CN112014357A - Trace pesticide residue detection system based on surface plasma resonance technology - Google Patents
Trace pesticide residue detection system based on surface plasma resonance technology Download PDFInfo
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Abstract
The invention discloses a trace pesticide residue detection system based on a surface plasma resonance technology, which comprises the following components: the system comprises an enhanced SPR biosensor, an adjustable laser pulse generator and an optical fiber loop demodulation system; the enhanced SPR biosensor detects light sources with different wavelengths emitted by the adjustable laser pulse generator; the fiber loop demodulation system is used for demodulating the enhanced SPR biosensor. The invention combines the nano particle reinforced SPR technology and the optical fiber loop absorption technology to design and manufacture the biomass sensing system; the nano particle enhanced SPR sensor is a research hotspot in the field of SPR at present, and the high-sensitivity characteristic of the nano particle enhanced SPR sensor is suitable for sensing various biomasses; the system sensitivity is further improved and the quick response capability is ensured by adopting the demodulation of the optical fiber loop absorption technology; the system has ultrahigh sensitivity (10-8RIU) and quasi-real-time response capability (ms level).
Description
Technical Field
The invention relates to the technical field of pesticide residue detection, in particular to a trace pesticide residue detection system based on a surface plasma resonance technology.
Background
The pesticide residue refers to a pesticide original or toxic metabolite remaining in a use object after the pesticide is used, and is generally not easy to volatilize and degrade. With the forbidding of strong toxicity pesticides, pesticide residue distribution of organochlorine pesticide > organophosphorus pesticide > plant pesticide is gradually formed. At present, food and drug safety management mechanisms in all levels of markets are established, and new requirements of portability and low cost are provided for detection instruments. Qualitative and quantitative detection sensing research on agricultural harmful substances is actively carried out by research units at all levels and related departments. The research method can be mainly summarized as follows: an instrument detection method; an enzyme inhibition method; a biosensor method; biological biopsy, and the like.
The main method for detecting the comparative pesticide residue, such as gas chromatography, liquid chromatography and the like, is an accepted standard detection method due to mature detection principle and equipment, and can realize direct and accurate detection of a sample. The living organism method is not suitable for being popularized and applied as a quick detection method because the living organism is used for direct measurement, and the detection precision and the effectiveness are poor. The enzyme inhibition detection method based on acetylcholinesterase activity inhibition can realize on-site preliminary screening of pesticides and has practical value, but is easily interfered by multi-stage transmission and conversion of detection signals, so the detection instrument also has certain improvement and promotion space.
Disclosure of Invention
In order to solve the problems in the prior art, the embodiment of the invention provides a trace pesticide residue detection system based on a surface plasmon resonance technology. The technical scheme is as follows:
in one aspect, a trace pesticide residue detection system based on a surface plasmon resonance technology is provided, which includes: the system comprises an enhanced SPR biosensor, an adjustable laser pulse generator and an optical fiber loop demodulation system;
the enhanced SPR biosensor detects light sources with different wavelengths emitted by the adjustable laser pulse generator; the fiber loop demodulation system is used for demodulating the enhanced SPR biosensor.
Further, the enhanced SPR biosensor is manufactured based on a metal nanoparticle enhancement scheme and a grating type input and output structure.
Furthermore, the tunable laser pulse generator adopts a high-power fixed-wavelength laser Nd: YAG and a tunable diode laser TDL to be differentiated in a PPLN crystal to be modulated into tunable laser in a wide range.
Further, the tunable laser pulse generator comprises a gain-tunable erbium-doped fiber amplifier; the front end and the rear end of the gain-adjustable erbium-doped fiber amplifier are respectively connected with a fiber grating; the first fiber grating is arranged at the front end, and the second fiber grating is arranged at the rear end.
Further, the tunable laser pulse generator further comprises a tunable optical attenuator; one end of the adjustable optical attenuator is connected with the enhanced SPR biosensor, and the other end of the adjustable optical attenuator is connected with the second fiber bragg grating of the gain-adjustable erbium-doped fiber amplifier.
The technical scheme provided by the embodiment of the invention has the following beneficial effects:
1) the design and the manufacture of the biomass sensing system are carried out by combining the nano particle enhanced SPR technology and the optical fiber loop absorption technology.
The nano particle enhanced SPR sensor is a research hotspot in the field of SPR at present, and the high-sensitivity characteristic of the nano particle enhanced SPR sensor is suitable for sensing various biomasses; and the system sensitivity is further improved and the quick response capability is ensured by adopting the demodulation of the optical fiber loop absorption technology. The system has ultrahigh sensitivity (10-8RIU) and quasi-real-time response capability (ms level).
