CN102590147A - Surface plasma resonance system capable of adjusting sensitivity and dynamic range and detection method thereof - Google Patents
Surface plasma resonance system capable of adjusting sensitivity and dynamic range and detection method thereof Download PDFInfo
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- CN102590147A CN102590147A CN2012100221965A CN201210022196A CN102590147A CN 102590147 A CN102590147 A CN 102590147A CN 2012100221965 A CN2012100221965 A CN 2012100221965A CN 201210022196 A CN201210022196 A CN 201210022196A CN 102590147 A CN102590147 A CN 102590147A
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Abstract
The invention discloses a surface plasma resonance system capable of adjusting sensitivity and dynamic range and a method thereof. The surface plasma resonance system consists of a reflective index adjustable surface plasma resonance coupling unit, a wide waveband polychromatic light source, an incident beam shaping unit and a reflected light detection unit, wherein the reflective index adjustable surface plasma resonance coupling unit comprises a reflective index adjustable fluid prism, a sensing chip and a sample flowing cell; the sensing chip is positioned on the fluid prism; the sample flowing cell is positioned on the sensing chip; the sensing chip comprises an optical transparent substrate and a sensing membrane positioned on the optical transparent substrate; the optical transparent substrate is contacted with a fluid medium in the fluid prism; and the sensing membrane forms one bottom surface of the sample flowing cell. The system can perform high-sensitivity detection analysis by aiming at various samples to be detected on the premise of guaranteeing the dynamic range. The system is not provided with a mechanical moving part and has high stability.
Description
Technical field
The invention belongs to the testing tool technical field, be specifically related to a kind of sensitivity and dynamic range adjustable surface plasma body resonant vibration system and detection method.
Background technology
Surface plasma body resonant vibration has been widely used in fields such as chemistry, biology, medical science, physics, material as a kind of mark, real-time interface analysis technology of original position exempted from.The ultimate principle of surface plasma body resonant vibration technology is based on the condition that surface plasma body resonant vibration takes place on the interface between sensing membrane and dielectric sample and changes with sample change of refractive on the interface.Can obtain the refractive index and the thickness information of sensing membrane surface sample through detection thus to the surface plasma body resonant vibration condition; And the detection through the surface plasma body resonant vibration condition is changed; Can monitor and analyze sensing membrane Surface Physical and chemical reaction; If target molecule is bonded in the sensing membrane surface; Biomolecule specific in the analyte will combine with target molecule generation specificity, then can carry out the interaction of molecules analysis.
Surface plasma body resonant vibration and surface plasma resonance image-forming two alanysis systems have been developed based on the surface plasma body resonant vibration technology.High sensitivity almost is pursuing one's goal of all analytic systems, and surface plasma body resonant vibration is no exception.At present; In the practical application of surface plasma body resonant vibration and imaging; Developed based on the raising sensitivity method that sample is modified and sensing membrane is modified, but these methods limitation method that all to be specific aims very strong, and improve sensitivity and also can bring reducing of dynamic range.Thereby if can set up a kind of sensitivity and dynamic range adjustable, the surface plasma resonance sensing method of tool universality is very important and significant.
Summary of the invention
The object of the present invention is to provide a kind of have universality, sensitivity and the adjustable surface plasma body resonant vibration system of dynamic range.This system can be directed against various testing samples, under the prerequisite that guarantees dynamic range, carries out the high-sensitivity detection analysis; And this system does not have mechanical moving-member, and system stability is high.
The surface plasma body resonant vibration system that sensitivity provided by the present invention and dynamic range are adjustable is made up of the adjustable surface plasma body resonant vibration coupling unit of refractive index, broadband polychromatic source, incident beam shaping unit and reflected light detecting unit; Wherein, the adjustable surface plasma body resonant vibration coupling unit of said refractive index comprises the adjustable fluid prism of a refractive index, is positioned at the sensing chip on the said fluid prism and is positioned at the sample flow cell on the said sensing chip; Said sensing chip comprises an optical clear substrate and on it sensing membrane of position, and said optical clear substrate contacts with fluid media (medium) in the said fluid prism, and said sensing membrane constitutes a bottom surface of said sample flow cell.
The light that said incident beam shaping unit sends the broadband polychromatic source is shaped as adjustable p polarization parallel light of bulk or the little angle of p polarization converging beam, is incident in sensing chip through the fluid prism; Said reflected light detecting unit is used to resolve the catoptrical spectrum through the fluid prism.
