CN111834193B - Laser analysis ionization method based on optical fiber conduction - Google Patents
Laser analysis ionization method based on optical fiber conduction Download PDFInfo
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- CN111834193B CN111834193B CN202010699881.6A CN202010699881A CN111834193B CN 111834193 B CN111834193 B CN 111834193B CN 202010699881 A CN202010699881 A CN 202010699881A CN 111834193 B CN111834193 B CN 111834193B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0409—Sample holders or containers
- H01J49/0418—Sample holders or containers for laser desorption, e.g. matrix-assisted laser desorption/ionisation [MALDI] plates or surface enhanced laser desorption/ionisation [SELDI] plates
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- 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
- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0459—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for solid samples
- H01J49/0463—Desorption by laser or particle beam, followed by ionisation as a separate step
Abstract
The invention relates to the technical field of laser analysis, in particular to a laser analysis ionization method based on optical fiber conduction, which comprises the following steps: s1, etching the end part of the optical fiber by using hydrofluoric acid; s2, coating a solid-phase micro-extraction coating on the etched part of the optical fiber; s3, extracting a target analyte in a sample to be detected by using the optical fiber to enable the target analyte to be adsorbed on the solid-phase micro-extraction coating; s4, the laser system emits laser, the laser is coupled into the optical fiber, and the laser can be emitted to the solid phase micro-extraction coating through the optical fiber; s5, after the step S4, the laser is absorbed by the solid phase micro-extraction coating, so that the molecules of the target analyte attached to the solid phase micro-extraction coating are ionized and then separated from the solid phase micro-extraction coating. The invention can realize high flux ionization and improve excitation efficiency; and the background interference during the detection of the small molecules can be obviously reduced, and the detection sensitivity is improved.
Description
Technical Field
The invention relates to the technical field of laser analysis, in particular to a laser analysis ionization method based on optical fiber conduction.
Background
The existing laser ionization method is Matrix Assisted Laser Desorption Ionization (MALDI) and is widely applied to the analysis and detection of biological macromolecules, but because the technology can simultaneously excite molecules of a target analyte and excite matrix molecules, the analysis of small molecular compounds can be interfered by the matrix molecules; also, this technique is limited by the laser spot size, only the analyte within the laser spot will be excited, and therefore its sensitivity is limited; furthermore, the inevitable human error in the sample preparation and spotting process causes the difference in the shortcut status between the target analyte and the matrix, so that the signal deviation between multiple target spots is large, and the quantitative detection has a large limitation.
Chinese patent publication No. CN111092359A discloses a laser system for matrix-assisted laser desorption ionization time-of-flight mass spectrometer, which solves the scattering phenomenon of single-mode pulsed light generated by a solid laser in a multimode optical fiber, and achieves the purpose of improving the sample ionization effect of the matrix-assisted laser desorption ionization time-of-flight mass spectrometer.
However, the above scheme is to apply laser from the surface of the substrate to ionize molecules, so that only target molecules and the substrate in the laser spot can be excited, resulting in low excitation efficiency.
Disclosure of Invention
The invention aims to overcome the defect of low excitation efficiency, and provides a laser analysis ionization method based on optical fiber conduction, which can realize high-flux ionization and improve excitation efficiency; and the background interference during the detection of the small molecules can be obviously reduced, and the detection sensitivity is improved.
In order to solve the technical problems, the invention adopts the technical scheme that:
the laser analysis ionization method based on optical fiber conduction comprises an optical fiber, a laser system and a sample to be detected, and comprises the following steps:
s1, etching the end of the optical fiber by hydrofluoric acid;
s2, after the step S1, coating a solid phase micro-extraction coating on the etched part of the optical fiber;
s3, after the step S2, extracting the target analyte in the sample to be tested by using the optical fiber, so that the target analyte is adsorbed on the solid phase micro-extraction coating;
s4, after the step S3, the laser system emits laser light and couples the laser light into the optical fiber, so that the laser light can be emitted to the solid phase microextraction coating through the optical fiber;
s5, after step S4, the laser light is absorbed by the solid phase microextraction coating, ionizes molecules of the target analyte attached to the solid phase microextraction coating, and then detaches from the solid phase microextraction coating.