2) The system combines the advantages of intensity and wavelength SPR sensing systems.
The potential contradiction between the sensitivity and the dynamic range of the system is overcome, and the system can be suitable for large-dynamic-range measurement and reaction dynamics research on the basis of quick and sensitive measurement through the design of a servo control system.
3) All-fiber systems are suitable for remote monitoring applications.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic diagram of a trace pesticide residue detection system based on surface plasmon resonance technology according to an embodiment of the invention;
FIG. 2 is a workflow diagram of a project technique of an embodiment of the invention;
FIG. 3 is a schematic diagram of an enhanced SPR detection scheme of an embodiment of the present invention;
FIG. 4 is a flow chart of an embodiment of the invention for implementing SPR fabrication by nanosphere etching;
FIG. 5 is a schematic diagram of a diffraction grating structure according to an embodiment of the present invention;
FIG. 6 is a schematic diagram of a tunable laser pulse generator according to an embodiment of the present invention;
FIG. 7 is a schematic diagram of an embodiment of an erbium doped fiber amplifier with adjustable gain;
FIG. 8 is a schematic diagram of a variable optical attenuator according to an embodiment of the present invention;
FIG. 9 is a schematic diagram of a protein measurement experiment system according to an embodiment of the present invention
FIG. 10 is a schematic diagram of gain versus input signal strength for an embodiment of the present invention;
fig. 11 is a schematic diagram showing the relationship of the variation of the gain bragg wavelength according to the embodiment of the present invention;
FIG. 12 is a graphical illustration of the amount of attenuation versus longitudinal separation h for an embodiment of the present invention;
FIG. 13 is a graphical illustration of the relationship of attenuation versus L for an embodiment of the present invention;
fig. 14 is a schematic diagram of wavelength micro-loss characteristics of the variable optical attenuator according to the embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
The invention provides a trace pesticide residue detection system based on a surface plasma resonance technology, which is shown in figure 1 and comprises the following components: the system comprises an enhanced SPR biosensor 100, an adjustable laser pulse generator 200 and an optical fiber loop demodulation system 300;
the enhanced SPR biosensor 100 detects light sources emitting different wavelengths from the tunable laser pulse generator 200; the fiber loop demodulation system 300 is used to demodulate the enhanced SPR biosensor 100.
Further, the enhanced SPR biosensor is manufactured based on a metal nanoparticle enhancement scheme and a grating type input and output structure.
Furthermore, the tunable laser pulse generator adopts a high-power fixed-wavelength laser Nd: YAG and a tunable diode laser TDL to be differentiated in a PPLN crystal to be modulated into tunable laser in a wide range.
Further, the tunable laser pulse generator comprises a gain-tunable erbium-doped fiber amplifier; the front end and the rear end of the gain-adjustable erbium-doped fiber amplifier are respectively connected with a fiber grating; the first fiber grating is arranged at the front end, and the second fiber grating is arranged at the rear end.
Further, the tunable laser pulse generator further comprises a tunable optical attenuator; one end of the adjustable optical attenuator is connected with the enhanced SPR biosensor, and the other end of the adjustable optical attenuator is connected with the second fiber bragg grating of the gain-adjustable erbium-doped fiber amplifier.
In particular, Surface Plasmon Resonance (SPR) technology is a novel biosensing technology for studying interactions between molecules. The principle is that molecules capable of being combined with an object to be measured are physically or chemically fixed on the surface of an SPR sensor chip, and when the object to be measured and a corresponding coupling object on the surface of the chip act, optical parameters on the surface of the chip are changed and are expressed in the form of electric signals. Compared with the traditional analysis method, the SPR technology has the advantages of no need of labeling of samples, easy realization, real-time dynamic analysis, high selectivity, high sensitivity, high analysis speed and the like, is particularly suitable for the research of the interaction kinetic effect of molecules of various biomasses, such as the detection of the interaction between antigens and antibodies, between proteins and proteins, between drugs and proteins, between nucleic acids and nucleic acids, between receptors and ligands and other biomolecules, and has wide application in the fields of life science, environmental monitoring, drug research, food safety, protein detection and the like.
Trace amounts in the field of applied science refer to a substance content below one part per million. The pesticide residue detection is trace or trace analysis and can be realized only by adopting a high-sensitivity detection technology, and the SPR biosensor is a cross field of multiple disciplines and technologies and benefits from the rapid development of material science, life science, nanotechnology, semiconductor micromachining technology and electronic technology. The development of biomass measurement systems based on SPR technology is an important development of cross scientific research, and is a necessary way for the biosensor to be taken out of a laboratory to obtain practical application. The SPR biomass measurement system is utilized to improve the sensitivity, response speed and precision of biomass measurement and realize the ultra-sensitive and ultra-fast detection of trace pesticide residues, which has direct and important practical significance for various biochemical researches and the protection of human life health and safety.