Among the present invention, the fluid prism in the surface plasma body resonant vibration coupling unit that said refractive index is adjustable is made up of cavity and the fluid media (medium) that is positioned at the chamber; The cavity of wherein said fluid prism is provided with two apertures and a macropore, and two apertures are used separately as the input and the delivery outlet of said fluid media (medium), and macropore is as the installing port of said sensing chip, so that sensing chip directly contacts with fluid media (medium).
The cavity of said fluid prism can be half round post, semisphere, triangle etc., or other scalable shape etc.This cavity can be processed by optically transparent glass, quartz, silicon, plastic or other material.
Fluid media (medium) in the said fluid prism can be various pure or the liquid, the gases that mix such as optically transparent water, oil, ionic liquid, magnetic fluid, or supercritical fluid etc.; The refractive index of said fluid prism can be carried out continuous or discontinuous adjusting through the displacement fluid medium or through pressure, temperature, electric field, magnetic field, electromagnetic wave etc.
Said sensing chip comprises an optical clear substrate and preparation sensing membrane on it, can carry out functionalized modification to sensing membrane as required; Said optical clear substrate can be glass, quartz, silicon, plastics etc.; Said sensing membrane is the material that surface plasma body resonant vibration can take place gold, silver etc.
Optical clear substrate in the said sensing chip directly contacts with fluid media (medium) in the said fluid prism, and the sensing membrane in the said sensing chip directly contacts with sample.
Said incident beam shaping unit is made up of optical alignment element, linear polarizer, adjustable diaphragm, lens etc.
Said reflected light detecting unit is made up of signal collection element and spectrum resolution device; Said spectrum resolution device can be that monochromator cooperates photo-electric conversion element or linear array photo-electric conversion elements such as spectrograph cooperation photodiode, charge-coupled device (CCD) such as photodiode, photoelectric cell, photomultiplier; Said signal collection element and spectrum resolution device can directly be coupled or be coupled through optical fiber.
The light that said incident beam shaping unit sends the broadband polychromatic source is shaped as adjustable p polarization parallel light of bulk or little angle converging beam; Optical clear substrate through fluid prism, sensing chip; Focus on optical clear substrate and sensing membrane interface and receive to press down attenuated total internal reflection; Reflected light carries out spectrum resolution through optical clear substrate, the fluid prism of sensing chip by the reflected light detecting unit, obtains wavelength resonances surface plasma body resonant vibration curve.
The refractive index of said fluid prism is under the condition that surface plasma body resonant vibration can take place, and refractive index is low more, and detection sensitivity is high more, and dynamic range is narrow more; And refractive index is high more, and detection sensitivity is low more, and dynamic range is wide more.
Another object of the present invention is to provide a kind of method of utilizing above-mentioned sensitivity and the adjustable surface plasma body resonant vibration system of dynamic range to detect testing sample.
This method comprises the steps: 1) select to realize the refractive index of the fluid prism of surface plasma body resonant vibration according to the refractive index of testing sample; 2) testing sample is joined among the claim 1-7 in the sample flow cell of each described surface plasma body resonant vibration system; 3) utilize among the claim 1-7 each described surface plasma body resonant vibration system to detect, obtain wavelength resonances surface plasma body resonant vibration curve.
According to the refractive index (given value or estimated value) of testing sample, selection can realize the minimum fluid prismatic refraction rate of surface plasma body resonant vibration, and can obtain maximum sensitivity this moment; According to the maximum refractive index (given value or estimated value) of testing sample group, selection can realize the minimum fluid prismatic refraction rate of surface plasma body resonant vibration, and can obtain maximum sensitivity this moment under the prerequisite that guarantees dynamic range; For unknown sample or the transactional analysis that is difficult to estimate, can select suitable fluid prismatic refraction rate through preliminary experiment.
The surface plasma body resonant vibration system that sensitivity provided by the present invention and dynamic range are adjustable; Be based on flexible, the continuous or discontinuous adjustable fluid prism of a refractive index; It can be directed against various testing samples, under the prerequisite that guarantees dynamic range, carries out the high-sensitivity detection analysis.No mechanical moving-member in the surface plasma body resonant vibration of the present invention system, system stability is high, can be used for the analysis of various samples, is particularly useful for the sample analysis that sensitivity is had relatively high expectations.The present invention is equally applicable to the sensitivity and the dynamic range adjustment of surface plasma resonance image-forming.
