CN117074509B - Mass spectrum method for detecting carotenoid based on core-shell nanomaterial - Google Patents
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Abstract
The invention discloses a mass spectrometry method for detecting carotenoid based on core-shell nano materials. The SiO 2 @Ag core-shell nanomaterial has a controllable core-shell structure and nanoscale roughness, excellent photo-thermal conversion efficiency and higher desorption/ionization efficiency. The SiO 2 @Ag core-shell nanomaterial can be used for high-sensitivity detection of carotenoid substances, and the preparation method is simple and does not need complex sample pretreatment steps. Compared with the traditional MALDI matrix and the bare noble metal nano material, the SiO 2 @Ag core-shell nano material can obtain a higher spectrogram signal-to-noise ratio and a lower detection limit for carotenoid substances, has wide universality and application prospect, and is suitable for commercial MALDI-MS or LDI-MS instruments in the market.
Description
Technical Field
The invention belongs to the field of analytical chemistry, and particularly relates to an LDI-MS detection method for detecting carotenoid by using SiO 2 @Ag core-shell nanomaterial as a nano matrix in an auxiliary laser desorption/ionization process.
Background
The carotenoid has remarkable antioxidation, anti-tumor and immunity improving effects, and mainly comprises alpha-/beta-/gamma-carotene, lutein, lycopene and the like. However, such materials are difficult to detect by laser desorption/ionization mass spectrometry (LDI-MS) due to inherent structural characteristics, such as long carbon chain, complex structure, high melting point, difficulty in thermal desorption by laser radiation, lack of ionization sites in molecular structure, unstable structure and easy fragmentation after light irradiation. Meanwhile, the low carotenoid content in the actual sample further limits the detection capability of LDI-MS in the actual carotenoid sample.
Since self-emission, matrix assisted laser desorption/ionization mass spectrometry (MALDI-MS) has been widely used in molecular mass spectrometry, particularly in the detection of biological macromolecules, with the advantages of soft ionization characteristics, high sensitivity, high salt tolerance, high throughput, small sample consumption, and the like. However, conventional MALDI methods have a number of drawbacks in the detection of small molecule metabolites, for example, the use of conventional organic matrices (e.g., DHB, HCCA, 9-AA, etc.) often results in severe matrix background peak interference in the low m/z range of the spectrogram, greatly impeding the detection of small molecule metabolites. In addition, the organic matrix is easy to generate a dessert effect in the process of co-crystallization with a substance to be detected, and particles are large, so that the problems of large spectrogram signal fluctuation, poor reproducibility and the like are caused. Although in recent years, inorganic nano materials are gradually developed to solve the defects of the traditional matrix and partially solve the problems of spectral peak background interference and matrix crystallization non-uniformity, in actual analysis, the nano materials and the liquid to be tested still need to be pre-mixed and then spotted, and high-throughput analysis cannot be realized.
For this reason, surface-assisted laser desorption/ionization mass spectrometry (SALDI-MS) based on inorganic nanomaterials is increasingly attracting great attention. Inorganic nanomaterials, including carbon-based, silicon-based, metal oxide-based, metal-organic frameworks and multi-element composites, all exhibit unique analytical capabilities and superior analytical performance in small molecule mass spectrometry thanks to the advantages of specific surface area, good photo-thermal effect, high electrical conductivity and low thermal conductivity. In contrast to MALDI matrices, the nanoscale nature of inorganic nanomaterials, whether spray or sputter, provides a uniform matrix surface. While some advances have been made in nanomaterial-assisted LDI-MS applications, these nanomaterials with a single structure or morphology have not been satisfactory for their analytical performance, particularly when applied to complex biological sample analysis. Because carotenoid mainly comprises C, H elements, has a longer carbon chain and lacks ionization sites, development of a composite nano material is urgently needed, so that the composite nano material can be used for high-efficiency ionization and high-sensitivity mass spectrum detection of substances such as carotenoid and the like, and the application capability of the SALDI-MS technology in actual samples is further expanded.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a core-shell nano material. The material can be used as a nano base material of the SALDI-MS method, can provide specific detection capability for functional metabolites such as carotenoid and the like, and is suitable for analysis of various small molecular metabolites.
It is therefore a first object of the present invention to provide the use of SiO 2 @ Ag core-shell nanomaterials as nanomatrix in laser desorption/ionization mass spectrometry detection of carotenoids.