The invention relates to a laser desorption ionization method based on optical fiber conduction, which can realize high enrichment capacity on target analyte molecules by coating a solid-phase microextraction coating, has high laser absorption capacity and photoelectric conversion efficiency, thereby realizing the laser ionization process on the target analyte molecules, and meanwhile, the coating can not be separated by laser excitation, thereby obviously reducing the background interference during small molecule detection. The method can realize the laser ionization process of the whole coating at the same time, realize high-flux ionization and improve the detection sensitivity. Moreover, the solid phase microextraction coating has good stability and low damage rate, and can be repeatedly used in a plurality of continuous analysis processes, so that the repeatability of analysis and detection is good, and the quantitative detection is facilitated.
Furthermore, the optical fiber comprises a coating layer, an outer cladding layer and a fiber core which are sequentially arranged from outside to inside.
Further, the step S1 specifically includes the following steps:
s11, peeling off the coating layer at the end of the optical fiber to expose the outer cladding layer;
s12, after the step S11, the outer cladding layer is immersed in hydrofluoric acid water solution and stands to expose the fiber core.
Further, in step S2, the solid-phase microextraction coating is one or more of a high molecular polymer, a carbon material, or metal oxide particles.
Further, in step S2, coating of a coating layer is performed on the etched portion of the optical fiber by any one of an in-situ growth method, a chemical bonding method, a sol-gel method, or a dip coating method.
Further, in step S3, when the optical fiber is used to extract the target analyte in the sample to be tested, the target analyte in the sample to be tested is extracted by a headspace extraction or immersion extraction method.
Further, in step S4, the laser system includes a laser generator and a laser coupling device, and the laser generated by the laser generator is coupled into the optical fiber through the laser coupling device, so that the laser is transmitted at the fiber core and then exits to the solid phase microextraction coating.
Further, the laser coupling device comprises a three-dimensional base and a convex lens arranged on the three-dimensional base.
Further, the step S4 specifically includes the following steps:
s41, fixing the end of the optical fiber which is not etched on the three-dimensional base;
s42, the laser generator emits laser, and the laser is converged by the convex lens to form a laser spot;
s43, aligning the fiber core with the laser by adjusting the three-dimensional base, and enabling the laser spot size to be close to or equal to the diameter of the fiber core.
Further, after step S5, the ionized target analyte is subjected to mass detection by using a time-of-flight mass spectrometer, so as to realize qualitative and quantitative detection of the target analyte.
Compared with the prior art, the invention has the beneficial effects that:
(1) through coating the solid-phase microextraction coating, the high enrichment capacity of target analyte molecules can be realized, and the coating also has high laser absorption capacity and photoelectric conversion efficiency, so that the laser ionization process of the target analyte molecules is realized, and meanwhile, the coating cannot be separated by laser excitation, so that the background interference during small molecule detection can be remarkably reduced.
(3) The solid phase microextraction coating has good stability and low damage rate, and can be repeatedly used in a plurality of continuous analysis processes, so that the repeatability of analysis and detection is good, and the quantitative detection is facilitated.
(4) The invention can realize the laser ionization process of the whole coating at the same time, realize high-flux ionization and improve the detection sensitivity.
Drawings
FIG. 1 is a flow chart of a laser desorption ionization method based on fiber optic transmission according to the present invention.
Fig. 2 is a schematic structural diagram of a laser desorption ionization method based on optical fiber conduction according to the present invention.
Fig. 3 is a schematic structural diagram of the optical fiber obtained after step S2 of the laser desorption ionization method based on optical fiber transmission according to the present invention.
Fig. 4 is a schematic structural diagram of a laser system and an optical fiber portion of the present invention.
The graphic symbols are illustrated as follows:
1-laser generator, 2-laser coupling device, 21-three-dimensional base, 22-convex lens, 3-optical fiber, 31-coating layer, 32-outer cladding layer, 33-fiber core, 4-solid phase micro-extraction coating and 5-target analyte.
Detailed Description
The present invention will be further described with reference to the following embodiments. Wherein the showings are for the purpose of illustration only and are shown by way of illustration only and not in actual form, and are not to be construed as limiting the present patent; to better illustrate the embodiments of the present invention, some parts of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.
The same or similar reference numerals in the drawings of the embodiments of the present invention correspond to the same or similar components; in the description of the present invention, it should be understood that if there is an orientation or positional relationship indicated by the terms "upper", "lower", "left", "right", etc. based on the orientation or positional relationship shown in the drawings, it is only for convenience of describing the present invention and simplifying the description, but it is not intended to indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and therefore, the terms describing the positional relationship in the drawings are only used for illustrative purposes and are not to be construed as limiting the present patent, and the specific meaning of the terms may be understood by those skilled in the art according to specific circumstances.
