation of the analysis method of iipidomic also increasingly diversification mainly has thin-layered chromatography, gas chromatography-mass spectrum
With, soft ionization mass-spectrometric technique, nuclear magnetic resonance method etc..Mass spectrum is the most important analysis instrument of iipidomic research, with soft ionization
The development and its application in lipid analysis of ionization techniques and high resolution mass spectrum technology, have been realized in in biological sample
Various micro lipids carry out quick, high-precision analysis detection." shotgun " and positive or hydrophilic based on electro-spray ionization
Combined gas chromatography mass spectrometry is the common analysis method of iipidomic.However, before current iipidomic mass spectrometry method is to sample
Manage more demanding, step is complex, is unable to satisfy researcher to quick, high-throughput, real-time detection demand.
Rapid evaporation ionization massspectrum technology (Rapid evaporative ionization mass
Spectrometry, REIMS) it is a kind of novel ionization mass spectrometry technology in situ that need not be prepared or liquid chromatogram separates, it uses
The hand-held sampling apparatuses such as iKnife, electric heating probe directly evaporate sample surfaces, generate informative aerosol and pass through ion
Transfer conduit enters mass spectrum mass analyzer, and the accurate molecular masses spectrum of analyte is provided in the several seconds.Biology based on REIMS
Without any sample pre-treatments, being usually only necessary to several seconds time can be completed data collection and analysis and realizes life for fabric analysis
Object tissue identification, accuracy reach 90%-98%.
IKnife intelligent operation knife mass spectrum be it is a kind of need not any sample pre-treatments, target compound in real-time detection sample
A kind of novel mass-spectrometric technique.IKnife smart machine is developed based on electrosurgery knife, by electronic cutter and mass spectrometer two
A part composition.Unlike conditional electronic scalpel, iKnife is passed through using aerosol is generated during charge burning tissue
Venturi system sucking mass spectrum port simultaneously carries out chemical composition analysis, and useful information is extracted from big data and throws analysis result
It penetrates on touch panel monitor system device.It is domestic at present that there has been no iKnife relation technological researching reports.
Existing iipidomic profile testing method is unable to satisfy quick, high-throughput, real-time detection demand.Needle at present
To the iipidomic contour detecting of South Pole canine tooth fish, there is not been reported.
Summary of the invention
The purpose of the present invention is to provide a kind of based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS
Method.The present invention can meet the needs of quick, high-throughput, real-time detection.
Technical solution of the present invention: the method based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS, packet
Include following steps:
A, South Pole canine tooth fish tissues slice surface is cut using iKnife electric knife, forms aerosol, the aerosol warp
Venturi pump nitrogen driving, using orthogonal manner through PTFE tube introduce mass spectrum port after with 1.1 Ω, 3V, 500 DEG C of Kanthal
A1 filament collides, and the lipid ion in subsequent aerosol enters mass spectrometric StepWave device and detected by mass analyzer,
Using propylene glycol/leucine enkephalin mixture as secondary solvent, through needle pump sample injection device with the flow leading-in end of 0.1mL/min
Mouthful；Mass spectrograph sweep time is 1 second, and scanning range is m/z 100-1200；Data are collected from mode with negative electricity, obtain South Pole dog
Tooth fish tallow matter mass spectrum profile diagram；
B, mass spectrum profile diagram is subjected to peak match through MassLynx, filter is made an uproar, the processing of centralization and mass calibration, mass spectrometric data
Txt text formatting is saved as, the mass-to-charge ratio for the quasi-molecular ions that relative amount is 5% or more is obtained according to mass spectrometric data and peak area is believed
Breath, ion secondary's ms fragment, Lipid MS Predictor and LipidMap lipid in conjunction with relative amount for 10% or more
Molecular database compares the iipidomic profile for determining South Pole canine tooth fish.
In method above-mentioned based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS, in step A, institute
The output power for stating iKnife electric knife is 25.08W, cutting speed 0.49mm/s, and the iKnife electric knife cuts South Pole canine tooth
The Cutting Length of fish tissues slice surface is 1.03cm.
