CN109459484A - A kind of mass spectrometric analysis method of the small molecule sample based on nano material - Google Patents
A kind of mass spectrometric analysis method of the small molecule sample based on nano material Download PDFInfo
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- CN109459484A CN109459484A CN201710794691.0A CN201710794691A CN109459484A CN 109459484 A CN109459484 A CN 109459484A CN 201710794691 A CN201710794691 A CN 201710794691A CN 109459484 A CN109459484 A CN 109459484A
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- small molecule
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- 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
- G01N27/64—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 using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
Abstract
The present invention provides a kind of mass spectrometric analysis method of small molecule sample based on nano material, this method are as follows: water-soluble gold nanoclusters material is dissolved into formation nano material homogeneous phase solution in deionized water, the homogeneous phase solution is covered on the mottling of small molecule sample, ionization and mass spectral analysis finally are carried out to small molecule sample using Matrix-assisted laser desorption ionization.This method is based on ionization of the water-soluble gold nanoclusters material to small molecule sample with UV Absorption characteristic.The method high sensitivity, ionization processing and mass spectral analysis suitable for small molecule sample.
Description
Technical field
The invention belongs to the mass spectral analysis fields of small molecule sample, more particularly to a kind of small molecule sample based on nano material
The mass spectrometric analysis method of product.
Background technique
Substance assistant laser desorpted ionization (MALDI) technology is to absorb to swash using the organic substrate with UV Absorption
Light energy has the characteristics that label-free, high-throughput and automation to realize the analytical technology of the laser desorption ionisation of determinand, real
The analysis to non-volatile sample is showed.Simultaneously compared with other mass spectrums, MALDI salt tolerant with higher, resistance to buffer and its
The advantages of its involatile constituent.Since sample molecules most of in MALDI analysis are all to be dissociated into single charged molecular ions,
So obtained mass spectrogram is fairly simple, be conducive to spectrum elucidation.
There are three classes using more matrix at present, is derived with the cinnamic acid that alpha-cyano -4- hydroxyl-cinnamic acid (CHCA) is representative
Object, with 2,5- dihydroxy-benzoic acid (DHB) be representative aromatic carboxylic acid derivatives and aniline series.Wherein CHCA non-selectivity
Peptide fragment and protein are ionized, strong ion signal is generated, is suitble to the analysis of peptide fragment and glycopeptide.DHB is most normal matrix, generation
Matrix peak and matrix association peak are few, are widely used in the analysis of all kinds of macromolecular compounds.Oligonucleotide
Measurement uses 3- hydroxy-picolinic acid usually under anionic textiles mode.
MALDI has many advantages in the analysis of macromolecular compound, but it has not been widely available on small molecule
Close the analysis of object.Its main reason is matrix ion signal interference.However, MALDI-MS has multicomponent while analyzing,
High sensitivity analyzes fireballing feature, so that researcher very payes attention to MALDI small molecule analysis.In order to overcome MALDI
Matrix interference problem, people improve MALDI technology, and by using new matrix, new sample preparation method and new material can
Matrix interference is reduced to bottom line.
Summary of the invention
The mass spectrometric analysis method of it is an object of the invention to a kind of small molecule sample based on nano material.
To achieve the above object, the present invention is at Matrix-assisted laser desorption ionization (MALDI-TOF MS)
On the basis of handling small molecule sample, using the gold nanoclusters material with water-soluble, high UV Absorption characteristic, realize
The ionization and mass spectral analysis of small molecule sample.
A kind of mass spectrometric analysis method of the small molecule sample based on nano material, this method are as follows: by water-soluble gold nano
Clustered materials are dissolved into formation nano material homogeneous phase solution in deionized water, which is covered on to the mottling of small molecule sample
On, ion finally is carried out to small molecule sample using Matrix-assisted laser desorption ionization (MALDI-TOF MS)
Change and mass spectral analysis；
The water-soluble gold nanoclusters material is a kind of gold nanoclusters material synthesized using cysteine as blocking group
Material, or with the water-soluble metal cluster materials of others,
The water-soluble metal cluster material of others is that glutathione and polyethylene glycol (PEG) are used as blocking group
Gold nanoclusters material；
The small molecule sample is glucose, lactose, galactolipin, oleic acid and linoleic acid equimolecular quantity less than 1000
Substance.