Example 1
Fig. 1 to 4 show a first embodiment of a laser desorption ionization method based on optical fiber transmission according to the present invention, which includes an optical fiber 3, a laser system, and a sample to be tested, and the method includes the following steps:
s1, pretreatment of the optical fiber: the end of the optical fiber 3 is etched using hydrofluoric acid. The optical fiber 3 includes a coating layer 31, an outer cladding layer 32, and a fiber core 33, which are sequentially disposed from outside to inside, and step S1 specifically includes the following steps:
s11, stripping the coating layer 31 of the 1-1.5cm length part at one end of the optical fiber 3 to expose the outer cladding layer 32; in this embodiment, the coating layer 31 is stripped off from a 1cm length portion of the optical fiber 3 at one end thereof.
S12, after the step S11, the optical fiber 3 is fixed on a stage, and then the bare outer cladding 32 is immersed in an aqueous hydrofluoric acid solution and left to stand, so that the outer cladding 32 is removed and the core 33 is bare. When hydrofluoric acid with the purity of 48% -51% is selected, dilution is needed, and 10ml of deionized water and 10ml of hydrofluoric acid with the same volume are added into a polytetrafluoroethylene container for dilution to obtain hydrofluoric acid aqueous solution; the outer clad 32 can be removed by leaving the hydrofluoric acid aqueous solution for 3 hours.
In this embodiment, the optical fiber 3 is Fiblet FOPC-SMA 905-1000/1035/1400.
S2 coating: after step S1, the solid phase microextraction coating 4 is applied at the etched portion of the optical fiber 3, i.e., the solid phase microextraction coating 4 is applied at the bare portion of the fiber core 33.
In step S2, the solid-phase microextraction coating 4 is one or more of a high molecular polymer, a carbon material, or metal oxide particles. Wherein the high molecular polymer can be selected from porous organic polymer, Polydimethylsiloxane (PDMS), Polyaniline (PANI), etc.; the porous organic polymer can be selected from Metal Organic Framework (MOF), covalent organic polymer framework (COF) and the like; the carbon material can be selected from graphene, graphene oxide, mesoporous carbon, etc.; the metal oxide particles may be titanium dioxide. It should be noted that, the material selection of the solid phase microextraction coating 4 includes, but is not limited to, the above listed materials, and it is sufficient to select a high performance material having high enrichment capacity for the target analyte 5, and also having high laser absorption capacity and photoelectric conversion rate.
In step S2, the etched portion of the optical fiber 3, i.e., the bare core 33 portion, is coated with a coating layer by any one of in-situ growth, chemical bonding, sol-gel, or dip coating. The coated optical fiber 3 is shown in fig. 3. When a high molecular polymer is selected as the solid phase microextraction coating 4, the coating can be carried out by any of the above methods; when the carbon material or the metal oxide particle and the composite material thereof are selected as the solid phase micro-extraction coating 4, or when any several of the high molecular polymer, the carbon material and the metal oxide particle are selected as the solid phase micro-extraction coating 4, the coating can be coated by any one of an in-situ growth method, a sol-gel method and a dip coating method. The method of applying the solid phase microextraction coating 4 includes, but is not limited to, the above-mentioned methods, and a method capable of applying the solid phase microextraction coating 4 to the optical fiber 3 may be selected. It should be noted that the thickness of the solid phase micro-extraction coating 4 coated on the core 33 can be adjusted according to the actual requirement.
S3, extraction: after step S2, the target analyte 5 in the sample to be tested is extracted using the optical fiber 3, so that the target analyte 5 is adsorbed on the solid phase microextraction coating 4. The target analyte 5 in the sample to be tested can be extracted by a headspace extraction or immersion extraction method. The conditions of the extraction mode, the extraction time, the extraction temperature and the like are correspondingly selected according to the difference of the material of the solid-phase micro-extraction coating 4 and the target analyte 5, so that the sensitivity in detection can be greatly improved. The sample to be detected can be an environmental water sample, urine, serum and the like.
For example, when BTEX, a volatile benzene-based substance in an environmental water sample, is selected as the target analyte 5, a headspace extraction method may be used, and a polydimethylsiloxane/titanium dioxide composite material may be used as the solid phase microextraction coating 4. The polydimethylsiloxane has stronger adsorption capacity and is a common solid-phase microextraction probe coating on the market, and the titanium dioxide has better photoelectric conversion efficiency and can improve the ionization efficiency of the coating to target molecules; the probe coating may be prepared using a dip coating method when performing the coating.