In method above-mentioned based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS, in step A, institute
The mass ratio for stating propylene glycol and leucine enkephalin is 98:2.
In method above-mentioned based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS, the South Pole dog
The analysis of phosphatide ion in the iipidomic profile of tooth fish is, to m/z650- in the canine tooth fish iipidomic profile diagram of the South Pole
Mass spectrogram in 1000 regions processing, the screening peak area such as carries out noise reduction, removes isotope and being greater than the quasi-molecular ions of 3.00E+05, calculate
Its mass of ion is calculated its chemical structure according to mass of ion measured value, and is verified using MS2 second order ms.
Compared with the prior art, the present invention is directly taken using iKnife electric knife cutting South Pole canine tooth fish tissues slice surface
Sample forms aerosol, South Pole canine tooth fish tallow matter compound ions can be realized, and the South Pole canine tooth fish of ionization is lipidization
Object is closed to be measured in real time by Pipe transfer to mass analyzer.Mass spectrograph, which only scans 1 second, can be obtained mass spectrum profile diagram, pass through
Comparison data can determine the iipidomic profile of sample.Fatty acid ion 17 kind are detected in South Pole canine tooth fish altogether, wherein signal
Maximum response intensity is m/z 327.23, and relative amount has reached 17.81%, its identified structure is FA 22:6, is secondly divided
It Wei not m/z 255.23 (FA 16:0,9.81%), m/z 281.25 (FA 18:1,9.09%)；10 kinds of phosphatide ion of detection, matter
Range m/z 736.49-909.55 is measured, the most strong quasi-molecular ions m/z 885.55 of signal is identified as [PI 38:4-H]–, relative abundance
Reach 19.30%, has secondly been m/z 790.54 ([PE 40:6-H]–, 15.24%).Verifying obtains, the noise of object ion
Than being 3.7-5.6% for 35.4-95.3, mass deviation 4.17-9.78ppm, withinday precision RSD, day to day precision RSD is
5.9-7.3%.The present invention detects fast speed, sensitivity and high resolution, result is stablized, and is iipidomic research and piscine organism
Infomation detection provides new detection means.The present invention can meet the needs of quick, high-throughput, real-time detection.
Detailed description of the invention
Fig. 1 is the detection device of the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS iKnife；
Fig. 2 is output power and cutting speed circle of equal altitudes；
Fig. 3 is output power and cutting speed response surface figure；
Fig. 4 is output power and Cutting Length circle of equal altitudes；
Fig. 5 is output power and Cutting Length response surface figure；
Fig. 6 is cutting speed and Cutting Length circle of equal altitudes；
Fig. 7 is cutting speed and Cutting Length response surface figure,
Fig. 8 is the fatty acid ion peak in the region South Pole canine tooth fish iipidomic profile diagram m/z 200-400；
Fig. 9 is the phosphatide quasi-molecular ions in South Pole canine tooth fish iipidomic profile diagram in the region m/z650-1000.
Appended drawing reference in figure are as follows: the diathermanous hair equipment of 1-, 2-iKninfe electric knife, the South Pole 3- canine tooth fish tissues slice, 4- gas
Colloidal sol, 5- syringe pump (i.e. needle pumps sample injection device), 6- mass spectrograph.
Specific embodiment
The present invention will be further described below with reference to the drawings, but is not intended as the foundation limited the present invention.
It is experimental example of the invention below.
Experimental example.
1.1 reagents and instrument
Xevo G2-XS quadrupole rod time of-flight mass spectrometer, holding sampling apparatus equipped with iKnife, (U.S. Waters is public
Department)；Pump11 elite needle pumps sample injection device (Harvard company of the U.S.)；2150 ultra-pure-water treatment system of Milliplus
(Millipore company of the U.S.)；(U.S. Waters is public for 4.1 data acquisition software of Masslynx and LiveID statistical analysis software
Department)；Other is laboratory common instrument and equipment.Methanol, acetonitrile, propylene glycol (chromatographically pure, Merck company of the U.S.)；Leucine
Enkephalins (Sigma Co., USA)；Experimental water is the ultrapure water prepared through Millipore ultrapure water instrument；South Pole canine tooth fish group
Section sample is knitted to be provided by Zhejiang ocean limited liability company of family.