The core-shell nano material is formed by forming an AgNP core-shell layer on the surface of SiO 2 nano particles through multiple silver mirror reactions, and the SiO 2 @Ag core-shell nano particles are further prepared by optimizing, and the core-shell nano material has nano-scale roughness, excellent photo-thermal conversion efficiency and higher desorption/ionization efficiency. Meanwhile, ag nano particles on the outer layer of the SiO 2 @Ag core-shell nano material can be specifically combined with carotenoid substances containing C=C double bonds, for example, s orbitals of Ag easily form sigma bonds with pi orbitals of olefin substances, d orbitals of Ag easily form pi bonds with pi orbitals of empty reverse bonds of the C=C double bonds of the olefin substances, so that [ M+Ag ] + spectrum peaks are easily formed in a spectrogram, substances such as carotenoid can be specifically detected, and the problems of uneven crystallization, low sensitivity and the like of a traditional organic matrix are effectively avoided.
The SiO 2 @Ag core-shell nanomaterial is prepared by the following steps:
S1, preparing a SiO 2 nano material with a smooth surface and a single dispersion: adding Tetraethoxysilane (TEOS) into the mixed solvent, stirring at room temperature for reaction, washing with ethanol after the reaction is finished, and drying to obtain a monodisperse SiO 2 nano material;
s2, introducing an Ag nano shell layer on the surface of the SiO 2 nano material: dispersing the SiO 2 nano material obtained in the step S1 in ethanol solution, adding freshly prepared [ Ag (NH 3)2]+ silver ammonia solution), carrying out ultrasonic reaction, adding polyvinylpyrrolidone (PVP) ethanol solution, stirring for reaction, repeating silver mirror reaction for a plurality of times, washing the reaction product with ethanol, and drying to obtain the SiO 2 @Ag core-shell nano material.
In step S1, the SiO 2 nanomaterial with a smooth surface and monodispersed surface can be prepared by referring to the existing method.
Preferably, in step S1, the mixed solvent is composed of absolute ethanol, ammonia water and deionized water according to a volume ratio of 53:2.1:2.33; the volume ratio of tetraethoxysilane to the mixed solvent is 3:57.43.
Preferably, in step S1, the reaction time is 6 to 8 hours, more preferably 7 hours.
Preferably, in step S1, the particle size of the monodisperse SiO 2 nanomaterial is 50 to 300nm, more preferably 150nm.
Preferably, in the step S2, the particle concentration of the SiO 2 nano-material is 5-50 mg/mL, more preferably 20mg/mL;
Preferably, in step S2, the concentration of the [ Ag (NH 3)2]+ silver ammonia solution is 50-150 mg/mL, more preferably 100 mg/mL), and the [ Ag (NH 3)2]+ silver ammonia solution needs to be freshly prepared and used.
Preferably, in step S2, the concentration of the PVP ethanol solution is 10-20 mg/mL, more preferably 14.5mg/mL.
Preferably, in step S2, the volume ratio of the ethanol solution, the silver ammonia solution and the PVP ethanol solution is 12:1:28.
Preferably, in step S2, after the PVP ethanol solution is mixed, the reaction temperature is 60-80 ℃, more preferably 70 ℃; the reaction is stirred for 6 to 8 hours, more preferably 7 hours.
Preferably, in step S2, the time of the ultrasonic reaction is 30min.
Preferably, in the step S2, the reaction is carried out at 60-80 ℃ for 6-8 hours under stirring.
Preferably, in step S2, the number of times of the silver mirror reaction is 2 to 5, more preferably 3.
The second object of the invention is to provide a mass spectrometry method for detecting carotenoids based on core-shell nanomaterials, comprising the following steps:
(1) Dispersing SiO 2 @Ag core-shell nano material to obtain a suspension, and using the suspension as a nano matrix for assisting a laser desorption/ionization process;
(2) Preparing a mixture of SiO 2 @Ag core-shell nanomaterial solution and sample solution to be detected in equal proportion on a mass spectrum target plate for the subsequent direct laser desorption/ionization process and mass spectrum detection;
(3) Mass spectrometry detection: and carrying out ablation sampling on the mixed sample residues by adopting laser, and detecting by a mass analyzer to obtain the mass spectrum signal intensity of the carotenoid in the sample.
Preferably, the carotenoids include, but are not limited to, beta-carotene and lutein.
Preferably, in the step (1), the particle concentration of the SiO 2 @Ag core-shell nanomaterial is 0.05-5 mg/mL, and more preferably 1mg/mL.
