CN106093227A - The LC-MS method of 113 kinds of lipids in a kind of high flux detection organism blood sample - Google Patents
The LC-MS method of 113 kinds of lipids in a kind of high flux detection organism blood sample Download PDFInfo
- Publication number
- CN106093227A CN106093227A CN201610380851.2A CN201610380851A CN106093227A CN 106093227 A CN106093227 A CN 106093227A CN 201610380851 A CN201610380851 A CN 201610380851A CN 106093227 A CN106093227 A CN 106093227A
- Authority
- CN
- China
- Prior art keywords
- sub
- tof
- phase
- sample
- kinds
- 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
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The LC-MS method of 113 kinds of lipids in a kind of high flux detection organism blood sample, it belongs to bioanalytical chemistry field.The method uses after sample to be tested being pre-processed and added reaction dissolvent and extractant extraction, carries out liquid chromatography mass spectrometric detection.The method is simple to operate, selectivity is high, highly sensitive, can quickly detect 113 kinds of lipids in blood, wherein phosphatid ylcholine (PC) 48, lysophosphatidyl choline (Lyso PC) 21, phosphatidyl-ethanolamine (PE) 17, lysophosphatidyl ethanolamine (LPE) 4, haemolysis phosphinositides (PI) 6, sphingomyelins (SM) 9, ceramide (Cer) 8.The precision of the method meets the requirement of serum sample analysis, has good stability, and the detection sensitivity for major part lipid metabolin is higher, it is adaptable to the iipidomics analysis of serum sample.
Description
Technical field
The present invention relates to the LC-MS method of 113 kinds of lipids in a kind of high flux detection organism blood sample, it belongs to
In biochemical analysis detection field, can be greatly improved with the detection carrying out 113 kinds of lipid components in blood of fast high-flux
Detection efficiency and accuracy.
Background technology
Blood is important component part in human body, flows through each organ, tissue in human body, participate in human body metabolism,
Regulatory function and the internal and external environment balance maintaining human body, any position of human body occurs all can produce specifically during pathologic change
Biomarker is discharged in blood, and blood sample detection is noninvasive, being be easy to get most a kind of can be as in-vitro diagnosis
Biological specimen, therefore routine blood test is also the detection data being the most directly easy to get in medical diagnosis[1]。
At present, the metabolism group of blood is known on the early stage biomarker finding new disease day by day.
2012, the blood plasma to the 100 case patients with lung cancer collected from Moscow and 100 case healthy volunteers for the mass spectrography such as Lokhov
Sample is detected.Research finds 70 metabolins related to lung cancer, and lung cancer group level is above healthy volunteer；And
And the level of these metabolins just there occurs rise at the lung cancer initial stage[2].2015, Tang little Hu etc. used the generation with nuclear magnetic resonance
Thank to group and learn the difference of metabolin in the Comparison between detecting methods serum sample of 51 patient with esophageal carcinoma and 50 normal persons, have found
Metabolin proline is the related biomarker of the cancer of the esophagus with glutamine, and uses cluster analysis to the two biological marker
Thing is verified, has finally carried out the contrast on content to the two metabolin, and discovery proline and glutamine are in the cancer of the esophagus
Content in the serum of patient is all low than normal person[3].2012, Du Zhi was bravely waited and intends being suffered from by metabonomic technology detection heart failure
The blood serum metabolic spectrum of person, analyzes itself and ultrasonic cardiac muscle energy consumption index MEE correlation, this research totally 61 people, wherein Normal group
15 people, heart failure group 46 people, find that 44 species diversity lipid-metabolism products are related to heart failure altogether by detection[4].Therefore blood mark
Will thing is that the further investigation of disease provides effective evidence, has deep Research Significance and explores value.
Lipid compounds is the important component part of membrane structure, its cell development, energy reserve, signal conduction,
Vital effect is all played during the vital movements such as matter transportation.Lipid compound includes following big class: fatty acyl
Class, glyceride type, glycerophosphatide class, sphingolipid, stay alcohol lipid, isoamyl refines alcohol lipid, glycolipid class and poly ketone, different lipids
The biological function of reaction is also different.Therefore, the dynamic change of lipid-metabolism can reflect lipid and metabolism thereof directly or indirectly
Interaction situation between the physiology of thing and biosystem such as cell, body fluid, tissue, organ and body, pathology.In view of fat
The special biological significance of matter, checks that the lipid in blood has irreplaceable importance, and fat in metabolic disease examination
Matter be present in cell, organelle and extracellular body fluid such as blood plasma, bile, breast, in intestinal juice, the lipid therefore detecting in blood becomes
Point also become patient go to a doctor detection when most convenient detection methods[5].The abnormal metabolism of lipid and arteriosclerosis, diabetes,
Obesity, Alzheimer disease and tumour occur closely related, and iipidomic obtains in the raising with detection technique in recent years
Increasing development, but the cognition of the 26S Proteasome Structure and Function that people are to lipid still far lags behind gene and protein,
Main reasons is that the diversity complexity due to lipid molecular structure, and the delayed of corresponding analysis means hinders people couple
The metabolism network of the overall lipid of life entity and complexity thereof and function controlling carry out the system research of scale globality[6].In order to
Avoid flase drop and the missing inspection of disease, need fast and accurate detection method to take into account blood multi-analyte immunoassay simultaneously.At various points
In analysis means, efficient liquid phase tandem mass spectrum, with its high flux high accuracy, has played big advantage in blood lipid context of detection.
The precision of this method meets the requirement of serum sample analysis, has good stability, for the detection of major part lipid metabolin
Sensitivity is higher, it is adaptable to the iipidomics analysis of serum sample.
2014, Qu Feng etc. employed two clinical queues, added up to 156 case serum samples to use high performance liquid chromatography series connection
Triple level Four bar mass spectrums establish the quantitative analysis method of a set of targeting sheath iipidomic, retrieve (Lipid by internet database
Maps) 43 sphingolipid metabolism network core compounds of identification and analysis, have carried out chronic third venereal disease virus hepatitis associated biomolecule mark
Research in terms of will thing[7].2013, practise the analysis method that acute hearing etc. uses high performance liquid chromatography tandem mass spectrum to set up, carried out 80
Example type-II diabetes patient and the iipidomic research of 28 case healthy volunteer's serum samples, examine with type-II diabetes to find
Break, treat closely related potential lipid biomarker.Retrieve (Lipid maps, METLIN) by internet database
And the cleavage of mass spectrum feature of metabolite structures, infer the possible structure of possible biomarker.Result identifies 35 and two types
The structure of the closely related lipid potential source biomolecule mark of diabetes diagnosis, additionally identifies 49 and treats with type-II diabetes
The structure of closely related lipid potential source biomolecule mark[8].Jeanson L etc. use iipidomic method to describe blood plasma
Network metabolic alterations in pulmonary cystic fibrosis for the lipid, the pathogenesis of pulmonary cystic fibrosis and cystic fibrosis transmembrane transmit
Regulatory factor gene mutation causes airway mucus to block, bacteria planting, and lung necrosis progrediens is relevant.The pulmonary cystic fiber of research discovery
Changing multiple PC and LPC in patients blood plasma all to significantly reduce, this shows that the change of phospholipid metabolism in blood plasma is sick to pulmonary cystic fibrosis
Change process plays an important role, and is the potential target spot of drug therapy[9]。
In the blood detecting of current existing report, lipid quantity is all less, or simply single a certain lipoid
The different detecting instrument using in matter, and different report detects the disunity of the testing result causing, and many counting methods knot
The means such as conjunction metabolism correlation networks analysis and database retrieval, the structure of the possible biomarker of analysis deduction, and non-usage
Standard items are pointed out, and result accuracy remains to be discussed, it is impossible to provide authentic and valid examination criteria.Also there is not a kind of pre-treatment of use
Detect 113 kinds of lipids of seven classes the report using whole standard items to point out by the technology of Liquid Chromatography-Tandem Mass Spectrometry after method simultaneously
Road.
