CN106645374A - Online-internal-extraction electrospray-ionization mass-spectroscopy detection device for rapidly analyzing body fluid samples of human body - Google Patents
Online-internal-extraction electrospray-ionization mass-spectroscopy detection device for rapidly analyzing body fluid samples of human body Download PDFInfo
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- CN106645374A CN106645374A CN201611215422.6A CN201611215422A CN106645374A CN 106645374 A CN106645374 A CN 106645374A CN 201611215422 A CN201611215422 A CN 201611215422A CN 106645374 A CN106645374 A CN 106645374A
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- 210000001124 body fluid Anatomy 0.000 title claims abstract description 28
- 239000010839 body fluid Substances 0.000 title claims abstract description 28
- 238000001514 detection method Methods 0.000 title claims abstract description 21
- 238000004949 mass spectrometry Methods 0.000 title claims abstract description 18
- 238000000093 extraction electrospray ionisation Methods 0.000 title claims abstract description 12
- 238000011065 in-situ storage Methods 0.000 claims abstract description 21
- 238000004458 analytical method Methods 0.000 claims abstract description 20
- 238000011068 loading method Methods 0.000 claims abstract description 5
- 239000000945 filler Substances 0.000 claims description 34
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 27
- 238000002470 solid-phase micro-extraction Methods 0.000 claims description 27
- 239000012528 membrane Substances 0.000 claims description 23
- 238000000605 extraction Methods 0.000 claims description 22
- 239000003480 eluent Substances 0.000 claims description 20
- 238000002347 injection Methods 0.000 claims description 19
- 239000007924 injection Substances 0.000 claims description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 18
- 230000002146 bilateral effect Effects 0.000 claims description 16
- 239000007921 spray Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- 239000004696 Poly ether ether ketone Substances 0.000 claims description 12
- JUPQTSLXMOCDHR-UHFFFAOYSA-N benzene-1,4-diol;bis(4-fluorophenyl)methanone Chemical compound OC1=CC=C(O)C=C1.C1=CC(F)=CC=C1C(=O)C1=CC=C(F)C=C1 JUPQTSLXMOCDHR-UHFFFAOYSA-N 0.000 claims description 12
- 239000012071 phase Substances 0.000 claims description 12
- 229920002530 polyetherether ketone Polymers 0.000 claims description 12
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 9
- 235000019253 formic acid Nutrition 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000007689 inspection Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 5
- 239000004677 Nylon Substances 0.000 claims description 4
- 238000010612 desalination reaction Methods 0.000 claims description 4
- 229920001778 nylon Polymers 0.000 claims description 4
- 239000007790 solid phase Substances 0.000 claims description 4
- 239000004568 cement Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 238000005349 anion exchange Methods 0.000 claims description 2
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- 238000012799 strong cation exchange Methods 0.000 claims description 2
- 230000010148 water-pollination Effects 0.000 claims description 2
- 238000003780 insertion Methods 0.000 claims 1
- 230000037431 insertion Effects 0.000 claims 1
- 210000004369 blood Anatomy 0.000 abstract description 5
- 239000008280 blood Substances 0.000 abstract description 5
- 238000003745 diagnosis Methods 0.000 abstract description 5
- 238000012216 screening Methods 0.000 abstract description 4
- 210000002700 urine Anatomy 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 210000004243 sweat Anatomy 0.000 abstract description 2
- 238000000132 electrospray ionisation Methods 0.000 abstract 2
- 208000028399 Critical Illness Diseases 0.000 abstract 1
- 238000007787 electrohydrodynamic spraying Methods 0.000 abstract 1
- 210000003296 saliva Anatomy 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 60
- 206010033128 Ovarian cancer Diseases 0.000 description 9
- 206010061535 Ovarian neoplasm Diseases 0.000 description 9
- 201000010099 disease Diseases 0.000 description 8
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 8
- 210000002381 plasma Anatomy 0.000 description 8
- 206010028980 Neoplasm Diseases 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 201000011510 cancer Diseases 0.000 description 6
- 238000011282 treatment Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 238000000889 atomisation Methods 0.000 description 2
- 238000001574 biopsy Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
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- 238000004140 cleaning Methods 0.000 description 1
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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
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
Abstract
The invention relates to an online-internal-extraction electrospray-ionization mass-spectroscopy detection device for rapidly analyzing body fluid samples of a human body, and belongs to the technical field of chemical analysis. The detection device consists of an eluate introduction device, an in-situ sample enriching extractor, a sample introduction device, an electrospray ionization source and a mass spectrograph, wherein the eluate introduction device is used for introducing a flowing phase for sample eluting, the in-situ sample enriching extractor is used for carrying out sample loading and online extracting and enriching, the sample introduction device is used for introducing eluted samples into the electrospray ionization source for electrospraying, and the mass spectrograph is used for carrying out detection and analysis on online samples, so as to obtain mass-spectroscopy molecular fingerprint spectrogram information on the samples. According to the detection device, the detected human body fluid samples may be human body fluids such as blood, urine, sweat and saliva, do not need sample pretreatment, and are subjected to in-situ sample loading. The device provided by the invention is simple in structure and low-cost, the practicability is high, the detection time and economic cost are reduced greatly, and a technical support is provided for the rapid diagnosis and screening of critical illnesses.