Preferably, in the step (2), the sample solution to be tested may be a standard solution of carotenoid substance, an extract of fresh fruits and vegetables (such as carrot and corn), a sample of carrot juice sold in the market, and the like.
Preferably, in the step (3), the molecular weight range of the mass spectrum detection method is 100-1000 Da, and the positive ion detection mode is adopted.
Preferably, in the step (3), the light source of the laser is a continuous or pulsed light source, more preferably, the wavelength of the light beam of the continuous light source is 46.9-2940 nm, the diameter of the light beam is 0.01-10 mm, and the average power is not less than 0.1mW; the light beam wavelength of the pulse light source is 46.9-2940 nm, the pulse width is 1 fs-1 ms, the light beam diameter is 0.01-10 mm, the instantaneous pulse energy is 1 nJ-100 mJ, and the pulse frequency is 0.05-100 MHz. More preferably, the light source of the laser is 355nm pulse laser.
Preferably, in the step (3), the mass analyzer may be a quadrupole rod analyzer, an ion trap analyzer, a time-of-flight analyzer, a magnetic field analyzer, a fourier transform analyzer, or the like.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a mass spectrometry method for detecting carotenoid based on core-shell nano materials. The SiO 2 @Ag core-shell nanomaterial has a controllable core-shell structure and nanoscale roughness, excellent photo-thermal conversion efficiency and higher desorption/ionization efficiency. The inherent structural characteristics of carotenoid substances, such as long carbon chain, complex structure and high melting boiling point, make laser radiation difficult to thermally desorb, lack of ionization sites in a molecular structure, unstable structure and easy fragmentation after light irradiation, and the like, make the carotenoid substances very difficult in traditional laser desorption/ionization mass spectrometry (LDI-MS) detection. The Ag nano particles on the outer layer of the SiO 2 @Ag core-shell nano material can be specifically combined with carotenoid substances containing C=C double bonds, for example, s orbitals of Ag easily form sigma bonds with pi orbitals of olefin substances, and d orbitals of Ag easily form pi bonds with empty reverse pi orbitals of C=C double bonds of the olefin substances, so that [ M+Ag ] + spectral peaks are easily formed in a spectrogram. Compared with noble metal nano materials, the core-shell nano materials can obtain higher spectrogram signal-to-noise ratio and lower detection limit for substances such as carotenoid, have wide universality and commercialization prospect, and can be used for commercial MALDI-MS or LDI-MS instruments in the market. The preparation method of the core-shell nano material is simple, and complex pretreatment of tissue samples is not needed.
Drawings
FIG. 1 is a schematic diagram of the synthesis of SiO 2 @Ag core-shell nanomaterial according to example 1 of the present invention, each labeled: 1-SiO 2 nano material, 2-SiO 2 @Ag seed nano material, 3-SiO 2 @Ag core-shell nano material, 4-LDI-MS analysis and 5-mass spectrogram.
FIG. 2 shows electron microscope characterization results of SiO 2 @Ag core-shell nanomaterial and a synthetic precursor material thereof, (A) SiO 2 nanomaterial, (B) SiO 2 @Ag core-shell nanomaterial after 1 silver mirror reaction (SiO 2 @Ag-1), (C) SiO 2 @Ag core-shell nanomaterial after 2 silver mirror reaction (SiO 2 @Ag-2), (D) SiO 2 @Ag core-shell nanomaterial after 3 silver mirror reaction (SiO 2 @Ag-3), and (E) SiO 2 @Ag core-shell nanomaterial after 4 silver mirror reactions (SiO 2 @Ag-4), with a scale of 50nm.
FIG. 3 is a Zeta potential diagram of five nanomaterials, siO 2 nanomaterials, siO 2@Ag-1、SiO2@Ag-2、SiO2@Ag-3、SiO2 @ Ag-4.
FIG. 4 is a mass spectrum of the SiO 2 @ Ag core-shell nanomaterial for beta-carotene and lutein substances in a positive ion mode, wherein the concentration ratio of (A) SiO 2 @ Ag core-shell nanomaterial to analyte is 1:1, (B) SiO 2 @ Ag core-shell nanomaterial to analyte is 10:1, (C) SiO 2 @ Ag core-shell nanomaterial to analyte is 1:10, and the concentration of analyte is 1mg/mL.
FIG. 5 shows the detection limit results of the SiO 2 @ Ag core-shell nanomaterial of the present invention for (A) beta-carotene and (B) lutein respectively, wherein the nanomaterial concentration is 1mg/mL.