[1]. Fan Shaojuan. the optical joint detection method of blood biomarker is explored. Tianjin. University Of Tianjin,
2013.
[2]. Lokhov PG, Trifonova OP, Maslov DL, Archakov AI. Blood plasma
Metabolites and the risk of developing lung cancer in Russia. ［ J ］. Eur J
Cancer Prev. 2013 Jul; 22(4):335-41.
[3]. Tang little Hu. find cancer of the esophagus biomarker based on metabolism group and the resistant organism mark of lung cancer grinds
Study carefully. Beijing. Beijing University of Chemical Technology, 2015.
[4]. Du Zhiyong. metabolism group method evaluates the basic and clinic studies of chronic heart failure metabolism reconstruct. ［ D ］.
Guangdong Province: south medical courses in general are big, 2012.
[5]. Cai Tanxi. Liu Pingsheng. Yang Fuquan. Yang Fuyu. iipidomic progress. biochemistry and biophysics
Progress, 2010,37 (2): 121-128.
[6]. Ma little Qiong, lipidomics and neurolipidomics are in progress [J], Chinese J Pharmacol Toxicol, and 2008,22
(2):156-160.
[7]. Qu Feng. iipidomics analysis technology and in discovery immunity disease and virus hepatitis associated biomarkers
The research of aspect. ［ D ］. Beijing: Beijing Union Medical College, 2014.
[8]. practise acute hearing, based on the patients with type Ⅰ DM serum lipids group research of technology. Beijing. Beijing Union Medical College, 2013.
[9]. Jeanson L, Guerrera IC, Papon JF, Chhuon C, Zadigue P, et. al.
Proteomic analysis of nasal epithelial cells from cystic fibrosis patients.
J ］. PLoS One. 2014 Sep 30;9(9).
Content of the invention
For solving problems of the prior art, the present invention provides 113 kinds of lipids in a kind of high flux detection blood
LC-MS method, provides a kind of detection efficiency height, degree of accuracy lipid detection technique accurately.Use high performance liquid chromatography
(HPLC) separate, electric spray ion source high-resolution time-of-flight mass spectrometry (ESI-Q-TOF-MS) measures in biological sample simultaneously
The composition of 113 kinds of lipid compounds.Wherein, high performance liquid chromatography with the methanol-water solution containing formic acid for flowing phase, electron spray from
Component high-resolution time-of-flight mass spectrometry uses internal standard method, carries out 113 kinds of lipid compounds qualitative simultaneously and analyzes.
The technical solution used in the present invention is: the liquid matter of 113 kinds of lipids in a kind of high flux detection organism blood sample
Method for combined use, uses Ultra Performance Liquid Chromatography to separate and electric spray ion source high-resolution time-of-flight mass spectrometry (ESI-Q-
TOF-MS) range of lipids composition detection in sample is analyzed by positive and negative ion scan pattern.Including phosphatid ylcholine (PC), haemolysis
Phosphatid ylcholine (Lyso-PC), phosphatidyl-ethanolamine (PE), lysophosphatidyl choline (Lyso-PC), haemolysis phosphinositides
(Lyso-PI), sphingomyelins (SM), ceramide (ceramide) amount to 7 constituents, totally 113 kinds of lipid monomeric compounds.
(1) foundation of reference material database
According to the ionized form under ESI source and chemical formula, obtain the accurate mass number of every kind of compound parent ion, form TOF/
MS database.Under Q-TOF/MS pattern, gather fragment ion under 3 different collision energies for the every kind of lipid reference material respectively
Mass spectrogram, forms Q-TOF/MS database；Described 3 different collision energies are respectively as follows: 20psi, 35psi and 50psi；Standard items
The dilution of inner mark solution is 80% methanol aqueous solution；
(2) biological blood sample process
1) take frozen blood plasma at-80 DEG C, thaw in 4 DEG C of refrigerators, take 10 μ L blood plasma, be sequentially added into 10 μ L mixing inner mark solutions,
10 μ L 0.9% NaCl, 100 μ L extracts, vortex 20s stands 30min after 4 DEG C of refrigerators, and described extract is volume ratio 2:1
The mixed liquor of chloroform and methyl alcohol；Described mixing inner mark solution is phosphatid ylcholine containing 19:0-19:0,17:0-17:0 phosphatide
Acyl monoethanolamine, 12:0 sphingomyelins, 19:0 lysophosphatidyl choline, concentration is the isopropanol-acetonitrile solution of 5 μ g/mL, different
Propyl alcohol, the ratio of acetonitrile are 1:1；
2) after taking standing, sample 7800g/min centrifuges 3min, with 1mL syringe absorption subnatant in 0.5mLEP pipe, inhales at once
Take 40 μ L in internal lining pipe, nitrogen seal after drying up be stored in-20 DEG C of refrigerators stand-by；
3) with 40 μ L acetonitriles before sample introduction: isopropanol volume ratio is that the mixed liquor of 1:1 redissolves, vortex 60s, sample introduction；
(3) qualitative detection
Use HPLC/ESI-Q-TOF-MS determination step 3) in blood sample treatment fluid, by comparison sample retain when
Between, first mass spectrometric and second order ms information, determine whether sample contains 113 kinds of target lipid components；
Chromatographic condition: column temperature: 50 DEG C, Sample Room temperature: 4 DEG C, flow velocity: 0.4 mL/min, sampling volume: 2 μ L, flow phase: A
Phase: 10 mmoL/L ammonium acetate+0.1% formic acid+99.9% water, B phase: 10 mmoL/L ammonium acetate+0.1% formic acid+49.95% acetonitriles
+ 49.95% isopropanol gradient elution.
Described gradient elution program is: 65/35(A/B, V/V during 0.01min), gradually change gradient and become 20/ to 2min
80(A/B, V/V), change gradient further and become 0/100(A/B, V/V to 9min), and maintain 15min, become to 16min
Initial concentration 65/35(A/B, V/V) and maintain 20min.
Cation detection Mass Spectrometry Conditions is: ion gun: ESI source；Ion spray voltage :+5.5kV；Turbine injection temperation
(TEM): 550 DEG C；GS1:50 psi；GS2:50 psi；CUR:30psi；TOF MS and TOF MS/MS sweep limits are respectively
For: m/z 100 1500 and 50 1200.Anionic textiles Mass Spectrometry Conditions is: ion gun: ESI source；Ion spray voltage :-
4.5kV；Turbine injection temperation (TEM): 550 DEG C；GS1:50 psi；GS2:50 psi；CUR:30psi；TOF MS and TOF-
MS/MS sweep limits is respectively as follows: m/z 200 1200 and 50 1200.
(4) relative quantification detection
With phosphatid ylcholine containing 19:0-19:0,17:0-17:0 phosphatidyl-ethanolamine, 12:0 sphingomyelins, 19:0 lysophosphatide
Isopropanol-the acetonitrile solution of phatidylcholine is internal standard, carries out relative quantification to the lipid components detecting in biological sample, at sample
Preprocessing process adds the internal standard compound that concentration determines, 19:0-19:0 phosphatid ylcholine, 17:0-17:0 phosphatidyl second
Hydramine, 12:0 sphingomyelins, 19:0 lysophosphatidyl choline, use peak area ratio method, the compound of each class corresponding its
Internal standard carries out relative quantification, if target in not corresponding, uses the principle that retention time is close to select internal standard to carry out relative quantification.
This patent method determines ionized form and chemical formula under this 113 kinds of compound ESI sources, obtains every kind of compound
Accurate mass number in negative ions collection for the parent ion, forms TOF/MS database.Under Q-TOF/MS pattern, gather respectively
Fragment ion mass spectrogram under the different collision energy of the positive and negative drainage pattern of every kind of lipid reference material, forms Q-TOF/MS database.
HPLC/ESI-Q-TOF-MS is used to measure biological sample treatment fluid, by retention time, one-level matter in comparison sample
Spectrum and second order ms information, determine whether contain 113 kinds of target lipid components in sample.