For another example, when persistent organic pollutants such as Polycyclic Aromatic Hydrocarbons (PAHs) or polychlorinated biphenyl (PCBs) which are difficult to volatilize in an environmental water sample or urine are selected as the target analyte 5, immersion extraction can be used, a metal organic framework material ZIF-8 and the like is used as the solid-phase micro-extraction coating 4, an in-situ growth method or a chemical bonding method can be used for coating, organic monomers are firstly fixed by utilizing functional group modification, and then the metal organic framework material is grown in a self-assembly mode. The metal organic framework material has a large specific surface area, so that the metal organic framework material has strong adsorption capacity, metal element sites and strong photoelectric conversion capacity.
S4. laser transmission: after step S3, the laser system emits laser light and couples the laser light into the optical fiber 3, so that the laser light can exit through the optical fiber 3 to the solid phase microextraction coating 4. The laser system comprises a laser generator 1 and a laser coupling device 2, wherein laser emitted by the laser generator 1 is coupled into an optical fiber 3 through the laser coupling device 2, so that the laser is transmitted at a fiber core 33 and then is emitted to a solid phase microextraction coating 4.
The laser coupling device 2 includes a three-dimensional base 21 and a convex lens 22 disposed on the three-dimensional base 21. As shown in fig. 4, step S4 specifically includes the following steps:
s41, fixing the end of the optical fiber 3 which is not etched on the three-dimensional base 21;
s42, the laser generator 1 emits laser and converges the laser through the convex lens 22 to form a laser spot;
s43, the fiber core 33 is aligned with the laser by adjusting the three-dimensional base 21, and the distance between the three-dimensional base 21 and the laser generator 1 is adjusted to make the laser spot size infinitely close to or equal to the diameter of the fiber core 33.
In order to prevent the laser from hurting a person, in step S41, the optical fiber 3, the laser generator 1, and the laser coupling device 2 may be shielded by using a metal housing. In this embodiment, the laser generator 1 is an adjustable laser generator, and has the following formula:
E=hc/λ；
where E represents the photon energy generated, h represents the planck constant, c represents the speed of light, and λ represents the laser wavelength. Because the wavelength of the laser generator 1 is adjustable, the photon energy can be adjusted by adjusting the laser wavelength; different chemical bonds in different target analytes 5 have different bond energies, so that the photon energy can be adjusted by adjusting the laser wavelength, thereby realizing selective breakage of the chemical bonds.
S5 ionization of laser: after step S4, the laser light is absorbed by the solid phase microextraction coating 4 and transfers energy to the target analyte 5, ionizing molecules of the target analyte 5 attached to the solid phase microextraction coating 4 and then detaching from the solid phase microextraction coating 4. And the solid phase micro-extraction coating 4 can not be separated by laser excitation, so that the background interference in small molecule detection can be obviously reduced.
Example 2
This embodiment is similar to embodiment 1, except that step S6 is further included in this embodiment: after step S5, the target analyte 5 that is ionized is mass-detected using a time-of-flight mass spectrometer, enabling qualitative and quantitative detection of the target analyte 5.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. A laser analysis ionization method based on optical fiber conduction is characterized by comprising an optical fiber (3), a laser system and a sample to be detected, and the method comprises the following steps:
s1, etching the end of the optical fiber (3) by hydrofluoric acid;
s2, after the step S1, coating a solid phase micro-extraction coating (4) on the etching part of the optical fiber (3);
s3, after the step S2, extracting a target analyte (5) in a sample to be tested by using the optical fiber (3), and enabling the target analyte (5) to be adsorbed on the solid phase micro-extraction coating (4);
s4, after the step S3, the laser system emits laser light and couples the laser light into the optical fiber (3) so that the laser light can be emitted to the solid phase microextraction coating (4) through the optical fiber (3);
s5, after step S4, the laser light is absorbed by the solid phase microextraction coating (4), ionizing molecules of the target analyte (5) attached to the solid phase microextraction coating (4), and then detaching from the solid phase microextraction coating (4).
2. The method of claim 1, wherein the optical fiber (3) comprises a coating layer (31), an outer cladding layer (32) and a fiber core (33) which are arranged in sequence from outside to inside.
3. The method according to claim 2, wherein the step S1 specifically comprises the following steps:
s11, peeling off the coating layer (31) at the end of the optical fiber (3) to expose the outer cladding layer (32);
s12, after the step S11, the outer cladding layer (32) is immersed in hydrofluoric acid water solution and stands still to expose the fiber core (33).