Description
Technical field
The invention belongs to chemical analysis technology field, and in particular to a kind of online inside of quick analysis human body fluid sample
Extraction electrospray ionization mass spectrometry detection means.
Background technology
At present, in the face of substantial amounts of complicated substrate biological sample, traditional sample detection process operation is numerous and diverse, sample pretreatment
Time-consuming for process, easily causes sample loss, is unfavorable for the on-line monitoring of sample, seriously constrains the rapid screening of sample.Especially
It is at aspects such as the early detection for mankind's major disease (such as tumour, cancer), early diagnosis and early treatments, quickly
Sample sifter is checked the diagnosis and treatment in disease and is had great significance.At present, during body fluid (such as blood or urine) is as medical diagnosis on disease
The important sample of class, the fast development of " biopsy " technology of human body fluid, the analyzing detecting method to its online fast high-sensitive degree
There is high requirement, thus it is very urgent for the quick online examination technology of development and improvement major disease.
The direct mass-spectrometric technique of normal pressure is each due to as analysis and detection technology fast-developing in recent years, being widely used in
Plant ambit.Online inner extraction electrospray ionization mass spectrometry technology, in atmospheric conditions, without the need for sample pretreatment, can be right
Human body fluid sample is directly analyzed, and sets up the people of online pre-separation, quick, n.s loss, high sensitivity and high precision
Body humoral sample Direct Inspection Technology, is beneficial to promote the development of major disease early screening and diagnosis and treatment detection technique.
Bibliography:
[1]Nicholson J.K.,Wilson I.D.,Understanding‘Global’Systems Biology:
Metabonomics and the Continuum of Metabolism,Nat.Rev.Drug Discov.,2003,2,668-
676.
[2]Robertson D.G.,Metabonomics in Toxicology:A Review,Toxicol.Sci.,
2005,85,809-822.
The content of the invention
It is an object of the invention to provide a kind of online inner extraction electron spray ionisation matter of quick analysis human body fluid sample
Spectrum detection device.
A kind of online inner extraction electrospray ionization mass spectrometry detection of quick analysis human body fluid sample of the present invention
Device is by eluent introducing device 11, example enrichment extraction equipment 12, sample introduction device 13 in situ, the and of electron spray ionisation source 14
Mass spectrograph 15 is constituted.The eluent introducing device 11 introduces the mobile phase for sample elution;The example enrichment extraction in situ
Device 12 is taken for sample loading and on-line extraction enrichment;Sample after wash-out is introduced electron spray by the sample introduction device 13
Ionization source 14 carries out ionization atomization, is used to ionize the on-line checking analysis of atomized sample by mass spectrograph 15, so as to obtain sample
Mass spectroscopy molecular fingerprint chromatogram information.
In the present invention, using micro syringe as eluent introducing device 11.
In the present invention, example enrichment extraction equipment 12 in situ, by the organic filter membrane of the micropore of syringe-type structure and the micro- extraction of solid phase
Filler composition is taken, SPME filler is laid on the organic filter membrane of micropore;The organic filter membrane material of micropore can select polytetrafluoro
The materials such as ethene, organic system nylon, Kynoar, wherein aperture specification may be selected 0.22 μm or 0.45 μm.As shown in Fig. 2
The organic filter membrane of micropore of syringe-type structure includes entrance 21, outlet 22 and SPME filler 23.