Chromatographic condition
Column temperature: 50 DEG C of Sample Room temperature: 4 DEG C of flow velocitys: 0.4 mL/min sampling volume: 2 μ L
Flowing phase: A:10 mmoL/L ammonium acetate+0.1% formic acid+99.9% water
B:10 mmoL/L ammonium acetate+0.1% formic acid+49.95% acetonitrile+49.95% isopropanol
Condition of gradient elution:
| Time(min) | A% | B% |
| 0.01 | 65 | 35 |
| 2 | 20 | 80 |
| 9 | 0 | 100 |
| 15 | 0 | 100 |
| 16 | 65 | 35 |
| 20 | 65 | 35 |
Mass spectrometry method
Positive ion mode parameter is arranged
| Parameter | TOF MS(+) | Product Ion(+)IDA |
| Atomization gas | 50 | 50 |
| Auxiliary gas | 50 | 50 |
| Gas curtain gas | 30 | 30 |
| Atomization temperature | 550 | 550 |
| Spray voltage | 5500 | 5500 |
| Sweep limits | 100-1500 | 50-1200 |
| Remove a bunch voltage | 80 | 80 |
| Collision energy | 10 | 35 |
| Collision voltage difference | ---- | 15 |
| Ion Release Delay(IRD) | ---- | 67 |
| Ion Release Width(IRW) | ---- | 25 |
Negative ion mode parameter is arranged
| Parameter | TOF MS(-) | Product Ion(-)IDA |
| Atomization gas | 50 | 50 |
| Auxiliary gas | 50 | 50 |
| Gas curtain gas | 30 | 30 |
| Atomization temperature | 550 | 550 |
| Spray voltage | 4500 | 4500 |
| Sweep limits | 200-1200 | 50-1200 |
| Remove a bunch voltage | -80 | -80 |
| Collision energy | -10 | -35 |
| Collision voltage difference | ---- | 15 |
| Ion Release Delay(IRD) | ---- | 67 |
| Ion Release Width(IRW) | ---- | 25 |
The application provides the benefit that: the method uses and sample to be tested pre-processed and added reaction dissolvent and extractant extraction
After, carry out liquid phase-Mass Spectrometer Method.The method is simple to operate, selectivity is high, highly sensitive, can quickly detect 113 kinds of fat in blood
Matter, wherein phosphatid ylcholine (PC) 48, lysophosphatidyl choline (Lyso-PC) 21, phosphatidyl-ethanolamine (PE) 17, molten
Serium inorganic phosphorus acyl monoethanolamine (LPE) 4, haemolysis phosphinositides (PI) 6, sphingomyelins (SM) 9, ceramide (Cer) 8.
The method simultaneously qualitative and quantitative can detect 113 kinds of lipids, and detection sensitivity is high.The precision of this method meets serum sample one's duty
Analysis requirement, have good stability, for major part lipid metabolin detection sensitivity higher, it is adaptable to the fat of serum sample
Matter group credit is analysed.
Brief description
Fig. 1 is lipid standard items LC-TOF-MS cation drainage pattern TIC chromatogram of the present invention.
Fig. 2 is lipid standard items LC-TOF-MS anion drainage pattern TIC chromatogram of the present invention.
Fig. 3 is blood sample lipid detection LC-TOF-MS cation drainage pattern TIC chromatogram in the actual application of the present invention
Figure.
Fig. 4 is blood sample lipid detection LC-TOF-MS anion drainage pattern TIC chromatogram in the actual application of the present invention
Figure.
Fig. 5 is lipid standard items LC-TOF-MS cation drainage pattern XIC chromatogram of the present invention.
Specific embodiments
Lipid species detection in one haemophiliac's blood
1) internal standard liquid and extract preparation
Inner mark solution: PC containing 19:0-19:0,17:0-17:0 PE, 12:0 SM, 19:0 Lyso PC concentration are 5 μ g/mL
Isopropanol-acetonitrile solution (1:1).Extract: chloroform-methanol (2:1).
2) patient blood samples's process
Patient blood samples's process, frozen blood plasma at-80 DEG C, thaws in 4 DEG C of refrigerators, takes 10 μ L blood plasma, be sequentially added into 10 μ L
Mixing inner mark solution, 10 μ L 0.9%NaCl, 100 μ L chloroform-methanol (2:1) extracts, vortex 20s, 4 DEG C of refrigerators stand
30min.7800g/min centrifuges 3min.1mL syringe absorption subnatant, in 0.5mLEP pipe, draws 40 μ L at once in internal lining pipe
In.Nitrogen dries up, and sealing is stored in-20 DEG C of refrigerators stand-by.Redissolve with 40 μ L acetonitriles-isopropanol (1:1) before sample introduction, vortex 60s,
Sample introduction.
3) standard items Database
Use HPLC/ESI-Q-TOF-MS to survey 113 kinds of lipid standard items mixed solutions in blood, determine this 113 kinds of compounds
Ionized form under ESI source and chemical formula, obtain the accurate mass number of every kind of compound parent ion, forms TOF/MS data
Storehouse.Under Q-TOF/MS pattern, gather fragment under the different collision energy of 35 ± 15psi tri-for the every kind of lipid reference material respectively
Ion massspectrum figure, forms Q-TOF/MS database.
4) qualitative detection
Use HPLC/ESI-Q-TOF-MS determination step 2) in blood sample treatment fluid, cation detection Mass Spectrometry Conditions be: from
Component: ESI source；Ion spray voltage :+5.5kV；Turbine injection temperation (TEM): 550 DEG C；GS1:50 psi；GS2:50 psi；
CUR:30psi；TOF MS and TOF MS/MS sweep limits are respectively as follows: m/z 100 1500 and 50 1200.Anion is examined
Surveying Mass Spectrometry Conditions is: ion gun: ESI source；Ion spray voltage :-4.5kV；Turbine injection temperation (TEM): 550 DEG C；GS1:50
psi；GS2:50 psi；CUR:30psi；TOF MS and TOF-MS/MS sweep limits are respectively as follows: m/z 200 1200 and 50
1200。
By retention time, first mass spectrometric and second order ms information in comparison sample, determine in human serum sample whether contain
Having 113 kinds of target lipid components, testing result sees attached list the 2nd, 3.