4. The method for laser desorption ionization based on optical fiber transmission according to claim 1, wherein in step S2, the solid phase microextraction coating (4) is any one or more of high molecular polymer, carbon material or metal oxide particles.
5. The method of claim 1, wherein the coating of the coating layer is performed at the etched portion of the optical fiber (3) by any one of an in-situ growth method, a chemical bonding method, a sol-gel method, or a dip coating method in step S2.
6. The method of claim 1, wherein in step S3, the target analyte (5) in the sample to be tested is extracted by a headspace extraction or immersion extraction method.
7. The method for laser desorption ionization based on optical fiber transmission according to claim 2, wherein in step S4, the laser system comprises a laser generator (1) and a laser coupling device (2), the laser generated by the laser generator (1) is coupled into the optical fiber (3) through the laser coupling device (2), so that the laser is transmitted at the fiber core (33) and then exits to the solid phase microextraction coating (4).
8. The method for laser desorption ionization based on optical fiber transmission according to claim 7, wherein the laser coupling device (2) comprises a three-dimensional base (21) and a convex lens (22) arranged on the three-dimensional base (21).
9. The method according to claim 8, wherein the step S4 specifically comprises the following steps:
s41, fixing the end of the optical fiber (3) which is not etched on the three-dimensional base (21);
s42, emitting laser by the laser generator (1), and converging the laser by the convex lens (22) to form a laser spot;
s43, aligning the fiber core (33) with the laser by adjusting the three-dimensional base (21), and enabling the laser spot size to be close to or equal to the diameter of the fiber core (33).
10. The method of claim 1, wherein after step S5, the ionized target analyte (5) is mass detected using a time-of-flight mass spectrometer, thereby achieving qualitative and quantitative detection of the target analyte (5).
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| CN202010699881.6A CN111834193B (en) | 2020-07-20 | 2020-07-20 | Laser analysis ionization method based on optical fiber conduction |
| PCT/CN2020/113967 WO2022016681A1 (en) | 2020-07-20 | 2020-09-08 | Laser desorption ionization method based on optical fiber conduction |
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| CN109939658A (en) * | 2019-04-17 | 2019-06-28 | 邱俊琅 | A kind of extraction coating, solid phase micro extraction probe and its preparation method and application |
| CN110887891A (en) * | 2019-11-07 | 2020-03-17 | 广东省测试分析研究所（中国广州分析测试中心） | Micro-extraction-nano-liter electrospray ion source system in capillary and application |
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| JP2014524121A (en) * | 2011-07-14 | 2014-09-18 | ザ・ジョージ・ワシントン・ユニバーシティ | Plume collimation for laser ablation and electrospray ionization mass spectrometry |
| CN103308474A (en) * | 2013-05-29 | 2013-09-18 | 燕山大学 | Method for detecting petroleum pollutants in water by employing optical-fiber evanescent wave probe unit |
| TW201601827A (en) * | 2014-07-04 | 2016-01-16 | Nat Tainan Junior College Of Nursing | Solid phase micro-extraction fiber preparation method |
| CN108362653B (en) * | 2018-02-05 | 2019-06-14 | 西南石油大学 | A kind of Solid Phase Extraction functional fiber fadout field sensor and its assemble method |
| WO2020050829A1 (en) * | 2018-09-05 | 2020-03-12 | Bae Systems Information And Electronic Systems Integration Inc. | Carbide-derived carbon for solid-phase micro extraction media |
| CN109724952B (en) * | 2018-11-21 | 2022-02-11 | 华南师范大学 | Optical fiber probe and preparation method thereof, optical fiber sensor and application thereof |
| CN110554014B (en) * | 2019-08-30 | 2022-04-19 | 华南师范大学 | Molecular imprinting fluorescence optical fiber sensor, construction method thereof and fluorescence detection method |
| CN111092359A (en) * | 2019-12-27 | 2020-05-01 | 安图实验仪器(郑州)有限公司 | Laser system for matrix-assisted laser desorption ionization time-of-flight mass spectrometer |
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| CN109939658A (en) * | 2019-04-17 | 2019-06-28 | 邱俊琅 | A kind of extraction coating, solid phase micro extraction probe and its preparation method and application |
| CN110887891A (en) * | 2019-11-07 | 2020-03-17 | 广东省测试分析研究所（中国广州分析测试中心） | Micro-extraction-nano-liter electrospray ion source system in capillary and application |
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