FIG. 6 shows the mass spectrum of the SiO 2 @ Ag core-shell nanomaterial used for analyzing carrot juice of a certain brand in the market (A) and the isotope profiles of (B) [ beta-carotene+Ag ] + and (C) [ lutein+Ag ] + in the positive ion mode, wherein the concentration of the nanomaterial is 1mg/mL.
FIG. 7 is a mass spectrum comparison of (A) the SiO 2 @Ag core-shell nanomaterial of the present invention and (B) AgNP material for analysis of a brand of carrot juice in the market under a positive ion mode.
FIG. 8 is a graph of mass spectrum (A) and signal stability (B) of the SiO 2 @Ag core-shell nanomaterial of the invention at 10 different sampling points.
Detailed Description
The invention will be further illustrated with reference to specific examples. It is to be understood that these examples are provided for illustrative purposes only and are not meant to limit the invention. The test methods, which are not specified in the following examples, are generally carried out under conventional conditions, and the instruments involved are commercially available. Percentages and parts are by weight unless otherwise indicated.
Example 1: preparation of SiO 2 @ Ag core-shell nano material
The synthetic schematic diagram and LDI-MS mechanism diagram of the SiO 2 @Ag core-shell nanomaterial disclosed by the invention can be referred to as figure 1.
A preparation method of the SiO 2 @Ag core-shell nanomaterial comprises the following steps:
s1, preparing a SiO 2 nano material with smooth surface and monodispersed (shown in the figure 1-1): 3mL of TEOS is added dropwise into a mixed solvent consisting of 53mL of absolute ethyl alcohol, 2.1mL of ammonia water and 2.33mL of deionized water, stirred at room temperature for reaction for 7h, washed with ethanol for several times and dried at 60 ℃ to prepare the monodisperse SiO 2 nano-material.
S2, introducing an Ag nano shell layer on the surface of the SiO 2 nano material (figures 1-2 and 1-3): dispersing the SiO 2 nano material obtained in the step S1 in 60mL of ethanol water solution (ethanol: water=3:1, v/v), enabling the concentration of monodisperse SiO 2 particles to be 20mg/mL, adding freshly prepared [ Ag (NH 3)2]+ silver ammonia solution, [ Ag (NH 3)2]+ silver ammonia solution concentration is 100 mg/mL), adding 5mL in volume, carrying out ultrasonic reaction for 30min, adding PVP ethanol solution, PVP ethanol solution concentration is 14.5mg/mL, adding 140mL in volume, stirring at 70 ℃ for reaction for 7h, repeating 3 times of silver mirror reaction, washing a reaction product with ethanol, and drying at 60 ℃ to obtain the SiO 2 @Ag core-shell nano material.
Wherein the SiO 2 @Ag core-shell nanomaterial prepared by 1 silver mirror reaction is SiO 2 @Ag-1; siO 2 @ Ag core-shell nano material prepared by 2 times of silver mirror reaction is SiO 2 @ Ag-2; the SiO 2 @Ag core-shell nano material prepared by 3 times of silver mirror reaction is SiO 2 @Ag-3; the SiO 2 @Ag core-shell nanomaterial prepared by 4 times of silver mirror reaction is SiO 2 @Ag-4.
Example 2: electron microscope characterization of the product of example 1
FIG. 2 reflects the characterization results of SiO 2 @ Ag core-shell nanomaterials. From the electron microscope image, the particle size of SiO 2 particles is about 150nm, and the surface is very smooth; after the surface undergoes silver mirror reaction, agNPs with uniform size are gradually modified on the surface of SiO 2 particles, and the AgNPs on the surface of SiO 2 particles are higher and higher in density and relatively uniform in distribution along with the increase of the number of silver mirror reaction times, so that a stable SiO 2 @Ag core-shell nano material is formed; it was found that the AgNPs were almost entirely covered with SiO 2 particles after 4 silver mirror reactions.
Example 3: zeta potential characterization of the product of example 1
FIG. 3 reflects the Zeta potential characterization results of SiO 2 nanoparticles and SiO 2 @Ag core-shell nanomaterials. From the zeta potential results, the zeta potential of the SiO 2 nano-particles is about-30 mV, and the zeta potential of the SiO 2 @Ag core-shell nano-material moves in the negative direction along with the continuous coverage of AgNPs, so that the formation of the sum peak of [ M+Na ] +、[M+K]+ and [ M+Ag ] + in the LDI process is facilitated, and the ionization efficiency is improved.