1.2 Mass Spectrometry Conditions
South Pole canine tooth fish tissues slice surface is cut using iKnife electric knife, generation contains large amount of complex ion mixture
(formation) aerosol, through Venturi pump nitrogen driving, using orthogonal manner through PTFE tube introduce mass spectrum port after with Kanthal
A1 filament (1.1 Ω, 3V, 500 DEG C) collision, subsequent lipid ion enter mass spectrograph StepWave device and are examined by mass analyzer
Survey analysis, experimental provision such as Fig. 1；With propylene glycol/leucine enkephalin mixture (mass ratio of propylene glycol and leucine enkephalin
It is secondary solvent for 98:2), pumps sample injection device with the flow inlet port of 0.1mL/min, for cleaning impurity, improving through needle
Signal strength, lock mass correction；Mass spectrograph sweep time: 1 second；Scanning range: m/z 100-1200；All data are with negative
Ionization mode is collected.
The analysis of 1.3 data
Mass spectrogram is made an uproar through MassLynx progress peak match, filter, the processing of centralization and mass calibration, as a result (i.e. spectra count
According to) save as txt text formatting.Mass-to-charge ratio and the peak face for the quasi-molecular ions that relative amount is 5% or more are obtained according to mass spectrometric data
Product information, ion secondary's ms fragment, Lipid MS Predictor and LipidMap in conjunction with relative amount for 10% or more
Lipid molecular database compares the structural information for determining or speculating lipid.
2 results and discussion
The optimization of 2.1 iKnife ionization conditions
South Pole canine tooth fish is a kind of high protein, low fat fish, and musculature low fat characteristic is to REIMS testing result
It is affected.Previous experiments the study found that iKnife in cutting poultry class muscle or viscera tissue, ion signal response compared with
By force, noise is relatively high；When cutting Fish Tissue, the especially low-fat fishes musculature such as canine tooth fish, lipid ion is more difficult tested
It measures, noise effect is significant.Therefore, iKnife cutting condition is optimized first, adjustment output power, is adopted at cutting speed
Sample length parameter, to be stablized, reliable South Pole canine tooth fish muscle tissue iipidomic profile map.
Optimize experiment parameter using response phase method, with Box-Benhnken design principle, chooses phosphatide ion parent peak m/z
885.55 signal-to-noise ratio is worth in response, and output power, cutting speed, Cutting Length are empirical factor, and design optimization is different real
Conditional combination is tested, result such as table 1 is obtained.
1 iKnife electric knife of table cuts the optimization of South Pole canine tooth fish tissues slicing conditions
Regression analysis and fitting, obtained letter are carried out to the experimental data in table 1 using 8.0 software of Design Expert
It makes an uproar and compares regression equation are as follows:
S/N=46.44+0.19A-0.30B+0.51C+1.87AB-0.6AC+0.47C-2.07A2-2.84B2-3.47C2
Show that model P < 0.0001 is extremely significant by 2 variance result of table, the quasi- item P=0.1604 of mistake is not significant, R2=0.9766,
The regression equation and real data degree of fitting are higher.
2 variance result of table
According to fig. 2 to 3 factor response surface shown in Fig. 7 and contour map, optimum extraction condition is obtained after optimality analysis
Are as follows: energy (output power) 25.08W, cutting speed 0.49mm/s, Cutting Length 1.03cm, signal-to-noise ratio predicted value are
46.4656.For convenient for practical operation, experiment condition is adjusted are as follows: energy 25W, cutting speed 0.50mm/s, Cutting Length
1.0cm.5 repetitions are carried out at optimum conditions to test, it is (46.32 ± 1.21) % that verifying, which obtains practical signal-to-noise ratio average value,
This optimal conditions is effective.