5) quantitatively detect
Subordinate list 1:113 kind lipid standard items essential information
| Numbering | Trade name | Molecular formula | Cation m/z | Anion m/z |
| 1 | Egg Lyso PC | C<sub>24</sub>H<sub>50</sub>NO<sub>7</sub>P | 496.3398 | 540.3296 |
| 2 | Soy Lyso PC | C<sub>24</sub>H<sub>50</sub>NO<sub>7</sub>P | 496.3398 | 540.3296 |
| 3 | 06:0 Lyso PC | C<sub>14</sub>H<sub>30</sub>NO<sub>7</sub>P | 356.1833 | 400.1731 |
| 4 | 07:0 Lyso PC | C<sub>15</sub>H<sub>32</sub>NO<sub>7</sub>P | 370.1989 | 414.1887 |
| 5 | 08:0 Lyso PC | C<sub>16</sub>H<sub>34</sub>NO<sub>7</sub>P | 384.2146 | 428.2044 |
| 6 | 09:0 Lyso PC | C<sub>17</sub>H<sub>36</sub>NO<sub>7</sub>P | 398.2302 | 442.2200 |
| 7 | 10:0 Lyso PC | C<sub>18</sub>H<sub>38</sub>NO<sub>7</sub>P | 412.2459 | 456.2357 |
| 8 | 11:0 Lyso PC | C<sub>19</sub>H<sub>40</sub>NO<sub>7</sub>P | 426.2615 | 470.2513 |
| 9 | 12:0 Lyso PC | C<sub>20</sub>H<sub>42</sub>NO<sub>7</sub>P | 440.2772 | 484.2670 |
| 10 | 13:0 Lyso PC | C<sub>21</sub>H<sub>44</sub>NO<sub>7</sub>P | 454.2928 | 498.2826 |
| 11 | 14:0 Lyso PC | C<sub>22</sub>H<sub>46</sub>NO<sub>7</sub>P | 468.3085 | 512.2983 |
| 12 | 15:0 Lyso PC | C<sub>23</sub>H<sub>48</sub>NO<sub>7</sub>P | 482.3241 | 526.3139 |
| 13 | 16:0 Lyso PC | C<sub>24</sub>H<sub>50</sub>NO<sub>7</sub>P | 496.3398 | 540.3296 |
| 14 | 17:0 Lyso PC | C<sub>25</sub>H<sub>52</sub>NO<sub>7</sub>P | 510.3554 | 554.3452 |
| 15 | 18:0 Lyso PC | C<sub>26</sub>H<sub>54</sub>NO<sub>7</sub>P | 524.3711 | 568.3609 |
| 16 | 18:1 Lyso PC | C<sub>26</sub>H<sub>52</sub>NO<sub>7</sub>P | 522.3554 | 566.3452 |
| 17 | 19:0 Lyso PC | C<sub>27</sub>H<sub>56</sub>NO<sub>7</sub>P | 538.3867 | 582.3765 |
| 18 | 20:0 Lyso PC | C<sub>28</sub>H<sub>58</sub>NO<sub>7</sub>P | 552.4024 | 596.3922 |
| 19 | 22:0 Lyso PC | C<sub>30</sub>H<sub>62</sub>NO<sub>7</sub>P | 580.4337 | 624.4235 |
| 20 | 24:0 Lyso PC | C<sub>32</sub>H<sub>66</sub>NO<sub>7</sub>P | 608.4650 | 652.4548 |
| 21 | 26:0 Lyso PC | C<sub>34</sub>H<sub>70</sub>NO<sub>7</sub>P | 636.4963 | 680.4861 |
| 22 | 13:0 Lyso PI | C<sub>22</sub>H<sub>46</sub>NO<sub>12</sub>P | 548.2830 | 529.2408 |
| 23 | 16:0 Lyso PI | C<sub>25</sub>H<sub>52</sub>NO<sub>12</sub>P | 590.3300 | 571.2877 |
| 24 | 18:0 Lyso PI | C<sub>27</sub>H<sub>56</sub>NO<sub>12</sub>P | 618.3613 | 599.31909 |
| 25 | 17:1 Lyso PI | C<sub>26</sub>H<sub>52</sub>NO<sub>12</sub>P | 602.3300 | 583.2877 |
| 26 | 18:1 Lyso PI | C<sub>27</sub>H<sub>54</sub>NO<sub>12</sub>P | 616.3456 | 597.3034 |
| 27 | 20:4 Lyso PI | C<sub>29</sub>H<sub>52</sub>NO<sub>12</sub>P | 638.3300 | 619.2877 |
| 28 | 06:0 PE | C<sub>17</sub>H<sub>34</sub>NO<sub>8</sub>P | 412.2095 | 410.1949 |
| 29 | 08:0 PE | C<sub>21</sub>H<sub>42</sub>NO<sub>8</sub>P | 468.2721 | 466.2575 |
| 30 | 10:0 PE | C<sub>25</sub>H<sub>50</sub>NO<sub>8</sub>P | 524.3347 | 522.3201 |
| 31 | 12:0 PE | C<sub>29</sub>H<sub>58</sub>NO<sub>8</sub>P | 580.3973 | 578.3827 |
| 32 | 14:0 PE | C<sub>33</sub>H<sub>66</sub>NO<sub>8</sub>P | 636.4599 | 634.4453 |
| 33 | 15:0 PE | C<sub>35</sub>H<sub>70</sub>NO<sub>8</sub>P | 664.4912 | 662.4766 |
| 34 | 16:0 PE | C<sub>37</sub>H<sub>74</sub>NO<sub>8</sub>P | 692.5225 | 690.5079 |
| 35 | 17:0 PE | C<sub>39</sub>H<sub>78</sub>NO<sub>8</sub>P | 720.5538 | 718.5392 |
| 36 | 18:0 PE | C<sub>41</sub>H<sub>82</sub>NO<sub>8</sub>P | 748.5851 | 746.5705 |
| 37 | 16:0-18:1 PE | C<sub>39</sub>H<sub>76</sub>NO<sub>8</sub>P | 718.5381 | 716.5235 |
| 38 | 16:0-18:2 PE | C<sub>39</sub>H<sub>74</sub>NO<sub>8</sub>P | 716.5225 | 714.5079 |
| 39 | 16:0-20:4 PE | C<sub>41</sub>H<sub>74</sub>NO<sub>8</sub>P | 740.5225 | 738.5079 |
| 40 | 16:0-22:6 PE | C<sub>43</sub>H<sub>74</sub>NO<sub>8</sub>P | 764.5225 | 762.5079 |
| 41 | 18:0-18:1 PE | C<sub>41</sub>H<sub>80</sub>NO<sub>8</sub>P | 746.5694 | 744.5548 |
| 42 | 18:0-18:2 PE | C<sub>41</sub>H<sub>78</sub>NO<sub>8</sub>P | 744.5538 | 742.5392 |
| 43 | 18:0-20:4 PE | C<sub>43</sub>H<sub>78</sub>NO<sub>8</sub>P | 768.5538 | 766.5392 |
| 44 | 18:0-22:6 PE | C<sub>45</sub>H<sub>78</sub>NO<sub>8</sub>P | 792.5538 | 790.5392 |
| 45 | 14:0 Lyso PE | C<sub>19</sub>H<sub>40</sub>NO<sub>7</sub>P | 426.2615 | 424.2469 |
| 46 | 16:0 Lyso PE | C<sub>21</sub>H<sub>44</sub>NO<sub>7</sub>P | 454.2928 | 452.2782 |
| 47 | 18:0 Lyso PE | C<sub>23</sub>H<sub>48</sub>NO<sub>7</sub>P | 482.3241 | 480.3095 |
| 48 | 18:1 Lyso PE | C<sub>23</sub>H<sub>46</sub>NO<sub>7</sub>P | 480.3085 | 478.2939 |
| 49 | 03:0 PC | C<sub>14</sub>H<sub>28</sub>NO<sub>8</sub>P | 370.1625 | 414.1523 |
| 50 | 04:0 PC | C<sub>16</sub>H<sub>32</sub>NO<sub>8</sub>P | 398.1938 | 442.1836 |
| 51 | 05:0 PC | C<sub>18</sub>H<sub>36</sub>NO<sub>8</sub>P | 426.2251 | 470.2149 |
| 52 | 06:0 PC (DHPC) | C<sub>20</sub>H<sub>40</sub>NO<sub>8</sub>P | 454.2564 | 498.2462 |
| 53 | 07:0 PC (DHPC) | C<sub>22</sub>H<sub>44</sub>NO<sub>8</sub>P | 482.2877 | 526.2775 |
| 54 | 08:0 PC | C<sub>24</sub>H<sub>48</sub>NO<sub>8</sub>P | 510.319 | 554.3088 |
| 55 | 09:0 PC | C<sub>26</sub>H<sub>52</sub>NO<sub>8</sub>P | 538.3503 | 582.3401 |
| 56 | 10:0 PC | C<sub>28</sub>H<sub>56</sub>NO<sub>8</sub>P | 566.3816 | 610.3714 |
| 57 | 11:0 PC | C<sub>30</sub>H<sub>60</sub>NO<sub>8</sub>P | 594.4129 | 638.4027 |
| 58 | 12:0 PC (DLPC) | C<sub>32</sub>H<sub>64</sub>NO<sub>8</sub>P | 622.4442 | 666.4340 |
| 59 | 13:0 PC | C<sub>34</sub>H<sub>68</sub>NO<sub>8</sub>P | 650.4755 | 694.4653 |
| 60 | 14:0 PC (DMPC) | C<sub>36</sub>H<sub>72</sub>NO<sub>8</sub>P | 678.5068 | 722.4966 |
| 61 | 15:0 PC | C<sub>38</sub>H<sub>76</sub>NO<sub>8</sub>P | 706.5381 | 750.5279 |
| 62 | 16:0 PC (DPPC) | C<sub>40</sub>H<sub>80</sub>NO<sub>8</sub>P | 734.5694 | 778.5592 |
| 63 | 17:0 PC | C<sub>42</sub>H<sub>84</sub>NO<sub>8</sub>P | 762.6007 | 806.5905 |
| 64 | 18:0 PC (DSPC) | C<sub>44</sub>H<sub>88</sub>NO<sub>8</sub>P | 790.632 | 834.6218 |
| 65 | 19:0 PC | C<sub>46</sub>H<sub>92</sub>NO<sub>8</sub>P | 818.6633 | 862.6531 |
| 66 | 20:0 PC | C<sub>48</sub>H<sub>96</sub>NO<sub>8</sub>P | 846.6946 | 890.6844 |
| 67 | 21:0 PC | C<sub>50</sub>H<sub>100</sub>NO<sub>8</sub>P | 874.7259 | 918.7157 |
| 68 | 22:0 PC | C<sub>52</sub>H<sub>104</sub>NO<sub>8</sub>P | 902.7572 | 946.7470 |
| 69 | 23:0 PC | C<sub>54</sub>H<sub>108</sub>NO<sub>8</sub>P | 930.7885 | 974.7783 |