Detailed process is as follows for this method:
1) aqueous solution for configuring the gold nanoclusters material of 1.0-5.0mg/mL is matrix liquid；
2) ultrasound 1-2min under above-mentioned system room temperature is formed it into uniform solution system；
3) the small molecule sample solution for configuring 0.5-5.0mg/mL is sample liquid
4) sample liquid is added drop-wise to the metallic target on piece of MALDI-TOF MS in a manner of being added dropwise, it is dry to solution；
5) matrix liquid is added drop-wise in a manner of being added dropwise on the mottling for the metallic target on piece that step 4) obtains, make matrix liquid with
The volume ratio of sample is 0.3-3:1, is made dry to solution；
6) dry mottling is subjected to MALDI-TOF MS detection.
Advantages of the present invention has the beneficial effect that the mass spectrometric analysis method of the small molecule sample based on nano material significantly
The detection difficulty of simplified small molecule sample improves the detection sensitivity of the MALDI-TOF MS of small molecule sample.The analysis
The enhancing processing of the exclusion and small molecule sample mass signal interfered mass spectra peak caused by matrix may be implemented in method.
Detailed description of the invention
Fig. 1 is the mass spectrometric analysis method schematic diagram of the small molecule sample based on nano material.
Fig. 2 is that the mass spectrometric analysis method of the small molecule sample based on nano material is used to analyze the MALDI-TOF of glucose
MS figure.(A) embodiment 1, (B) embodiment 2, (C) embodiment 3, (D) embodiment 4.
Fig. 3 is the mass spectrometric analysis method of the small molecule sample based on nano material for analyzing mixing sample (embodiment 5)
MALDI-TOF MS figure.
Specific embodiment
The maximum of the method for the present invention is characterized in that: special using the water solubility and strong UV Absorption of gold nanoclusters material
Property, the ionization rate and Ionization Efficiency of small molecule sample are improved, the mass spectral analysis of small molecule sample is realized in the short time.
Specific embodiment is introduced below by example.
Embodiment 1
The mass spectrometric analysis method of small molecule sample based on nano material:
1, the aqueous solution for configuring the gold nanoclusters material of 1.0mg/mL is matrix liquid；
2, ultrasound 1-2min under above-mentioned system room temperature is formed it into uniform solution system；
3, the glucose sample solution of 0.5mg/mL is configured, is sample liquid
4, sample liquid is added drop-wise to the metallic target on piece of MALDI-TOF MS in a manner of being added dropwise, it is dry to solution；
5, matrix liquid is added drop-wise in a manner of being added dropwise on the mottling for the metallic target on piece that step 4) obtains, make matrix liquid with
The volume ratio of sample is 0.3:1, is made dry to solution；
6, dry mottling is subjected to MALDI-TOF MS detection.
All MALDI-TOF mass spectral analyses are all completed on 5800 time of-flight mass spectrometer of AB Sciex.
Analyze result: by Fig. 2A as it can be seen that glucose can be detected by MALDI-TOF MS well, wherein glucose
(glucose): m/z=202.9 [M+Na]+.These results suggest that the mass spectrometric analysis method of the small molecule sample can be used well
In the Mass Spectrometer Method of small molecule sample.
Embodiment 2
The mass spectrometric analysis method of small molecule sample based on nano material:
1, the aqueous solution for configuring the gold nanoclusters material of 2.5mg/mL is matrix liquid；
2, ultrasound 1-2min under above-mentioned system room temperature is formed it into uniform solution system；
3, the glucose sample solution of 0.5mg/mL is configured, is sample liquid
4, sample liquid is added drop-wise to the metallic target on piece of MALDI-TOF MS in a manner of being added dropwise, it is dry to solution；
5, matrix liquid is added drop-wise in a manner of being added dropwise on the mottling for the metallic target on piece that step 4) obtains, make matrix liquid with
The volume ratio of sample is 1.5:1, is made dry to solution；
6, dry mottling is subjected to MALDI-TOF MS detection.