The analysis of 2.2 fatty acid ions
Using the hand-held sampling of iKnife REIMS technology need not any sample pre-treatments, by tissue sample surface from
Sonization, in real time obtain mass spectrum profile diagram, through the softwares such as LiveID identify, and to after characteristic ion peak dimensionality reduction, modeling, it can be achieved that not
The realtime qualification and accuracy for knowing sample score.Due to front end not isolation technics such as tandem liquid chromatography, REIMS is related at present
Research is mainly based on qualitative.Therefore, this experimental study purpose is mainly to obtain the iipidomic of low-fat fishes South Pole canine tooth fish
Profile diagram does not further investigate the absolute content quantitative approach of each lipid molecular.
By carrying out cutting ionization, scanning range m/z 100-1200, while with bright to South Pole canine tooth fish muscle tissue
Propylhomoserin enkephalins (m/z 554.2615) is internal standard lock mass and calibrating quality axis.Fig. 8 is South Pole canine tooth fish iipidomic wheel
Exterior feature schemes fatty acid ion peak in the region m/z 200-400, and ion is more in region, and matrix noise is also more obvious；By right
It is identified and integral, obtains structure and relative amount is shown in Table 3.Fatty acid ion feature is shown as, according to azo rule, in matter
Mass number is usually odd number in spectrogram.Experiment detects 17 kinds of fatty acid ion altogether, and it is m/z that wherein signal response intensity is maximum
327, relative amount has reached 17.81%, its identified structure is FA 22:6, i.e. known DHA.It secondly is respectively m/z
255 (FA 16:0,9.81%), m/z 281 (FA 18:1,9.09%).M/z 375, m/z 389 etc. doubtful are overlength chain fatty
Sour FA 24:3Ep (2.79%), FA 26:3 (2.96%), existing may promote with South Pole canine tooth fish by extremely cold environment-stress
It, which is metabolized, generates long chain fatty acids to improve body fluid mobility correlation；Correlation assumes that it is still necessary to biology further to verify.
The structure of fatty acid ion and opposite contain in 3 South Pole region canine tooth fish iipidomic profile diagram m/z 200-400 of table
Amount
2.3 phosphatide ion analysis
To 9 noise reduction of mass spectrogram, the processing such as remove isotope, screening peak area is greater than the quasi-molecular ions of 3.00E+05, according to its point
Protonatomic mass measured value calculates its possible chemical structure, and is verified using MS2 second order ms.By taking m/z 883.53 as an example,
Its mass of ion and [PI 38:5-H]–(C47H80O13P–, 883.5342) and closest, (Product is scanned by daughter ion
Ion scan) parent ion is dissociated to obtain, the fatty acid chain daughter ion m/z 283.2 being broken by m/z 883.53 can be observed
(FA 18:0) and m/z 301.1 (FA 20:5), carbon atom number and double key number and early period speculate that 38:5 coincide, so can confirm m/
Z 883.53 is [PI 38:5-H]–.Most of phosphatide ionic structures can be confirmed by this method, the low abundance in part
Ion is not because daughter ion signal response deficiency does MS2 confirmation.Phosphatide quasi-molecular ions 10 is identified altogether in the canine tooth fish muscle tissue of the South Pole
Kind, mass range m/z 736.49-909.55 calculates relative abundance, RSD 3.28- using normalization method according to peak area
6.21%.The most strong quasi-molecular ions m/z 885.55 of signal is identified as [PI 38:4-H]–, relative abundance reached 19.30%；Its
Secondary is m/z 790.54 ([PE 40:6-H]–), relative abundance 15.24%.The detection of content is most in organism PC molecule compared with
Few, reason may be that iKnife output energy is higher, causes PC to lose choline group by electric energy transmission during cutting and gives birth to
At [PA-H]–Ion has confirmed [PA-H] more in result–The detection of ion, such as m/z 747.50 ([PA40:6-H]–)、m/z
763.56([PA O-42:5-H]–) etc..In the region canine tooth fish iipidomic profile diagram m/z 650-1000 of the South Pole phosphatide ion from
The structure and relative amount of son are shown in Table 4.