In this embodiment, a trace pesticide residue detection system based on the surface plasmon resonance technology is also provided:
(1) fabrication of enhanced SPR biosensors
Referring to FIG. 2, the SPR enhanced detection scheme of FIG. 3 was designed according to the design requirements of the project. The analyte-ligand solution flows across the surface of the sensor chip on which the 'receptors' are immobilized, and when interacting and binding to each other, causes a change in the mass of the surface material, while the refractive index changes in proportion to the mass. SPR is graphically coupled to the fiber ring.
The project adopts a nanosphere etching method (NSL, shown in figure 4) to realize SPR manufacturing. A nanosphere self-assembly mask was first formed by polypropylene-ethylene sol deposition. Then, the metal is sputtered into the layer of nanospheres by high temperature or electron beam evaporation. After removing the polystyrene nanospheres, the remaining metal will form well-aligned triangular nanoparticles. By varying the radius of the deposited nanospheres and the thickness of the deposited metal, nanoparticles can be fabricated that achieve different widths, heights, and different particle spacings. Different sensitivity SPR designs can be realized by analyzing the shapes of the nanoparticles.
The sensitivity of the nano particles of the sensor to the local refractive index is close to 200 nm/unit refractive index through analysis. When molecules are bound to the nanotangular surface, a wavelength shift occurs when the refractive index changes, thus providing a basis for detecting, for example, protein binding.
The SPR was designed using a diffraction grating structure, and a resist layer of polymethyl methacrylate (PMMA) was formed on a Pyrex glass plate having a thickness of 1mm (fig. 5 diffraction grating structure). Using a Scanning Electron Microscope (SEM) equipped with a lithography system, a 100X 100 μm film was formed2The figure of the single-dimensional diffraction grating adopts fluorine ion groups to realize etching treatment, and anisotropic reaction ions of the single-dimensional diffraction grating complete the sub-wavelength grating with the etching depth of 35 nm. Ta of 285nm realized by sputtering treatment after depositing 40nm gold film2O5A waveguide layer.
The project is that the recycling of the sensor and the comparative experiment also adopt the following processing modes: the surface of the chip is rinsed by deionized water, washed by ethanol and dried by pure nitrogen. Then, the biochip is soaked in ethanol solution for six hours, and after soaking, the biochip is rinsed by deionized water, washed by ethanol and dried by pure nitrogen. Then, the NHS solution was soaked for 12 hours.
(2) Tunable laser pulse generator design
For the operation of SPR sensors at different wavelengths in the project, a tunable laser pulse generator was designed as shown in fig. 6. YAG and TDL are differentiated in PPLN crystal to modulate wide-range tunable laser. The adjustable mode locking fiber laser pulse generator provided by the invention is a programmable laser, overcomes the defects of the traditional laser, can adjust the wavelength of the emitted parallel laser pulse within the wide range of 1460-1610 nm according to the measurement type and the length of the measurement process, has the output pulse width of 5ns, and can output laser pulses with different periods according to the requirements.
(3) Gain-adjustable erbium-doped fiber amplifier design
The project also needs to complete the design of a gain-tunable erbium-doped fiber amplifier (VEDFA), the structure is shown in FIG. 7, the VEDFA is pumped back and forth, and fiber gratings (FBGt1 and FBGt2) are respectively connected to the front and back ends of the VEDFA, wherein FBGt1 is a fiber grating with a tunable Bragg wavelength.
The gain of the VEDFA in a natural state changes with the length of the erbium-doped fiber, and the gain of the unit erbium-doped fiber is set as
Wherein gamma is a scattering coefficient; alpha is an absorption coefficient;
is the inverse particle number per unit length, and
thus, the gain of an erbium doped fiber amplifier of length l is
In operation, since the reflection of the FBGs is equivalent to the formation of a resonant cavity in the amplifier, assuming that each FBG only affects the intra-cavity losses, there are[27]
Wherein G is the gain of VEDFA in the lasing state; rFPIs the intracavity equivalent reflectivity; k is a constant.
Experiments prove that RFPIs the reflectance R of FBGt11(lambda) and reflectivity R of FBGt22Product of (lambda) R1(λ)R2The maximum value of (lambda) is positiveParameters of ratios, i.e.