All MALDI-TOF mass spectral analyses are all completed on 5800 time of-flight mass spectrometer of AB Sciex.
Analyze result: by Fig. 2 B as it can be seen that glucose can be detected by MALDI-TOF MS well, wherein glucose
(glucose): m/z=202.9 [M+Na]+.These results suggest that the mass spectrometric analysis method of the small molecule sample can be used well
In the Mass Spectrometer Method of small molecule sample.
Embodiment 3
The mass spectrometric analysis method of small molecule sample based on nano material:
1, the aqueous solution for configuring the gold nanoclusters material of 5.0mg/mL is matrix liquid；
2, ultrasound 1-2min under above-mentioned system room temperature is formed it into uniform solution system；
3, the glucose sample solution of 5.0mg/mL is configured, is sample liquid
4, sample liquid is added drop-wise to the metallic target on piece of MALDI-TOF MS in a manner of being added dropwise, it is dry to solution；
5, matrix liquid is added drop-wise in a manner of being added dropwise on the mottling for the metallic target on piece that step 4) obtains, make matrix liquid with
The volume ratio of sample is 3:1, is made dry to solution；
6, dry mottling is subjected to MALDI-TOF MS detection.
All MALDI-TOF mass spectral analyses are all completed on 5800 time of-flight mass spectrometer of AB Sciex.
Analyze result: by Fig. 2 C as it can be seen that glucose can be detected by MALDI-TOF MS well, wherein glucose
(glucose): m/z=202.9 [M+Na]+.These results suggest that the mass spectrometric analysis method of the small molecule sample can be used well
In the Mass Spectrometer Method of small molecule sample.
Embodiment 4
The mass spectrometric analysis method of small molecule sample based on nano material:
1, the aqueous solution for configuring the gold nanoclusters material of 2.5mg/mL is matrix liquid；
2, ultrasound 1-2min under above-mentioned system room temperature is formed it into uniform solution system；
3, the glucose sample solution of 3.0mg/mL is configured, is sample liquid
4, sample liquid is added drop-wise to the metallic target on piece of MALDI-TOF MS in a manner of being added dropwise, it is dry to solution；
5, matrix liquid is added drop-wise in a manner of being added dropwise on the mottling for the metallic target on piece that step 4) obtains, make matrix liquid with
The volume ratio of sample is 1.5:1, is made dry to solution；
6, dry mottling is subjected to MALDI-TOF MS detection.
All MALDI-TOF mass spectral analyses are all completed on 5800 time of-flight mass spectrometer of AB Sciex.
Analyze result: by Fig. 2 D as it can be seen that glucose can be detected by MALDI-TOF MS well, wherein glucose
(glucose): m/z=202.9 [M+Na]+.These results suggest that the mass spectrometric analysis method of the small molecule sample can be used well
In the Mass Spectrometer Method of small molecule sample.
Embodiment 5
The mass spectrometric analysis method of small molecule sample based on nano material:
1, the aqueous solution for configuring the gold nanoclusters material of 1.0mg/mL is matrix liquid；
2, ultrasound 1-2min under above-mentioned system room temperature is formed it into uniform solution system；
3, the solution for configuring the mixing sample of respective concentration 1.0mg/mL, includes glucose (glucose), phenylalanine-
Alanine (FA), atropine (atropine), lactose (lactose), China tree sterol (azedarachol), 3-O-
Tigloylswietenolide, three oleoyl glycerides (triolein) are sample liquid
4, sample liquid is added drop-wise to the metallic target on piece of MALDI-TOF MS in a manner of being added dropwise, it is dry to solution；
5, matrix liquid is added drop-wise in a manner of being added dropwise on the mottling for the metallic target on piece that step 4) obtains, make matrix liquid with
The volume ratio of sample is 0.3:1, is made dry to solution；
6, dry mottling is subjected to MALDI-TOF MS detection.
All MALDI-TOF mass spectral analyses are all completed on 5800 time of-flight mass spectrometer of AB Sciex.