The structure of phosphatide ion ion and opposite in 4 South Pole region canine tooth fish iipidomic profile diagram m/z 650-1000 of table
Content
2.4 methodology validation
For the reliability for verifying South Pole canine tooth fish iipidomic contour method of this experiment based on REIMS, main peak rouge is chosen
Fat acid ion m/z 281.25, m/z 327.24 and phosphatide ion m/z 790.54, m/z 885.55 are characterized lipid quasi-molecular ions
Methodology validation is carried out to parameters such as sensitivity, selectivity, accuracy.It is diluted step by step to since tissue sample can not construct standard
System, this experiment use target lipid signal-to-noise ratio for index study method sensitivity.Result of study shows, the noise of target lipid
It is low-fat fishes in view of South Pole canine tooth fish than for 35.4-95.3, method sensitivity is higher, middle rouge higher for lipid content,
Fish high in fat are theoretically equally applicable.High-resolution matter is determined by the deviation of the actual measured value and theoretical value that calculate object ion
The selectivity of spectrum, the deviation of target lipid ion are 4.17-9.78ppm, show method high resolution, selectivity preferably, use
Relative molecular mass has biggish directive significance to lipid structure identification.Method precision with day to day precision by a few days surveying
Amount is continuously cut South Pole canine tooth fish muscle tissue 5 times in parallel using iKnife, and calculates the RSD of target lipid ion peak areas,
Obtain withinday precision；With the continuous parallel testing of same experimental conditions 7 days, calculates RSD and obtain day to day precision.It is wherein in a few days smart
The RSD of density is 3.7-5.6%, and the RSD of day to day precision is 5.9-7.3%, this experimental method precision is good, and testing result is steady
It is fixed.Method validation based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS is shown in Table 5.
Method validation of the table 5 based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS
3 conclusions
The REIMS method based on the hand-held acquisition of iKnife is established, for detecting the iipidomic profile of South Pole canine tooth fish.
After response surface optimization parameters, the ionization of lipid in low fat musculature is realized, successfully detects 17 kinds of fatty acid
Ion and 10 kinds of phosphatide ions.This method is without sample pre-treatments, it can be achieved that South Pole canine tooth fish muscle tissue iipidomic profile
Real-time detection, method choice, sensitivity, stability are more excellent, and new technological means is provided for iipidomic research.
It is the embodiment of the present invention below.
Embodiment.
Based on the method for the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS, the following steps are included:
A, South Pole canine tooth fish tissues slice surface is cut using iKnife electric knife, forms aerosol, the aerosol warp
Venturi pump nitrogen driving, using orthogonal manner through PTFE tube introduce mass spectrum port after with 1.1 Ω, 3V, 500 DEG C of Kanthal
A1 filament collides, and the lipid ion in subsequent aerosol enters mass spectrometric StepWave device and detected by mass analyzer,
Using propylene glycol/leucine enkephalin mixture as secondary solvent, through needle pump sample injection device with the flow leading-in end of 0.1mL/min
Mouthful；Mass spectrograph sweep time is 1 second, and scanning range is m/z 100-1200；Data are collected from mode with negative electricity, obtain South Pole dog
Tooth fish tallow matter mass spectrum profile diagram；
B, mass spectrum profile diagram is subjected to peak match through MassLynx, filter is made an uproar, the processing of centralization and mass calibration, mass spectrometric data
Txt text formatting is saved as, the mass-to-charge ratio for the quasi-molecular ions that relative amount is 5% or more is obtained according to mass spectrometric data and peak area is believed
Breath, ion secondary's ms fragment, Lipid MS Predictor and LipidMap lipid in conjunction with relative amount for 10% or more
Molecular database compares the iipidomic profile for determining South Pole canine tooth fish.