| 70 | 24:0 PC | C<sub>56</sub>H<sub>112</sub>NO<sub>8</sub>P | 958.8198 | 1002.8096 |
| 71 | 14:1 (Δ9-Cis) PC | C<sub>36</sub>H<sub>68</sub>NO<sub>8</sub>P | 674.4755 | 718.4653 |
| 72 | 14:1 (Δ9-Trans) PC | C<sub>36</sub>H<sub>68</sub>NO<sub>8</sub>P | 674.4755 | 718.4653 |
| 73 | 16:1 (Δ9-Cis) PC | C<sub>40</sub>H<sub>76</sub>NO<sub>8</sub>P | 730.5381 | 774.5279 |
| 74 | 16:1 (Δ9-Trans) PC | C<sub>40</sub>H<sub>76</sub>NO<sub>8</sub>P | 730.5381 | 774.5279 |
| 75 | 18:1 (Δ6-Cis) PC | C<sub>44</sub>H<sub>84</sub>NO<sub>8</sub>P | 786.6007 | 830.5905 |
| 76 | 18:1 (Δ9-Cis) PC (DOPC) | C<sub>44</sub>H<sub>84</sub>NO<sub>8</sub>P | 786.6007 | 830.5905 |
| 77 | 18:1 (Δ9-Trans) PC | C<sub>44</sub>H<sub>84</sub>NO<sub>8</sub>P | 786.6007 | 830.5905 |
| 78 | 18:2 (Cis) PC (DLPC) | C<sub>44</sub>H<sub>80</sub>NO<sub>8</sub>P | 782.5694 | 826.5592 |
| 79 | 18:3 (Cis) PC | C<sub>44</sub>H<sub>76</sub>NO<sub>8</sub>P | 778.5381 | 822.5279 |
| 80 | 20:1 (Cis) PC | C<sub>48</sub>H<sub>92</sub>NO<sub>8</sub>P | 842.6633 | 886.6531 |
| 81 | 20:4 (Cis) PC | C<sub>48</sub>H<sub>80</sub>NO<sub>8</sub>P | 830.5694 | 874.5592 |
| 82 | 22:1 (Cis) PC | C<sub>52</sub>H<sub>100</sub>NO<sub>8</sub>P | 898.7259 | 942.7157 |
| 83 | 22:6 (Cis) PC | C<sub>52</sub>H<sub>80</sub>NO<sub>8</sub>P | 878.5694 | 922.5592 |
| 84 | 24:1 (Cis) PC | C<sub>56</sub>H<sub>108</sub>NO<sub>8</sub>P | 954.7885 | 998.7783 |
| 85 | 14:0-16:0 PC | C<sub>38</sub>H<sub>76</sub>NO<sub>8</sub>P | 706.5381 | 750.5279 |
| 86 | 14:0-18:0 PC | C<sub>40</sub>H<sub>80</sub>NO<sub>8</sub>P | 734.5694 | 778.5592 |
| 87 | 16:0-02:0 PC | C<sub>26</sub>H<sub>52</sub>NO<sub>8</sub>P | 538.3503 | 582.3401 |
| 88 | 16:0-14:0 PC | C<sub>38</sub>H<sub>76</sub>NO<sub>8</sub>P | 706.5381 | 750.5279 |
| 89 | 16:0-18:0 PC | C<sub>42</sub>H<sub>84</sub>NO<sub>8</sub>P | 762.6007 | 806.5905 |
| 90 | 16:0-18:1 PC | C<sub>42</sub>H<sub>82</sub>NO<sub>8</sub>P | 760.5851 | 804.5749 |
| 91 | 18:0-18:2 PC | C<sub>44</sub>H<sub>84</sub>NO<sub>8</sub>P | 786.6007 | 830.5905 |
| 92 | 18:0-20:4 PC | C<sub>46</sub>H<sub>84</sub>NO<sub>8</sub>P | 810.6007 | 854.5905 |
| 93 | 18:0-22:6 PC | C<sub>48</sub>H<sub>84</sub>NO<sub>8</sub>P | 834.6007 | 878.5905 |
| 94 | 18:1-14:0 PC | C<sub>40</sub>H<sub>78</sub>NO<sub>8</sub>P | 732.5538 | 776.5436 |
| 95 | 18:1-16:0 PC | C<sub>42</sub>H<sub>82</sub>NO<sub>8</sub>P | 760.5851 | 804.5749 |
| 96 | 18:1-18:0 PC | C<sub>44</sub>H<sub>86</sub>NO<sub>8</sub>P | 788.6164 | 832.6062 |
| 97 | 02:0 SM (d18:1/2:0) | C<sub>25</sub>H<sub>51</sub>N<sub>2</sub>O<sub>6</sub>P | 507.3558 | 551.3455 |
| 98 | 06:0 SM (d18:1/6:0) | C<sub>29</sub>H<sub>59</sub>N<sub>2</sub>O<sub>6</sub>P | 563.4184 | 607.4081 |
| 99 | 12:0 SM (d18:1/12:0) | C<sub>35</sub>H<sub>71</sub>N<sub>2</sub>O<sub>6</sub>P | 647.5123 | 691.5020 |
| 100 | 16:0 SM (d18:1/16:0) | C<sub>39</sub>H<sub>79</sub>N<sub>2</sub>O<sub>6</sub>P | 703.5749 | 747.5646 |
| 101 | 17:0 SM (d18:1/17:0) | C<sub>40</sub>H<sub>81</sub>N<sub>2</sub>O<sub>6</sub>P | 717.5905 | 761.5803 |
| 102 | 18:0 SM (d18:1/18:0) | C<sub>41</sub>H<sub>83</sub>N<sub>2</sub>O<sub>6</sub>P | 731.6062 | 775.5959 |
| 103 | 18:1 SM (d18:1/18:1(9Z)) | C<sub>41</sub>H<sub>81</sub>N<sub>2</sub>O<sub>6</sub>P | 729.5905 | 773.5803 |
| 104 | 24:0 SM | C<sub>47</sub>H<sub>95</sub>N<sub>2</sub>O<sub>6</sub>P | 815.7001 | 859.6898 |
| 105 | 24:1 SM | C<sub>47</sub>H<sub>93</sub>N<sub>2</sub>O<sub>6</sub>P | 813.6844 | 857.6742 |
| 106 | 16:0 ceramide | C34H67NO3 | 560.5013 | 582.5092 |
| 107 | 18:0 ceramide | C36H71NO3 | 588.5326 | 610.5405 |
| 108 | 18:1 ceramide | C36H69NO3 | 586.517 | 608.5249 |
| 109 | 19:0 ceramide | C37H73NO3 | 602.5483 | 624.5562 |
| 110 | 20:0 ceramide | C38H75NO3 | 616.5639 | 638.5718 |
| 111 | 22:0 ceramide | C40H79NO3 | 644.5952 | 666.6031 |
| 112 | 24:0 ceramide | C42H83NO3 | 672.6265 | 694.6344 |
| 113 | 24:1 ceramide | C42H81NO3 | 670.6109 | 692.6188 |
Subordinate list 2: haemophiliac's serum lipids positive ion mode testing result
Subordinate list 3: haemophiliac's serum lipids negative ion mode testing result
Claims (3)
1. high flux detects a LC-MS method for 113 kinds of lipids in organism blood sample, uses ultra high efficiency liquid phase look
Spectrum separates with electric spray ion source high-resolution time-of-flight mass spectrometry (ESI-Q-TOF-MS) positive and negative ion scan pattern to sample
In Ben, range of lipids composition detection is analyzed, it is characterised in that said method comprising the steps of:
(1) foundation of reference material database
According to the ionized form under ESI source and chemical formula, obtain the accurate mass number of every kind of compound parent ion, form TOF/
MS database；Under Q-TOF/MS pattern, gather fragment ion under 3 different collision energies for the every kind of lipid reference material respectively
Mass spectrogram, forms Q-TOF/MS database；
(2) biological blood sample process
Take blood plasma and add mixing inner mark solution, add extract, centrifugal；Take off clear, after nitrogen dries up, add redissolution liquid to carry out
Redissolve, obtain testing sample；Described extract is the mixed liquor with methyl alcohol for the chloroform of volume ratio 2:1；Described mixing inner mark solution
For phosphatid ylcholine containing 19:0-19:0,17:0-17:0 phosphatidyl-ethanolamine, 12:0 sphingomyelins, 19:0 hemolytic phosphatidyl courage
Alkali concn is the isopropanol-acetonitrile solution of 5 μ g/mL；Described redissolution liquid is acetonitrile: isopropanol volume ratio is the mixing of 1:1
Liquid；
(3) qualitative detection
HPLC/ESI-Q-TOF-MS is used to measure testing sample, by retention time, first mass spectrometric and two grades in comparison sample
Information in Mass Spectra, determines whether contain 113 kinds of target lipid components in sample；
HPLC chromatogram condition: column temperature: 50 DEG C, Sample Room temperature: 4 DEG C, flow velocity: 0.4 mL/min, sampling volume: 2 μ L, flowing
Phase: A phase: ammonium acetate containing 10mM/L, the water of volume fraction 0.1% formic acid, B phase: ammonium acetate containing 10mM/L, volume fraction 0.1% first