The preparation of example enrichment extraction equipment 11 in situ and use step:
1) weigh SPME 1~5mg of filler, SPME filler include anti-phase SPME filler filler,
Hydrophily SPME filler filler, strong cation exchange material or strong anion exchange filler etc.;
2) by step 1) described in SPME filler disperse in methyl alcohol, prepare concentration be 1~5mg/mL suspension
Solution, ultrasound simultaneously shakes up, it is ensured that the dispersion of uniform filling in methyl alcohol, obtains homogenate solution;
3) by the entrance 21 of eluent introducing device by step 2) obtained in homogenate solution be injected into syringe-type structure
In the organic filter membrane of micropore, SPME filler is laid on the organic filter membrane of micropore, thickness be 1~2mm, example enrichment in situ
Extraction equipment is prepared and completed;
4) again by the entrance 21 of eluent introducing device by 1~5mL containing 95% volumes of acetonitrile, 4.9% volume of water and
The mixed solution of 0.1% volume formic acid is injected into step 3) process after the surface tiling that obtains have the micropore of SPME filler
Cleaned on organic filter membrane;
5) human body fluid sample Jing entrances 21 being directly added dropwise in step 4) the surface tiling cleaned has SPME
On the organic filter membrane of micropore of filler;
6) by the entrance 21 of eluent introducing device by 1~5mL containing 5% volumes of acetonitrile, 94.9% volume of water and
The mixed solution of 0.1% volume formic acid is injected into step 5) dropwise addition that the obtains surface tiling that has human body humoral sample has solid phase micro-
Desalination is carried out on the organic filter membrane of micropore of extraction stuffing;
7) by the entrance 21 of eluent introducing device by 1~5mL containing 35% volumes of acetonitrile, 64.9% volume of water and
The mixed solution of 0.1% volume formic acid is eluted to the human body fluid sample after desalination.
In the present invention, example enrichment extraction equipment in situ with low cost, prepares simple and quick, easily in high volume uses
The characteristics of.
In the present invention, sample introduction device 13, by tack injection needle 31, sleeve pipe 32, first-hand twist-on 33, bilateral
34th, second-hand's twist-on 35, pipeline 36 and the 3rd hand twist-on 37 are constituted.Tack injection needle 31 can select stainless steel tack
The tack injection needle of injection needle, or plastic cement seat bayonet socket, as shown in Figure 3.Before the plug-in-sleeve 32 of tack injection needle 31
The front end of first-hand twist-on 33 is inserted in end, the rear end of sleeve pipe 32, and the rear end of first-hand twist-on 33 is by screw thread and bilateral 34
Front end connection, the rear end of bilateral 34 is connected by screw thread with the front end of second-hand's twist-on 35, and the front end of pipeline 36 inserts the
Insert the front end of the 3rd hand twist-on 37, the rear end of the 3rd hand twist-on 37 in the rear end of second-hand twist-on 35, the rear end of pipeline 36
It is connected with electron spray ionisation source 14 by screw thread;Wherein, the internal diameter of tack injection needle 31 be 0.4mm, external diameter be 0.7mm;Set
Pipe 32 is that the PEEK that external diameter is 1/16 inch, internal diameter is 1mm is managed;It is 50~250 μm for 1/16 inch, internal diameter that pipeline 36 is external diameter
PEEK pipe;The internal diameter of hand twist-on 33,35,37 is 1/16 inch, the PEEK hand twist-ons with 10-32unf standard externals
Head;Bilateral 34 is the PEEK bilaterals with 10-32unf standard females or stainless steel bilateral, for introducing the sample after eluting.
In the present invention, electron spray ionisation source makes the ionization atomization of the sample liquids after wash-out, forms charged ion spraying.
In the present invention, the charged ion spraying of the human body fluid sample that mass spectrograph is produced to electron spray ionisation source is examined
Survey, obtain the mass spectroscopy molecular fingerprint chromatogram information of sample, obtained data are carried out into chemometrics application.
It is characteristic of the invention that:The human body fluid sample of present invention detection can be blood, urine, sweat, saliva et al.
Body body fluid, without the need for sample pre-treatments, loading in situ is cheap using simple, using quick, can fast direct online
Connect analysis human body fluid sample, it is to avoid sample is lost, easy to operate, system is steadily and surely coupled with mass spectrograph, the body to cancer patient
Liquid sample carries out on-line quick detection, and the discovery and examination for mankind's major disease provides technical method.