In step A, the output power of the iKnife electric knife is 25.08W, cutting speed 0.49mm/s, described
The Cutting Length that iKnife electric knife cuts South Pole canine tooth fish tissues slice surface is 1.03cm.
In step A, the mass ratio of the propylene glycol and leucine enkephalin is 98:2.
The analysis of phosphatide ion in the iipidomic profile of the South Pole canine tooth fish is, to South Pole canine tooth fish iipidomic
Mass spectrogram in profile diagram in the region m/z650-1000 processing, the screening peak area such as carries out noise reduction, removes isotope and being greater than 3.00E+
05 quasi-molecular ions calculates its mass of ion, calculates its chemical structure according to mass of ion measured value, and use MS2 second order ms
It is verified.
Certainly, the present invention can also have other various embodiments, without deviating from the spirit and substance of the present invention, ripe
It knows those skilled in the art and makes various corresponding changes and modifications, but these corresponding changes and change in accordance with the present invention
Shape all should fall within the scope of protection of the appended claims of the present invention.
Claims (4)
1. the method based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS, which is characterized in that including following step
It is rapid:
A, South Pole canine tooth fish tissues slice surface is cut using iKnife electric knife, forms aerosol, the aerosol is through Venturi
Pump nitrogen driving, using orthogonal manner through PTFE tube introduce mass spectrum port after with 1.1 Ω, 3V, 500 DEG C of Kanthal A1 filament
Collision, the lipid ion in subsequent aerosol enter mass spectrometric StepWave device and are detected by mass analyzer, with the third two
Alcohol/leucine enkephalin mixture is secondary solvent, through needle pump sample injection device with the flow inlet port of 0.1mL/min；Matter
Spectrometer sweep time is 1 second, and scanning range is m/z 100-1200；Data are collected from mode with negative electricity, obtain South Pole canine tooth fish
Lipid mass spectrum profile diagram；
B, mass spectrum profile diagram is made an uproar through MassLynx progress peak match, filter, the processing of centralization and mass calibration, i.e. mass spectrometric data is protected
Txt text formatting is saved as, the mass-to-charge ratio for the quasi-molecular ions that relative amount is 5% or more is obtained according to mass spectrometric data and peak area is believed
Breath, ion secondary's ms fragment, Lipid MS Predictor and LipidMap lipid in conjunction with relative amount for 10% or more
Molecular database compares the iipidomic profile for determining South Pole canine tooth fish.
2. the method according to claim 1 based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS,
Be characterized in that: in step A, the output power of the iKnife electric knife is 25.08W, cutting speed 0.49mm/s, described
The Cutting Length that iKnife electric knife cuts South Pole canine tooth fish tissues slice surface is 1.03cm.
3. the method according to claim 1 based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS,
Be characterized in that: in step A, the mass ratio of the propylene glycol and leucine enkephalin is 98:2.
4. according to the side according to claim 1 based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS
Method, it is characterised in that: the analysis of the phosphatide ion in the iipidomic profile of the South Pole canine tooth fish is, to South Pole canine tooth fish tallow
Mass spectrogram in matter group profile diagram in the region m/z650-1000 processing, the screening peak area such as carries out noise reduction, removes isotope and being greater than
The quasi-molecular ions of 3.00E+05 calculates its mass of ion, calculates its chemical structure according to mass of ion measured value, and use MS2 bis-