RFP＝k′[R1(λ)R2(λ)]max (11)
Since the bandwidth of the FBG is much smaller than the gain bandwidth of the VEDFA, at R1(lambda) and R2The maximum product position of (lambda) can generate a lasing state, and the Bragg wavelength value of the FBGt1 is adjusted, namely the product value of the reflectivities of the two FBGs can be changed, so that the gain of the VEDFA is changed, and the gain of the VEDFA is controlled in different states. As can be seen from equations (10) and (11), when the reflection spectra of the two FBGs are completely separated, the gain is maximized, and the FBGs enter a gain saturation state, and when the reflection spectra thereof are completely overlapped, the gain is minimized.
The gain control rule is realized by a self-adaptive control program of a PC (personal computer), and the change of the Bragg wavelength of the FBG is realized by the PZT (piezoelectric ceramic) electrostrictive effect. The driving direct current voltage of the PZT is adjusted by a variable direct current voltage source driven by a PC according to a program, and the FBGt1 is pasted on the PZT coated with a heat insulation layer, so that the expansion and contraction of the PZT lead the grating pitch Lambda of the FBG to be increased or reduced, and the change of the Bragg wavelength of the FBG is realized.
(4) Variable optical attenuator
In system design, the ring-down time of the output signal is a univariate function of the absorption intensity (reflecting the gas concentration), but in actual systems there are fiber losses, insertion element losses, ambient temperature, pressure variations, and losses due to photoelectric noise. This requires adjusting the gain of the VEDFA and the attenuation of the Variable Optical Attenuator (VOA) to keep the overall system in equilibrium. The system employs a variable optical attenuator as shown in fig. 8.
Assuming that the input power of signal light from fiber1 is P0, the output power P1 of fiber2 can be obtained according to the coupling characteristics of two tapered fibers in the coupler
P1＝P0sin(βz) (12)
Wherein z is the overlapping length of the two optical fibers; β is the coupling coefficient, which depends on the fiber core diameter a and the distance u between two parallel fiber core diameters, and can be expressed as:
wherein Δ ═ n1-n0)/n1(ii) a A, B and C are constants related to the cone angle.
From equation (13), it can be seen that the distance μ between two parallel fiber core diameters has a great influence on the coupling coefficient, and when the distance between the fiber core diameters increases, β tends to zero exponentially. P1/P0Changing according to sine rule, when using program-controlled stepping motor to control adjustable coupling cavity to regulate beta to make P1/P0An approximately linear attenuation of the VOA can be achieved when varying over a range of (pi/2, pi).
(5) Design and study of experimental systems
FIG. 9 shows an experimental system for single loop protein measurement using fiber optics.
1) Gain-adjustable erbium-doped fiber amplifier experiment
For the fig. 10 measurement system, the project will first experiment the EDFA, and the simulation virtual experiment of this work is already completed in the project pre-work. FIG. 14 is a graph showing the gain characteristic of an EDFA at an input signal wavelength of 1556.8nm, wherein the input power is controlled by an attenuator and the intensity is varied in the range of-30 dBm to-5 dBm. Figure 11 shows the gain as a function of the grating bragg wavelength interval with a signal input wavelength of 1556.8nm and an intensity of-30 dBm, with the amplifier gain varying from 2.8dB to 23dB over the experimental range.
The main content of the subsequent experiments is the gain stability research of the tunable erbium-doped fiber amplifier and the parameter selection by combining the SPR sensor characteristics.
2) Experiment with adjustable attenuator
The simulated virtual experiment of the experiment is completed in the project early stage work. FIG. 12 shows a curve of the longitudinal distance h versus the attenuation obtained from the experiment, wherein when 1.5< h <1.54 μm, the attenuation changes more gradually; when h is larger than 1.54 μm, the attenuation amount changes rapidly, the maximum value is close to 30dB, and the change of the longitudinal spacing h and the attenuation amount of the adjustable optical attenuator are approximately in an exponential relationship.
When the transverse overlap length L is adjusted, a curve of the amount of attenuation versus L can be obtained, as shown in fig. 13. It can be seen from the figure that when L is more than 0 and less than 70 μm, the attenuation of the variable optical attenuator is gradually reduced to approximately 0dB, and the coupling effect between the two optical fiber cones is enhanced; when L is more than 70 and less than 140 mu m, the attenuation of the variable optical attenuator is gradually increased, the coupling action between the two fiber cones is weakened, and the maximum attenuation reaches 37 dB. When a broadband light source with the wavelength range of 1530-1560 nm is used for carrying out wavelength-dependent test on the device, the wavelength micro-loss less than 0.2dB can be obtained, and the optical fiber attenuator has quite stable attenuation, as shown in FIG. 14. The subsequent experiments were mainly fast tuning response and error control experiments.