Description of the drawings
Fig. 1 is apparatus structure schematic diagram of the present invention;
Fig. 2 is example enrichment extraction equipment structural representation in situ of the present invention;
Fig. 3 is sample introduction device structural representation of the present invention;
Fig. 4 is the principal component scores figure of device detection normal person of the present invention and plasma of ovarian cancer patients sample.
Specific embodiment
Embodiment 1
It is further details of to the present invention with reference to the accompanying drawings and detailed description to make the present invention realize above-mentioned purpose
Explanation.
As shown in figure 1, a kind of online inner extraction electron spray electricity of quick analysis human body fluid sample of the present invention
From Mass Spectrometer Method device, by eluent introducing device 11, example enrichment extraction equipment 12, sample introduction device 13, EFI in situ
Mist ionization source 14 and mass spectrograph 15 are constituted.Normal person and human ovarian cancer patients' blood plasma sample can be entered using device of the present invention
The online quick Mass Spectrometer Method of row.
Sample introduction device 13 is twisted by tack injection needle 31, sleeve pipe 32, first-hand twist-on 33, bilateral 34, second-hand
Joint 35, pipeline 36, the 3rd hand twist-on 37.Tack injection needle 31 can from stainless steel tack injection needle, or
The tack injection needle of plastic cement seat bayonet socket, as shown in Figure 3.The front end of the plug-in-sleeve 32 of tack injection needle 31, the rear end of sleeve pipe 32
The front end of first-hand twist-on 33 is inserted, the rear end of first-hand twist-on 33 is connected by screw thread with the front end of bilateral 34, bilateral
34 rear end is connected by screw thread with the front end of second-hand's twist-on 35, and the front end of pipeline 36 is inserted after second-hand's twist-on 35
The front end of the 3rd hand twist-on 37 is inserted in end, the rear end of pipeline 36, and the rear end of the 3rd hand twist-on 37 is by screw thread and electron spray
Ionization source 14 connects
Tack injection needle 31 adopts internal diameter 0.4mm, the stainless steel tack injection needle of external diameter 0.7mm;Sleeve pipe 32 is outer
The PEEK that footpath is 1/16 inch, internal diameter is 1mm is managed;Hand twist-on 33,35,37 is internal diameter for 1/16 inch (i.e. 1.58mm), outer
Footpath is 16.6mm, the PEEK hand twist-on heads with 10-32unf standard externals;Bilateral 34 is with spiral shell in 10-32unf standards
The PEEK pipes of line, for introducing the sample after eluting;Pipeline 36 is the PEEK pipes that external diameter is 1/16 inch, internal diameter is 100 μm.
Using the Dispoable medical syringe of 1mL as eluent introducing device 11.Wherein, example enrichment extraction dress in situ
12 are put, using the organic filter membrane of micropore of 0.22 μm of the organic system nylon syringe structure in aperture, by anti-phase SPME filler
(particle diameter is 40 μm, biological purchased from Jinan Beaune) is laid on the organic filter membrane of micropore, and electron spray ionisation source 14 is (purchased from the silent winged generation of match
That company) it is installed on the rear end of the 3rd hand twist-on 37.
The preparation of example enrichment extraction equipment in situ and use step:
1) anti-phase SPME filler 3mg is weighed.
2) by step 1) anti-phase SPME filler is dispersed in 1mL methyl alcohol, and preparation concentration is the anti-phase solid phases of 3mg/mL
Micro-extraction filler aaerosol solution, ultrasound simultaneously shakes up, it is ensured that the dispersion of uniform filling in methyl alcohol, obtains homogenate solution.