Acetonitrile-isopropanol the mixed liquor of acid, acetonitrile in acetonitrile-isopropanol mixed liquor: the volume ratio of isopropanol is 1:1, eluent gradient
Wash-out；
Cation detection Mass Spectrometry Conditions is: ion gun: ESI source；Ion spray voltage :+5.5kV；Turbine injection temperation (TEM):
550℃；GS1:50 psi；GS2:50 psi；CUR:30psi；TOF MS and TOF MS/MS sweep limits are respectively as follows: m/z
100 1500 and 50 1200；
Anionic textiles Mass Spectrometry Conditions is: ion gun: ESI source；Ion spray voltage :-4.5kV；Turbine injection temperation (TEM):
550℃；GS1:50 psi；GS2:50 psi；CUR:30psi；TOF MS and TOF-MS/MS sweep limits are respectively as follows: m/z
200 1200 and 50 1200.
2. a kind of high flux according to claim 1 detects the LC-MS side of 113 kinds of lipids in organism blood sample
Method, it is characterised in that: it also include lipid relative quantification detection, detection method for phosphatid ylcholine containing 19:0-19:0,
17:0-17:0 phosphatidyl-ethanolamine, 12:0 sphingomyelins, the isopropanol-acetonitrile solution of 19:0 lysophosphatidyl choline are interior
Mark, carries out relative quantification to the lipid components detecting in biological sample, uses peak area ratio method, the compound of each class
Its internal standard corresponding carries out relative quantification, if target in not corresponding, uses the principle that retention time is close to select internal standard to carry out phase
To quantitatively.
3. a kind of high flux according to claim 1 detects the LC-MS side of 113 kinds of lipids in organism blood sample
Method, it is characterised in that: described gradient elution program is: during 0.01min, the volume ratio of A phase/B phase is 65/35, gradually changes gradient
The volume ratio becoming A phase/B phase to 2min is 20/80, and the volume ratio that change gradient becomes A phase/B phase to 9min further is 0/
100, and maintain 15min, the volume ratio becoming initial concentration A phase/B phase to 16min is 65/35 and maintains 20min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610380851.2A CN106093227A (en) | 2016-06-01 | 2016-06-01 | The LC-MS method of 113 kinds of lipids in a kind of high flux detection organism blood sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610380851.2A CN106093227A (en) | 2016-06-01 | 2016-06-01 | The LC-MS method of 113 kinds of lipids in a kind of high flux detection organism blood sample |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106093227A true CN106093227A (en) | 2016-11-09 |
Family
ID=57230130
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610380851.2A Pending CN106093227A (en) | 2016-06-01 | 2016-06-01 | The LC-MS method of 113 kinds of lipids in a kind of high flux detection organism blood sample |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106093227A (en) |
Cited By (32)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107085061A (en) * | 2017-05-22 | 2017-08-22 | 天津市第三中心医院 | The absolute quantification analysis method of lysophosphatidyl choline based on HPLC MS/MS detection platforms |
| CN107389847A (en) * | 2017-06-05 | 2017-11-24 | 中国农业科学院蜜蜂研究所 | A kind of method of lipid component in quick analysis Bee Pollen |
| CN107632095A (en) * | 2017-09-19 | 2018-01-26 | 中山大学 | A kind of detection method of crop glycolipid and phosphatide |
| CN107957467A (en) * | 2017-12-13 | 2018-04-24 | 上海景峰制药有限公司 | A kind of method of lysophosphatidyl choline in separation determination pharmaceutical preparation |
| CN108181387A (en) * | 2017-12-20 | 2018-06-19 | 烟台东诚药业集团股份有限公司 | The new method of phospholipid fraction content detection in a kind of Curosurf bulk pharmaceutical chemicals |
| CN108845051A (en) * | 2018-06-22 | 2018-11-20 | 中国农业科学院农业质量标准与检测技术研究所 | A method of based on sphingolipid in UHPLC-QTrap MS detection zebra fish brain tissue |
| CN109001360A (en) * | 2018-10-09 | 2018-12-14 | 南京财经大学 | A kind of method of high-throughput detection phospholipid in lipid content |
| CN109813813A (en) * | 2019-01-18 | 2019-05-28 | 中国农业科学院农业质量标准与检测技术研究所 | Method for identifying UHT milk and reconstituted milk based on lipidome |
| CN109870536A (en) * | 2017-12-05 | 2019-06-11 | 中国科学院大连化学物理研究所 | A high-coverage lipidomic analysis method based on liquid chromatography-mass spectrometry |
| CN109884200A (en) * | 2019-02-22 | 2019-06-14 | 嘉兴迈维代谢生物科技有限公司 | A kind of quick exploitation and the method for establishing standard items LC-MS database |
| CN109946390A (en) * | 2017-12-20 | 2019-06-28 | 上海生物信息技术研究中心 | A kind of combination of pulmonary cancer diagnosis marker and application |
| CN110007032A (en) * | 2019-04-30 | 2019-07-12 | 江南大学 | A kind of phospholipid detection method and application |
| CN110068638A (en) * | 2019-05-21 | 2019-07-30 | 中山大学孙逸仙纪念医院 | A kind of method of acid sphingolipid and glycosphingolipid in special separation and concentration human serum |
| CN110243956A (en) * | 2019-05-20 | 2019-09-17 | 北京三元食品股份有限公司 | A kind of food lipids extraction and the method for detecting food lipid |
| CN110470764A (en) * | 2019-08-30 | 2019-11-19 | 天津云检医学检验所有限公司 | A kind of semi-quantitative analysis method of lipid |
| CN110542730A (en) * | 2019-08-30 | 2019-12-06 | 天津云检医学检验所有限公司 | Absolute quantitative analysis method of ceramide |
| CN110596278A (en) * | 2018-10-22 | 2019-12-20 | 嘉兴迈维代谢生物科技有限公司 | Metabolite liquid chromatography-mass spectrometry combined detection method |
| CN111435132A (en) * | 2019-01-15 | 2020-07-21 | 武汉艾迪康医学检验所有限公司 | Lysophosphatidylcholine detection kit and detection method |
| CN111679026A (en) * | 2020-06-17 | 2020-09-18 | 中国农业科学院农业质量标准与检测技术研究所 | A cellular lipidomic analysis method based on ultra-high performance liquid chromatography tandem high-resolution mass spectrometry |
| CN111721859A (en) * | 2020-06-05 | 2020-09-29 | 珠海沅芷健康科技有限公司 | Early Alzheimer disease mouse lipidomics analysis method based on ultra-high performance liquid phase tandem high-resolution mass spectrometry and application |
| CN111830186A (en) * | 2020-09-04 | 2020-10-27 | 黄河三角洲京博化工研究院有限公司 | Method for representing molecular weight distribution of polyketone by liquid chromatography-mass spectrometry |
| CN112129875A (en) * | 2020-09-24 | 2020-12-25 | 中国农业科学院油料作物研究所 | A mass spectrometry method for identifying chain-length isomers of phosphatidylcholine |