Example 4: use of SiO 2 @ Ag core-shell nanomaterial for mass spectrometry detection of beta-carotene and lutein
The LDI-MS mechanism diagram of the SiO 2 @Ag core-shell nanomaterial for beta-carotene and lutein disclosed by the invention can be referred to as a figure 1, and specifically comprises the following steps of:
(1) Preparing a suspension of SiO 2 @Ag core-shell nanomaterial with a particle concentration of 1mg/mL, and using the suspension as a nanomatrix for assisting a laser desorption/ionization process (figures 1-4);
(2) Preparing a mixture of an equal volume of SiO 2 @Ag core-shell nanomaterial solution and a sample solution to be detected on a mass spectrum target plate, wherein the volume dosage of the two solutions is 1 mu L, and the mixture is used for the subsequent direct laser desorption/ionization process and mass spectrum detection;
(3) Detecting according to a conventional LDI-MS detection method, wherein the molecular weight range is 100-1000 Da, and the detection mode is positive ions; the mixed sample residues are degraded and sampled by adopting pulse laser, the light beam wavelength of a pulse light source is 355nm, the pulse width is 1 fs-1 ms, the light beam diameter is 0.01-10 mm, the instantaneous pulse energy is 1 nJ-100 mJ, the pulse frequency is 0.05-100 MHz, and the mass spectrum signals of beta-carotene/lutein in the sample to be detected are obtained by detecting the mixed sample residues by a mass analyzer (figures 1-5).
Example 5: mass spectrum detection of beta-carotene and lutein under different concentrations of SiO 2 @Ag core-shell nanomaterial
FIG. 4 shows that when the concentration of the analyte is fixed to be 1mg/mL, the ratio of the concentration of the SiO 2 @Ag core-shell nanomaterial to the concentration of the analyte is (A) 1:1, (B) 10:1, and (C) 1:10, respectively, and the LDI-MS mass spectrum detection results are compared. The result shows that when the SiO 2 @Ag core-shell nano material is excessive or equivalent to an analyte, the optimal carotenoid substance detection capability can be obtained, and the spectrogram signal-to-noise ratio is high.
Example 6: detection limit result of SiO 2 @ Ag core-shell nano material on beta-carotene and lutein
FIG. 5 reflects the detection limit results of the SiO 2 @ Ag core-shell nanomaterial of the present invention for beta-carotene and lutein materials, respectively. The result shows that the absolute detection limit of the SiO 2 @Ag core-shell nano material on carotenoid substances can reach 0.5-2.5 pmol.
Example 7: detection capability of SiO 2 @ Ag core-shell nano material in actual sample
FIG. 6 shows that under the positive ion mode, the SiO 2 @Ag core-shell nanomaterial of the invention is used for (A) mass spectrograms of carrot juice analysis of a certain brand in the market, and (B) [ beta-carotene+Ag ] + and (C) [ lutein+Ag ] + isotope distribution diagrams, and the concentration of the nanomaterial is 1mg/mL. The result shows that even in a complex actual sample matrix, siO 2 @Ag core-shell nano material can still well detect carotenoid substances such as beta-carotene, lutein and the like, and the spectrum chart has not only [ M+Na ] + spectrum peaks but also stronger [ M+Ag ] + spectrum peaks, so that the detection sensitivity and analysis specificity of the material to the carotenoid substances are further improved.
Example 8: comparison of detection results of SiO 2 @ Ag core-shell nano material and AgNP nano particles in actual samples
FIG. 7 shows that in the positive ion mode, the concentration of the nano material is 1mg/mL compared with the spectrogram of the (A) SiO 2 @Ag core-shell nano material and the (B) AgNP nano particle used for analyzing carrot juice of a certain brand in the market. The result shows that compared with AgNP nano particles only can obtain carotenoid substances with low response, the SiO 2 @Ag core-shell nano material can obtain higher signal intensity (improved by 1-2 orders of magnitude), and meanwhile, in a complex actual sample matrix, the spectrogram background of the SiO 2 @Ag core-shell nano material is cleaner, so that the spectral peak identification is facilitated. These results demonstrate that the nanoscale roughness and nanoslit of the SiO 2 @ Ag core-shell nanomaterial surface is more conducive to providing high capacity capture of target analytes and the resulting increase in laser desorption/ionization efficiency.