3) by the entrance 21 of eluent introducing device by step 2) obtained in homogenate solution be injected into 0.22 μm of aperture and have
In the organic filter membrane of micropore of machine system nylon syringe structure, anti-phase SPME filler is laid on the organic filter membrane of micropore, thick
Spend for 1mm, example enrichment extraction equipment in situ is prepared and completed;
4) by the entrance 21 of eluent introducing device by 1mL containing 95% volumes of acetonitrile, 4.9% volume of water and 0.1%
The mixed solution of volume formic acid is injected into step 3) the tiling micropore that has anti-phase SPME filler in the surface that obtains has machine filter
Cleaned on film;
5) without the need for sample pretreatment, 1 μ L human plasma samples (cancer patient or human normal plasma's sample), Jing entrances 21 are taken
Directly it is added dropwise in step 4) the surface tiling after cleaning has on the organic filter membrane of micropore of anti-phase SPME filler;
6) by the entrance 21 of eluent introducing device by 1mL containing 5% volumes of acetonitrile, 94.9% volume of water and 0.1%
The mixed solution of volume formic acid is injected into step 5) process after the dropwise addition that obtains have human body plasma sample (cancer patient or normal person
Plasma sample) surface tiling have on the organic filter membrane of micropore of anti-phase SPME filler, 1min is quickly taken off to sample
Salt treatment.
7) step 6) process after, by the entrance 21 of eluent introducing device by 1mL with containing 35% volumes of acetonitrile, 64.9%
The mixed solution of volume of water and 0.1% volume formic acid is eluted to desalted sample.
8) by Jing step 7) wash-out after sample, by sample introduction device 13 by after wash-out sample introduce electron spray electricity
Electron spray is carried out from source 14, sample is detected by matching the Orbitrap Fusion mass spectrographs 15 of Mo Feishier companies.
9) by 12 cancer patients of Mass Spectrometer Method and the blood sample of 7 normal persons, the mass spectroscopy molecular for obtaining sample refers to
Line spectrogram information, by the principal component analytical method in chemometrics method, establishes a kind of quick judgement cancer patient's
Mass spectrometric methods, Fig. 4 is the principal component scores figure of normal person and plasma of ovarian cancer patients sample, can effectively distinguish normal person with
Human ovarian cancer patients.In the diagram, transverse and longitudinal coordinate PC1 and PC2 represent the variable information of principal component.Wherein, one in figureRepresent one
The data point of example ovarian cancer patients sample a, ■ represents the data point of a normal human sample.The scores table of principal component
Bright chemometrics method realizes preferably differentiation to two class samples, and the blood sample of the normal person of ovarian cancer patients sum is divided equally
Cloth well can distinguish the normal person of ovarian cancer patients sum in respective region and without overlapping.
The present invention realizes the online quick detection of human body fluid sample in-situ without the need for sample pretreatment, online in situ fast
It is fast that normal person and human ovarian cancer patients' blood plasma sample are detected, the normal person of ovarian cancer patients sum can be efficiently differentiated, can
The quick diagnosis and rapid screening for being applied to major disease are distinguished, and apparatus structure is simple, with low cost, practical, saves significantly
About detection time and financial cost, have widened application of the analytical technique of mass spectrum in major disease body fluid biopsy field.
Claims (6)
1. a kind of online inner extraction electrospray ionization mass spectrometry detection means of quick analysis human body fluid sample, its feature exists
In:By eluent introducing device (11), example enrichment extraction equipment (12) in situ, sample introduction device (13), electron spray ionisation
Source (14) and mass spectrograph (15) are constituted;The eluent introducing device (11) introduces the mobile phase for sample elution, the original
Position example enrichment extraction equipment (12) is enriched with for sample loading and on-line extraction, after the sample introduction device (13) will elute
Sample introduce electron spray ionisation source (14) and carry out electron spray, mass spectrograph (15) for on-line sample detection and analysis, so as to obtain
Obtain the mass spectroscopy molecular fingerprint chromatogram information of sample.
2. the online inner extraction electrospray ionization mass spectrometry inspection of a kind of quick analysis human body fluid sample as claimed in claim 1
Survey device, it is characterised in that:Example enrichment extraction equipment (12) in situ is micro- by the organic filter membrane of micropore and solid phase of syringe-type structure
Extraction stuffing (23) is constituted, and SPME filler is laid on the organic filter membrane of micropore;The material of the organic filter membrane of micropore is poly- four
PVF, organic system nylon or Kynoar, aperture specification is 0.22 μm or 0.45 μm;The micropore of syringe-type structure has machine filter
Film includes entrance (21) and outlet (22).