| CN112362771A (en) * | 2020-10-29 | 2021-02-12 | 上海鹿明生物科技有限公司 | Method for high-throughput analysis of plant secondary metabolites based on LCMS and application |
| CN112730638A (en) * | 2020-11-25 | 2021-04-30 | 首都医科大学附属北京朝阳医院 | Diabetes combined myocardial infarction metabolism marker, detection reagent and kit |
| CN112881567A (en) * | 2020-12-31 | 2021-06-01 | 上海鹿明生物科技有限公司 | Detection method and application of phospholipid compounds classified in high abundance and low abundance in cells |
| CN113295793A (en) * | 2021-05-20 | 2021-08-24 | 复旦大学附属中山医院 | Biomarker for predicting early diabetes and diabetes occurrence, detection method and application thereof |
| CN113834888A (en) * | 2021-09-23 | 2021-12-24 | 大连润生康泰医学检验实验室有限公司 | Accurate detection method and kit for 4 ceramides in blood |
| WO2022033576A1 (en) * | 2020-08-14 | 2022-02-17 | 宝枫生物科技（北京）有限公司 | Method for diagnosing acting of nervonic acid, and application thereof |
| CN114236016A (en) * | 2022-01-21 | 2022-03-25 | 武汉迈特维尔生物科技有限公司 | A rapid and accurate method for the determination of 48 free fatty acids in biological samples |
| CN114778734A (en) * | 2022-04-22 | 2022-07-22 | 江南大学 | Quantitative determination method and application of polar lipid |
| CN115201392A (en) * | 2022-05-20 | 2022-10-18 | 澳优乳业（中国）有限公司 | Method for detecting phospholipid in dairy product |
| US20230138381A1 (en) * | 2020-11-27 | 2023-05-04 | Hainan Medical University | A lc-ms/ms method for measurement of aloesin in rat plasma |
-
2016
- 2016-06-01 CN CN201610380851.2A patent/CN106093227A/en active Pending
Cited By (48)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107085061A (en) * | 2017-05-22 | 2017-08-22 | 天津市第三中心医院 | The absolute quantification analysis method of lysophosphatidyl choline based on HPLC MS/MS detection platforms |
| CN107085061B (en) * | 2017-05-22 | 2019-03-15 | 天津市第三中心医院 | The absolute quantification analysis method of lysophosphatidyl choline based on HPLC-MS/MS detection platform |
| CN107389847A (en) * | 2017-06-05 | 2017-11-24 | 中国农业科学院蜜蜂研究所 | A kind of method of lipid component in quick analysis Bee Pollen |
| CN107389847B (en) * | 2017-06-05 | 2020-01-07 | 中国农业科学院蜜蜂研究所 | A method for rapid analysis of lipid components in bee pollen |
| CN107632095A (en) * | 2017-09-19 | 2018-01-26 | 中山大学 | A kind of detection method of crop glycolipid and phosphatide |
| CN109870536A (en) * | 2017-12-05 | 2019-06-11 | 中国科学院大连化学物理研究所 | A high-coverage lipidomic analysis method based on liquid chromatography-mass spectrometry |
| CN109870536B (en) * | 2017-12-05 | 2021-08-10 | 中国科学院大连化学物理研究所 | High-coverage lipidomics analysis method based on liquid chromatography-mass spectrometry |
| CN107957467A (en) * | 2017-12-13 | 2018-04-24 | 上海景峰制药有限公司 | A kind of method of lysophosphatidyl choline in separation determination pharmaceutical preparation |
| CN107957467B (en) * | 2017-12-13 | 2021-02-26 | 上海景峰制药有限公司 | Method for separating and measuring lysophosphatidylcholine in pharmaceutical preparation |
| CN109946390A (en) * | 2017-12-20 | 2019-06-28 | 上海生物信息技术研究中心 | A kind of combination of pulmonary cancer diagnosis marker and application |
| CN108181387A (en) * | 2017-12-20 | 2018-06-19 | 烟台东诚药业集团股份有限公司 | The new method of phospholipid fraction content detection in a kind of Curosurf bulk pharmaceutical chemicals |
| CN108845051A (en) * | 2018-06-22 | 2018-11-20 | 中国农业科学院农业质量标准与检测技术研究所 | A method of based on sphingolipid in UHPLC-QTrap MS detection zebra fish brain tissue |
| CN108845051B (en) * | 2018-06-22 | 2021-07-06 | 中国农业科学院农业质量标准与检测技术研究所 | A method for the detection of sphingolipids in zebrafish brain tissue based on UHPLC-QTrap MS |
| CN109001360A (en) * | 2018-10-09 | 2018-12-14 | 南京财经大学 | A kind of method of high-throughput detection phospholipid in lipid content |
| CN110596278B (en) * | 2018-10-22 | 2021-06-22 | 嘉兴迈维代谢生物科技有限公司 | Metabolite liquid chromatography-mass spectrometry combined detection method |
| CN110596278A (en) * | 2018-10-22 | 2019-12-20 | 嘉兴迈维代谢生物科技有限公司 | Metabolite liquid chromatography-mass spectrometry combined detection method |
| CN111435132A (en) * | 2019-01-15 | 2020-07-21 | 武汉艾迪康医学检验所有限公司 | Lysophosphatidylcholine detection kit and detection method |
| CN109813813A (en) * | 2019-01-18 | 2019-05-28 | 中国农业科学院农业质量标准与检测技术研究所 | Method for identifying UHT milk and reconstituted milk based on lipidome |
| CN109813813B (en) * | 2019-01-18 | 2022-01-28 | 中国农业科学院农业质量标准与检测技术研究所 | Method for identifying ultra-high temperature sterilized milk and reconstituted milk based on lipid group |
| CN109884200A (en) * | 2019-02-22 | 2019-06-14 | 嘉兴迈维代谢生物科技有限公司 | A kind of quick exploitation and the method for establishing standard items LC-MS database |
| CN110007032A (en) * | 2019-04-30 | 2019-07-12 | 江南大学 | A kind of phospholipid detection method and application |
| CN110243956A (en) * | 2019-05-20 | 2019-09-17 | 北京三元食品股份有限公司 | A kind of food lipids extraction and the method for detecting food lipid |
| CN110243956B (en) * | 2019-05-20 | 2021-06-18 | 北京三元食品股份有限公司 | Method for extracting and detecting food lipid |
| CN110068638B (en) * | 2019-05-21 | 2021-11-26 | 中山大学孙逸仙纪念医院 | Method for specifically separating and enriching acidic sphingolipids and glycosphingolipids in human serum |
| CN110068638A (en) * | 2019-05-21 | 2019-07-30 | 中山大学孙逸仙纪念医院 | A kind of method of acid sphingolipid and glycosphingolipid in special separation and concentration human serum |
| CN110542730A (en) * | 2019-08-30 | 2019-12-06 | 天津云检医学检验所有限公司 | Absolute quantitative analysis method of ceramide |
| CN110470764A (en) * | 2019-08-30 | 2019-11-19 | 天津云检医学检验所有限公司 | A kind of semi-quantitative analysis method of lipid |
| CN111721859A (en) * | 2020-06-05 | 2020-09-29 | 珠海沅芷健康科技有限公司 | Early Alzheimer disease mouse lipidomics analysis method based on ultra-high performance liquid phase tandem high-resolution mass spectrometry and application |
| CN111679026A (en) * | 2020-06-17 | 2020-09-18 | 中国农业科学院农业质量标准与检测技术研究所 | A cellular lipidomic analysis method based on ultra-high performance liquid chromatography tandem high-resolution mass spectrometry |