Analyze result: as seen from Figure 3, wherein small-molecule substance can be detected by MALDI-TOF MS well, grape
Sugar (glucose): m/z=202.9 [M+Na]+；Phenylalanine-alanine (FA): m/z=259.0 [M+Na]+；Atropine
(atropine): m/z=311.9 [M+Na]+；Lactose (lactose): m/z=364.9 [M+Na]+；China tree sterol
(azedarachol): m/z=443.0 [M+Na]+；3-O-tigloylswietenolide:m/z=591.0 [M+Na]+；Three oil
Acyl glyceride (triolein): m/z=907.8 [M+Na]+.These results suggest that the mass spectrometric analysis method energy of the small molecule sample
Perform well in the Mass Spectrometer Method of small molecule sample.
Claims (3)
1. a kind of mass spectrometric analysis method of the small molecule sample based on nano material, it is characterised in that this method are as follows: will be water-soluble
Gold nanoclusters material be dissolved into deionized water formation nano material homogeneous phase solution, which is covered on small molecule sample
On the mottling of product, ionization and matter finally are carried out to small molecule sample using Matrix-assisted laser desorption ionization
Spectrum analysis；
The water-soluble gold nanoclusters material is a kind of gold nanoclusters material synthesized using cysteine as blocking group, or
Other water-soluble metal cluster materials,
The small molecule sample is the object of glucose, lactose, galactolipin, oleic acid or linoleic acid and other molecular weight less than 1000
Matter.
2. the mass spectrometric analysis method of the small molecule sample according to claim 1 based on nano material, it is characterised in that institute
Stating other water-soluble metal cluster materials is the gold nanoclusters material of glutathione and polyethylene glycol as blocking group.
3. the mass spectrometric analysis method of the small molecule sample according to claim 1 based on nano material, it is characterised in that should
Detailed process is as follows for method:
1) aqueous solution for configuring the gold nanoclusters material of 1.0-5.0mg/mL is matrix liquid；
2) ultrasound 1-2min under above-mentioned system room temperature is formed it into uniform solution system；
3) the small molecule sample solution for configuring 0.5-5.0mg/mL is sample liquid；
4) sample liquid is added drop-wise to the metallic target on piece of MALDI-TOF MS in a manner of being added dropwise, it is dry to solution；
5) matrix liquid is added drop-wise on the mottling for the metallic target on piece that step 4) obtains in a manner of being added dropwise, makes matrix liquid and sample
Volume ratio be 0.3-3:1, make dry to solution；
6) dry mottling is subjected to MALDI-TOF MS detection.
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| CN110174459A (en) * | 2019-06-14 | 2019-08-27 | 广西师范大学 | Application of the golden cluster in Matrix-assisted laser desorption ionization detection |
| CN111426743A (en) * | 2020-04-21 | 2020-07-17 | 四川大学 | Application of silver nanosphere material in MA L DI-TOF MS (Mass Spectrometry) detection of small molecule metabolites |
| CN111426741A (en) * | 2020-04-21 | 2020-07-17 | 四川大学 | Method for performing liquid biopsy based on nano material assisted MA L DI-TOF MS |
| CN117110415A (en) * | 2023-10-16 | 2023-11-24 | 成都泰莱医学检验实验室有限公司 | Method for performing time-of-flight mass spectrometry detection by using cobalt carbide nanomaterial matrix |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110174459A (en) * | 2019-06-14 | 2019-08-27 | 广西师范大学 | Application of the golden cluster in Matrix-assisted laser desorption ionization detection |
| CN111426743A (en) * | 2020-04-21 | 2020-07-17 | 四川大学 | Application of silver nanosphere material in MA L DI-TOF MS (Mass Spectrometry) detection of small molecule metabolites |
| CN111426741A (en) * | 2020-04-21 | 2020-07-17 | 四川大学 | Method for performing liquid biopsy based on nano material assisted MA L DI-TOF MS |
| CN117110415A (en) * | 2023-10-16 | 2023-11-24 | 成都泰莱医学检验实验室有限公司 | Method for performing time-of-flight mass spectrometry detection by using cobalt carbide nanomaterial matrix |
| CN117110415B (en) * | 2023-10-16 | 2024-01-26 | 成都泰莱医学检验实验室有限公司 | Method for performing time-of-flight mass spectrometry detection by using cobalt carbide nanomaterial matrix |
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