Grade mass spectrum is verified.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810724111.5A CN108982644A (en) | 2018-07-04 | 2018-07-04 | Method based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810724111.5A CN108982644A (en) | 2018-07-04 | 2018-07-04 | Method based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108982644A true CN108982644A (en) | 2018-12-11 |
Family
ID=64536157
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810724111.5A Pending CN108982644A (en) | 2018-07-04 | 2018-07-04 | Method based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108982644A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110200231A (en) * | 2019-06-25 | 2019-09-06 | 浙江工商大学 | A kind of method and detection method retaining hairtail nutrition degree using air fry |
| CN110514732A (en) * | 2019-09-03 | 2019-11-29 | 北京出入境检验检疫局检验检疫技术中心 | Identify the method for the sea-buckthorn place of production and/or kind based on rapid evaporation ionization mass spectrometry technology |
| CN113720896A (en) * | 2021-09-26 | 2021-11-30 | 浙江工商大学 | In-situ rapid evaporation ionization mass spectrometry for real-time identification of seven shrimps |
| CN113740410A (en) * | 2021-09-26 | 2021-12-03 | 浙江工商大学 | Method for detecting wet-type maturation maturity of tuna meat |
| CN114062473A (en) * | 2021-11-04 | 2022-02-18 | 浙江工商大学 | Method for evaluating storage quality of dried sea cucumbers based on iKnife evaporation ionization mass spectrometry |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104254772A (en) * | 2011-12-28 | 2014-12-31 | 麦迪马斯责任有限公司 | System and method for rapid evaporative ionization of liquid phase samples |
| WO2016142679A1 (en) * | 2015-03-06 | 2016-09-15 | Micromass Uk Limited | Chemically guided ambient ionisation mass spectrometry |
| CN106281665A (en) * | 2016-08-25 | 2017-01-04 | 山东师范大学 | The extraction of free fatty and detection method in a kind of Antarctic krill lipid supramolecular system |
| WO2017178833A1 (en) * | 2016-04-14 | 2017-10-19 | Micromass Uk Limited | Spectrometric analysis of plants |
| CN107533032A (en) * | 2015-03-06 | 2018-01-02 | 英国质谱公司 | MALDI-MS in situ for directly being mapped from massive texture determines imaging platform |
| CN107635478A (en) * | 2015-03-06 | 2018-01-26 | 英国质谱公司 | The fabric analysis carried out by mass spectrum or ion mobility spectrometry |
| CN107646089A (en) * | 2015-03-06 | 2018-01-30 | 英国质谱公司 | Spectrum analysis |
-
2018
- 2018-07-04 CN CN201810724111.5A patent/CN108982644A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104254772A (en) * | 2011-12-28 | 2014-12-31 | 麦迪马斯责任有限公司 | System and method for rapid evaporative ionization of liquid phase samples |
| WO2016142679A1 (en) * | 2015-03-06 | 2016-09-15 | Micromass Uk Limited | Chemically guided ambient ionisation mass spectrometry |
| CN107533032A (en) * | 2015-03-06 | 2018-01-02 | 英国质谱公司 | MALDI-MS in situ for directly being mapped from massive texture determines imaging platform |
| CN107635478A (en) * | 2015-03-06 | 2018-01-26 | 英国质谱公司 | The fabric analysis carried out by mass spectrum or ion mobility spectrometry |
| CN107646089A (en) * | 2015-03-06 | 2018-01-30 | 英国质谱公司 | Spectrum analysis |
| WO2017178833A1 (en) * | 2016-04-14 | 2017-10-19 | Micromass Uk Limited | Spectrometric analysis of plants |
| CN106281665A (en) * | 2016-08-25 | 2017-01-04 | 山东师范大学 | The extraction of free fatty and detection method in a kind of Antarctic krill lipid supramolecular system |
Non-Patent Citations (4)
| Title |
|---|
| BENOIT FATOU: "Remote Atmospheric Pressure Infrared Matrix-Assisted Laser Desorption-Ionization Mass Spectrometry (Remote IR-MALDI MS) of Proteins", 《MOLECULAR & CELLULAR PROTEOMICS 》 * |
| CONNOR BLACK: "A real time metabolomic profiling approach to detecting fish fraud using rapid evaporative ionisation mass spectrometry", 《METABOLOMICS》 * |
| JULIA BALOG: "Identification of the Species of Origin for Meat Products by Rapid Evaporative Ionization Mass Spectrometry", 《JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY》 * |
| 白新鹏: "《食品检验新技术》", 31 January 2010, 中国计量出版社 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110200231A (en) * | 2019-06-25 | 2019-09-06 | 浙江工商大学 | A kind of method and detection method retaining hairtail nutrition degree using air fry |