| WO2022033576A1 (en) * | 2020-08-14 | 2022-02-17 | 宝枫生物科技（北京）有限公司 | Method for diagnosing acting of nervonic acid, and application thereof |
| CN111830186B (en) * | 2020-09-04 | 2022-12-06 | 黄河三角洲京博化工研究院有限公司 | Method for representing molecular weight distribution of polyketone by liquid chromatography-mass spectrometry |
| CN111830186A (en) * | 2020-09-04 | 2020-10-27 | 黄河三角洲京博化工研究院有限公司 | Method for representing molecular weight distribution of polyketone by liquid chromatography-mass spectrometry |
| CN112129875A (en) * | 2020-09-24 | 2020-12-25 | 中国农业科学院油料作物研究所 | A mass spectrometry method for identifying chain-length isomers of phosphatidylcholine |
| CN112129875B (en) * | 2020-09-24 | 2023-05-26 | 中国农业科学院油料作物研究所 | Mass spectrometry method for identifying phosphatidylcholine chain length isomer |
| CN112362771A (en) * | 2020-10-29 | 2021-02-12 | 上海鹿明生物科技有限公司 | Method for high-throughput analysis of plant secondary metabolites based on LCMS and application |
| CN112730638A (en) * | 2020-11-25 | 2021-04-30 | 首都医科大学附属北京朝阳医院 | Diabetes combined myocardial infarction metabolism marker, detection reagent and kit |
| CN112730638B (en) * | 2020-11-25 | 2022-07-29 | 首都医科大学附属北京朝阳医院 | Diabetes combined myocardial infarction metabolism marker, detection reagent and kit |
| US12105070B2 (en) * | 2020-11-27 | 2024-10-01 | Hainan Medical University | LC-MS/MS method for measurement of Aloesin in rat plasma |
| US20230138381A1 (en) * | 2020-11-27 | 2023-05-04 | Hainan Medical University | A lc-ms/ms method for measurement of aloesin in rat plasma |
| CN112881567A (en) * | 2020-12-31 | 2021-06-01 | 上海鹿明生物科技有限公司 | Detection method and application of phospholipid compounds classified in high abundance and low abundance in cells |
| CN113295793A (en) * | 2021-05-20 | 2021-08-24 | 复旦大学附属中山医院 | Biomarker for predicting early diabetes and diabetes occurrence, detection method and application thereof |
| CN113834888A (en) * | 2021-09-23 | 2021-12-24 | 大连润生康泰医学检验实验室有限公司 | Accurate detection method and kit for 4 ceramides in blood |
| CN113834888B (en) * | 2021-09-23 | 2022-06-28 | 大连润生康泰医学检验实验室有限公司 | Accurate detection method and kit for 4 ceramides in blood |
| CN114236016A (en) * | 2022-01-21 | 2022-03-25 | 武汉迈特维尔生物科技有限公司 | A rapid and accurate method for the determination of 48 free fatty acids in biological samples |
| CN114778734A (en) * | 2022-04-22 | 2022-07-22 | 江南大学 | Quantitative determination method and application of polar lipid |
| CN114778734B (en) * | 2022-04-22 | 2024-05-07 | 江南大学 | A quantitative determination method for polar lipids and its application |
| CN115201392A (en) * | 2022-05-20 | 2022-10-18 | 澳优乳业（中国）有限公司 | Method for detecting phospholipid in dairy product |
| CN115201392B (en) * | 2022-05-20 | 2023-12-15 | 澳优乳业（中国）有限公司 | A method for detecting phospholipids in dairy products |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106093227A (en) | The LC-MS method of 113 kinds of lipids in a kind of high flux detection organism blood sample | |
| Tao et al. | Metabolomics identifies serum and exosomes metabolite markers of pancreatic cancer | |
| Wolrab et al. | Oncolipidomics: Mass spectrometric quantitation of lipids in cancer research | |
| Ros-Mazurczyk et al. | Serum lipid profile discriminates patients with early lung cancer from healthy controls | |
| Guo et al. | Probing gender-specific lipid metabolites and diagnostic biomarkers for lung cancer using Fourier transform ion cyclotron resonance mass spectrometry | |
| CN108414660B (en) | Application of group of plasma metabolism small molecule markers related to early diagnosis of lung cancer | |
| US8653006B2 (en) | Metabolite biomarkers for the detection of esophageal cancer using NMR | |
| CN109725072A (en) | A targeted qualitative and quantitative metabolomic analysis method for screening cancer biomarkers based on LC-MS/MS technology | |
| CN107037144B (en) | A kind of ultra performance liquid chromatography tandem mass spectrum method of target metabolic object content in detection body fluid | |
| Zhu et al. | Metabolomic analysis of exosomal-markers in esophageal squamous cell carcinoma | |
| Baila-Rueda et al. | Simultaneous determination of oxysterols, phytosterols and cholesterol precursors by high performance liquid chromatography tandem mass spectrometry in human serum | |
| US9739780B2 (en) | Metabolite biomarkers for the detection of liver cancer | |
| Wu et al. | Absolute quantitative imaging of sphingolipids in brain tissue by exhaustive liquid microjunction surface sampling–liquid chromatography–mass spectrometry | |
| Dickinson et al. | Mass spectrometry–based lipidomics of oral squamous cell carcinoma tissue reveals aberrant cholesterol and glycerophospholipid metabolism—A Pilot study | |
| CN108680745A (en) | Application process of the serum lipids biomarker in NSCLC early diagnosis | |
| Matos Do Canto et al. | Metabolomic profiling of breast tumors using ductal fluid | |
| Seubnooch et al. | Characterisation of hepatic lipid signature distributed across the liver zonation using mass spectrometry imaging | |
| CN112183616B (en) | Diagnostic marker and kit for diagnosis of glioma, screening method and construction method of glioma diagnostic model | |
| Cao et al. | Database-assisted global metabolomics profiling of pleural effusion induced by tuberculosis and malignancy | |
| CN111896641B (en) | Small molecule screening method and application of colorectal cancer-related estrogen plasma metabolism | |
| Yang et al. | A green and efficient pseudotargeted lipidomics method for the study of depression based on ultra-high performance supercritical fluid chromatography-tandem mass spectrometry | |
| Zhong et al. | Serum metabolomic study for the detection of candidate biomarkers of tuberculosis | |
| ES2960011T3 (en) | Cancer diagnosis method based on lipidomic analysis of a body fluid | |
| Yang et al. | Determination of amino acid metabolic diseases from dried blood spots with a rapid extraction method coupled with nanoelectrospray ionization mass spectrometry | |
| Yifan et al. | Global serum metabolomic and lipidomic analyses reveal lipid perturbations and potential biomarkers of the colorectal cancer by adenoma-carcinoma sequence |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20161109 |