(6) Servo control System design and experiment
The main working modes of the system are as follows:
1) fixed wavelength measurement: the working wavelength is selected from the SPR sensor 3dB absorption wavelength, the whole loss of the optical fiber ring is adjusted to be in a low-loss state, and the measurement sensitivity to the SPR light intensity change is the highest. Stability control of gain-tunable erbium-doped fiber amplifiers is of critical importance.
2) Rapidly identifying a sample with unknown concentration: after the initial rough measurement, the working wavelength is tuned to the highest sensitivity according to the built-in sample database, and meanwhile, the gain-adjustable erbium-doped fiber amplifier is synchronously tuned to the optimal gain. And selecting an algorithm, and controlling the working process at 3-5 measurement periods.
3) And (3) reaction kinetic test: the intelligent adjustment of the working wavelength is realized by analyzing the measurement data, the optimal selection of the working wavelength and the gain system of the system is kept, and the tracking measurement of the reaction process is realized.
4) Ultrafast measurement mode: the system can sacrifice part of sensitivity and accelerate the measurement time, so that the overall loss of the optical fiber ring is high, the ring-down time can be reduced to more than ten pulse cycle periods, and the single measurement time can be reduced to the order of mu s.
In order to realize the functions, a servo system is required to be designed, corresponding control software and a sample characteristic database are established, and the performance test of a system platform is carried out.
The technical scheme provided by the embodiment of the invention has the following beneficial effects:
1) the design and the manufacture of the biomass sensing system are carried out by combining the nano particle enhanced SPR technology and the optical fiber loop absorption technology.
The nano particle enhanced SPR sensor is a research hotspot in the field of SPR at present, and the high-sensitivity characteristic of the nano particle enhanced SPR sensor is suitable for sensing various biomasses; and the system sensitivity is further improved and the quick response capability is ensured by adopting the demodulation of the optical fiber loop absorption technology. The system has ultrahigh sensitivity (10-8RIU) and quasi-real-time response capability (ms level).
2) The system combines the advantages of intensity and wavelength SPR sensing systems.
The potential contradiction between the sensitivity and the dynamic range of the system is overcome, and the system can be suitable for large-dynamic-range measurement and reaction dynamics research on the basis of quick and sensitive measurement through the design of a servo control system.
3) All-fiber systems are suitable for remote monitoring applications.
The above-described embodiments of the apparatus are merely illustrative, and the units described as separate parts may or may not be physically separate, and the parts displayed as units may or may not be physical units, may be located in one place, or may be distributed on a plurality of network units. Some or all of the modules may be selected according to actual needs to achieve the purpose of the solution of the present embodiment. One of ordinary skill in the art can understand and implement it without inventive effort.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent replacements, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A trace pesticide residue detection system based on surface plasmon resonance technology is characterized by comprising: the system comprises an enhanced SPR biosensor, an adjustable laser pulse generator and an optical fiber loop demodulation system;
the enhanced SPR biosensor detects light sources with different wavelengths emitted by the adjustable laser pulse generator; the fiber loop demodulation system is used for demodulating the enhanced SPR biosensor.
2. The system of claim 1, wherein the enhanced SPR biosensor is fabricated based on a metal nanoparticle enhancement scheme and a grating-based input-output structure.
3. The system of claim 2, wherein the tunable laser pulse generator employs a wide range of tunable lasers differentially modulated in a PPLN crystal by high power fixed wavelength lasers Nd: YAG and tunable diode lasers TDL.
4. The system of claim 3, wherein the tunable laser pulse generator comprises a gain-tunable erbium-doped fiber amplifier; the front end and the rear end of the gain-adjustable erbium-doped fiber amplifier are respectively connected with a fiber grating; the first fiber grating is arranged at the front end, and the second fiber grating is arranged at the rear end.
5. The system of claim 4, wherein the tunable laser pulse generator comprises a tunable optical attenuator; one end of the adjustable optical attenuator is connected with the enhanced SPR biosensor, and the other end of the adjustable optical attenuator is connected with the second fiber bragg grating of the gain-adjustable erbium-doped fiber amplifier.
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| CN113533261A (en) * | 2021-03-17 | 2021-10-22 | 广东工业大学 | Sensing system and detection method based on surface plasma resonance |
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| CN113533261A (en) * | 2021-03-17 | 2021-10-22 | 广东工业大学 | Sensing system and detection method based on surface plasma resonance |
| CN113533261B (en) * | 2021-03-17 | 2024-04-26 | 广东工业大学 | Sensing device and detection method based on surface plasmon resonance |
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