3. the online inner extraction electrospray ionization mass spectrometry inspection of a kind of quick analysis human body fluid sample as claimed in claim 2
Survey device, it is characterised in that:The preparation of example enrichment extraction equipment (11) in situ and as follows using step,
1) SPME 1~5mg of filler is weighed, SPME filler is anti-phase SPME filler filler, hydrophily
SPME filler filler, strong cation exchange material or strong anion exchange filler;
2) by step 1) described in SPME filler disperse in methyl alcohol, prepare concentration be 1~5mg/mL aaerosol solution,
Ultrasound simultaneously shakes up, it is ensured that the dispersion of uniform filling in methyl alcohol, obtains homogenate solution;
3) by the entrance (21) of eluent introducing device by step 2) obtained in homogenate solution be injected into the micro- of syringe-type structure
In the organic filter membrane in hole, SPME filler is set to be laid on the organic filter membrane of micropore, thickness is 1~2mm, example enrichment extraction in situ
Take device preparation to complete;
4) again by the entrance (21) of eluent introducing device by 1~5mL containing 95% volumes of acetonitrile, 4.9% volume of water and
The mixed solution of 0.1% volume formic acid is injected into step 3) process after the surface tiling that obtains have the micropore of SPME filler
Cleaned on organic filter membrane;
5) human body fluid sample Jing entrances (21) being directly added dropwise in step 4) the surface tiling cleaned has SPME to fill out
On the organic filter membrane of micropore of material;
6) by the entrance (21) of eluent introducing device by 1~5mL containing 5% volumes of acetonitrile, 94.9% volume of water and 0.1%
The mixed solution of volume formic acid is injected into step 5) dropwise addition that the obtains surface tiling that has human body humoral sample has SPME
Desalination is carried out on the organic filter membrane of micropore of filler;
7) by the entrance (21) of eluent introducing device by 1~5mL containing 35% volumes of acetonitrile, 64.9% volume of water and
The mixed solution of 0.1% volume formic acid is eluted to the human body fluid sample after desalination.
4. the online inner extraction electrospray ionization mass spectrometry inspection of a kind of quick analysis human body fluid sample as claimed in claim 1
Survey device, it is characterised in that:Sample introduction device (13) is by tack injection needle (31), sleeve pipe (32), first-hand twist-on head
(33), bilateral (34), second-hand's twist-on head (35), pipeline (36), the 3rd hand twist-on head (37) composition;Tack injection needle (31)
For stainless steel tack injection needle or plastic cement seat bayonet socket tack injection needle, before tack injection needle (31) plug-in-sleeve (32)
The front end of first-hand twist-on head (33) is inserted in end, the rear end of sleeve pipe (32), the rear end of first-hand twist-on head (33) by screw thread with
The front end connection of bilateral (34), the rear end of bilateral (34) is connected by screw thread with the front end of second-hand's twist-on head (35), pipeline
(36) insert before the 3rd hand twist-on head (37) rear end of front end insertion second-hand's twist-on head (35), the rear end of pipeline (36)
End, the rear end of the 3rd hand twist-on head (37) is connected by screw thread with electron spray ionisation source (14).
5. the online inner extraction electrospray ionization mass spectrometry inspection of a kind of quick analysis human body fluid sample as claimed in claim 4
Survey device, it is characterised in that:The internal diameter of tack injection needle (31) is 0.4mm, external diameter is 0.7mm;Sleeve pipe (32) is that external diameter is
1/16 inch, the PEEK that internal diameter is 1mm pipes;Pipeline (36) is the PEEK pipes that external diameter is 1/16 inch, internal diameter is 50~250 μm;
The internal diameter of hand twist-on head (33,35,37) is 1/16 inch, the PEEK hand twist-on heads with 10-32unf standard externals;Bilateral
(34) it is the PEEK bilaterals with 10-32unf standard females or stainless steel bilateral.
6. the online inner extraction electrospray ionization mass spectrometry inspection of a kind of quick analysis human body fluid sample as claimed in claim 1
Survey device, it is characterised in that:Using micro syringe as eluent introducing device (11).
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN201611215422.6A CN106645374A (en) | 2016-12-26 | 2016-12-26 | Online-internal-extraction electrospray-ionization mass-spectroscopy detection device for rapidly analyzing body fluid samples of human body |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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CN201611215422.6A CN106645374A (en) | 2016-12-26 | 2016-12-26 | Online-internal-extraction electrospray-ionization mass-spectroscopy detection device for rapidly analyzing body fluid samples of human body |
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CN106645374A true CN106645374A (en) | 2017-05-10 |
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