Example 9: siO 2 @ Ag core-shell nanomaterial for evaluating reproducibility between midpoint and point in LDI-MS analysis
FIG. 8 reflects the point-to-point reproducibility study when the SiO 2 @Ag core-shell nanomaterial was used for mass spectrometry of lutein mass. The result shows that the Relative Standard Deviation (RSD) of the SiO 2 @Ag core-shell nanomaterial to lutein can be lower than 5%, and the core-shell nanomaterial has good reproducibility and crystallization condition in a sampling area, so that the reliability and repeatability of the method are further improved.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that the above-mentioned preferred embodiment should not be construed as limiting the invention, and the scope of the invention should be defined by the appended claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.
Claims (2)
- Application of SiO 2 @Ag core-shell nanomaterial as a nanomatrix in laser desorption/ionization mass spectrometry detection of carotenoids; the SiO 2 @Ag core-shell nanomaterial is prepared by the following steps:S1, adding tetraethoxysilane into a mixed solvent, stirring at room temperature for reaction 7 h, washing with ethanol after the reaction is finished, and drying at 60 ℃ to prepare a monodisperse SiO 2 nano material; the mixed solvent consists of absolute ethyl alcohol, ammonia water and deionized water according to the volume ratio of 53:2.1:2.33; the volume ratio of the tetraethoxysilane to the mixed solvent is 3:57.43; the particle size of the monodisperse SiO 2 nano material is 150 nm;S2, dispersing the SiO 2 nano material obtained in the step S1 in an ethanol water solution consisting of ethanol and water according to a volume ratio of 3:1, enabling the concentration of monodisperse SiO 2 particles to be 20 mg/mL, adding freshly prepared [ Ag (NH 3)2]+ silver ammonia solution, [ Ag (NH 3)2]+ silver ammonia solution concentration is 100 mg/mL), carrying out ultrasonic reaction for 30: 30min, adding polyvinylpyrrolidone ethanol solution, enabling the concentration of polyvinylpyrrolidone ethanol solution to be 14.5 mg/mL, stirring at 70 ℃ for reaction for 7: 7h, repeating silver mirror reaction for 3 times, washing a reaction product with ethanol, and drying at 60 ℃ to obtain the SiO 2 @Ag core-shell nano material, wherein the volume ratio of the ethanol water solution, the silver ammonia solution and the polyvinylpyrrolidone ethanol solution is 12:1:28;The zeta potential of the SiO 2 nano-particles is-30 mV, and the zeta potential of the SiO 2 @Ag core-shell nano-material moves in the negative direction along with the continuous coverage of the silver nano-particles.
- 2. The mass spectrometry method for detecting carotenoid based on SiO 2 @Ag core-shell nanomaterial is characterized by comprising the following steps of:(1) Dispersing the SiO 2 @Ag core-shell nanomaterial prepared in the method of claim 1 to obtain a suspension with the particle concentration of 1 mg/mL, and using the suspension as a nanomatrix for assisting a laser desorption/ionization process;(2) Preparing a mixture of an equal volume of SiO 2 @Ag core-shell nanomaterial solution and a sample solution to be detected on a mass spectrum target plate, wherein the concentration of the sample solution to be detected is 1 mg/mL, and the mixture is used for subsequent direct laser desorption/ionization process and mass spectrum detection;(3) Mass spectrometry detection: carrying out degradation sampling on mixed sample residues by adopting laser, and detecting by a mass analyzer to obtain the mass spectrum signal intensity of carotenoid in the sample; the molecular weight range of the mass spectrum detection method is 100-1000 Da, and the mass spectrum detection method is a positive ion detection mode; the light source of the laser is a continuous or pulse light source; the wavelength of the light beam of the continuous light source is 46.9-2940 nm, the diameter of the light beam is 0.01-10 mm, and the average power is not less than 0.1 mW; the light beam wavelength of the pulse light source is 46.9-2940 nm, the pulse width is 1 fs-1 ms, the light beam diameter is 0.01-10 mm, the instant pulse energy is 1 nJ-100 mJ, and the pulse frequency is 0.05-100 MHz.
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| CN105026368A (en) * | 2013-02-22 | 2015-11-04 | 莎尤纳诺新加坡私人有限公司 | Process for the isolation of carotenoids |
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| CN108918647A (en) * | 2013-03-13 | 2018-11-30 | 基纳生物技术有限公司 | For the mass spectrographic preparation reinforcing of MALDI and application method |
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| CN105026368A (en) * | 2013-02-22 | 2015-11-04 | 莎尤纳诺新加坡私人有限公司 | Process for the isolation of carotenoids |
| CN108918647A (en) * | 2013-03-13 | 2018-11-30 | 基纳生物技术有限公司 | For the mass spectrographic preparation reinforcing of MALDI and application method |
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