| CN110514732A (en) * | 2019-09-03 | 2019-11-29 | 北京出入境检验检疫局检验检疫技术中心 | Identify the method for the sea-buckthorn place of production and/or kind based on rapid evaporation ionization mass spectrometry technology |
| CN110514732B (en) * | 2019-09-03 | 2022-03-22 | 北京出入境检验检疫局检验检疫技术中心 | Method for identifying sea-buckthorn producing area and/or variety based on rapid evaporation ionization mass spectrometry technology |
| CN113720896A (en) * | 2021-09-26 | 2021-11-30 | 浙江工商大学 | In-situ rapid evaporation ionization mass spectrometry for real-time identification of seven shrimps |
| CN113740410A (en) * | 2021-09-26 | 2021-12-03 | 浙江工商大学 | Method for detecting wet-type maturation maturity of tuna meat |
| CN113720896B (en) * | 2021-09-26 | 2024-08-23 | 浙江工商大学 | In-situ rapid evaporation ionization mass spectrometry for real-time identification of seven shrimps |
| CN114062473A (en) * | 2021-11-04 | 2022-02-18 | 浙江工商大学 | Method for evaluating storage quality of dried sea cucumbers based on iKnife evaporation ionization mass spectrometry |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108982644A (en) | Method based on the direct sample detecting South Pole canine tooth fish iipidomic profile of REIMS | |
| Ma et al. | Advances in mass spectrometry imaging for spatial cancer metabolomics | |
| Eberlin et al. | Desorption electrospray ionization mass spectrometry for lipid characterization and biological tissue imaging | |
| Fletcher et al. | A new dynamic in mass spectral imaging of single biological cells | |
| Swaney et al. | Decision tree–driven tandem mass spectrometry for shotgun proteomics | |
| Pól et al. | Molecular mass spectrometry imaging in biomedical and life science research | |
| Mullen et al. | Determination of agrochemical compounds in soya plants by imaging matrix‐assisted laser desorption/ionisation mass spectrometry | |
| Wang et al. | Matrix‐assisted laser desorption/ionization mass spectrometry imaging of cell cultures for the lipidomic analysis of potential lipid markers in human breast cancer invasion | |
| CN103760220A (en) | Method of forming two-dimensional distribution image of target constituent | |
| CN105301163A (en) | Targeted metabo lomics analysis method for determining metabolites of living body | |
| CN104297355A (en) | Simulative-target metabonomics analytic method based on combination of liquid chromatography and mass spectrum | |
| CN108828051B (en) | Method for detecting lipid of antarctic krill oil in real time by rapid evaporation ionization mass spectrometry | |
| EP2455759B1 (en) | Mass spectrometry imaging with substance identification | |
| CN107300620B (en) | Dead meat identification method and system based on MALDI-TOF-MS | |
| CN110320303A (en) | A kind of Efficiency for Soil Aquifer Treatment metabonomic analysis methods based on UPLC-MS | |
| Janda et al. | Determination of abundant metabolite matrix adducts illuminates the dark metabolome of MALDI-mass spectrometry imaging datasets | |
| CN109557165B (en) | Method for monitoring the quality of a mass spectrometry imaging preparation workflow | |
| Gao et al. | Mass spectrometry imaging technology in metabolomics: a systematic review | |
| US10132796B2 (en) | Method for detecting and quantifying a target molecule in a tissue | |
| CN105466991B (en) | Bisphenol-A disposable paper base sensor and its preparation method and application | |
| US20240321565A1 (en) | Processing of spatially resolved, ion-spectrometric measurement signal data to determine molecular content scores in two-dimensional samples | |
| CN111157664A (en) | Biological metabonomics data processing method, analysis method, device and application | |
| Guo et al. | Development of mass spectrometry imaging techniques and its latest applications | |
| CN109946413A (en) | The method of pulsed data dependent/non-dependent acquisition Mass Spectrometer Method protein group | |
| Colley et al. | High-Specificity Imaging Mass Spectrometry |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181211 |