Description of drawings
Fig. 1 is the general structure synoptic diagram of the adjustable surface plasma body resonant vibration system of sensitivity of the present invention and dynamic range.
Fig. 2 is the vertical view of fluid prism in the adjustable surface plasma body resonant vibration system of sensitivity of the present invention and dynamic range.
Fig. 3 is the light path synoptic diagram of the incident beam shaping unit of the adjustable surface plasma body resonant vibration system of sensitivity of the present invention and dynamic range.
Fig. 4 is the light path synoptic diagram of the reflected light detecting unit of the adjustable surface plasma body resonant vibration system of sensitivity of the present invention and dynamic range.
Fig. 5 is 1.4502 experimental analysis figure for the fluid prismatic refraction rate that adopts the adjustable surface plasma body resonant vibration system of sensitivity of the present invention and dynamic range.
Fig. 6 is 1.5174 experimental analysis figure for the fluid prismatic refraction rate that adopts the adjustable surface plasma body resonant vibration system of sensitivity of the present invention and dynamic range.
Fig. 7 is the sample segment enlarged drawing of 1.5174 experimental analysis figure for the fluid prismatic refraction rate that adopts the adjustable surface plasma body resonant vibration system of sensitivity of the present invention and dynamic range.
Embodiment
Below in conjunction with accompanying drawing and exemplary embodiments, describe the present invention.Following examples only are used to explain the present invention, but are not used for limiting scope of the present invention.
The general structure synoptic diagram of surface plasma body resonant vibration provided by the invention system is as shown in Figure 1.It comprises broadband polychromatic source and incident beam shaping unit 1, surface plasma body resonant vibration coupling unit 2 and reflected light detecting unit 3 that refractive index is adjustable.
Wherein, the adjustable surface plasma body resonant vibration coupling unit 2 of said refractive index comprises the adjustable fluid prism 4 of a refractive index, is positioned at sensing chip 6 on the fluid 5, is positioned at the sample flow cell 7 on the sensing chip 6; Said broadband polychromatic source and the little angle of incident beam shaping unit 1 output broadband polychrome p polarization converging beam 8, said converging beam 8 is incident in sensing chip 6 through fluid prism 4; Said reflected light detecting unit 3 is used to resolve the spectrum through the reflected light 9 of fluid prism 4.
Said fluid prism 4 has half-cylindrical cavity 10 and is contained in the fluid media (medium) 5 in the cavity.On the cavity 10 of half-cylindrical fluid prism, have 11,12 and macropores 13 of two apertures (like Fig. 1, shown in 2), two apertures 11,12 are used separately as the input port and the delivery outlet of said fluid media (medium), and a macropore 13 is used for the mounting hole of sensing chip 6; The refractive index of said fluid prism 4 can be regulated through changing fluid media (medium) 5.In the present embodiment, the cavity of fluid prism 4 is processed by the K9 glass material, and fluid media (medium) 5 is the mixed solution of cedar oil and isopropyl alcohol, can be through the refractive index of the continuous regulated fluid prism 4 of ratio of cedar oil and isopropyl alcohol in the adjusting mixed solution.
Said sensing chip 6 comprises an optical clear substrate 14 and preparation sensing membrane 15 on it.In the present embodiment, optical clear substrate 14 is the K9 glass sheet of a thickness 0.15mm, and sensing membrane is the golden film of thickness 50nm.Sensing chip 6 is realized sealing at macropore 13 places and the fluid prism 4 of fluid prism 4 through pressure through dimethyl silicone polymer (PDMS) elastomeric pad 16.The optical clear substrate 14 of sensing chip 6 directly contacts with fluid media (medium) 5 in the fluid prism 4, and sensing membrane 15 directly contacts with sample 17.
Said sample flow cell 7 is that a K9 glass sheet 18 is realized sealing through PDMS pad 19 and sensing chip 6 through pressure; On K9 glass sheet 18, have two apertures 20,21, import and delivery outlet as the sample of sample flow cell respectively.
Said broadband polychromatic source and incident beam shaping unit 1 are as shown in Figure 3, are made up of broadband polychromatic source 22, optical alignment element 23, linear polarizer 24, adjustable diaphragm 25, long burnt optical lens 26.In the present embodiment, broadband polychromatic source 22 is an iodine-tungsten lamp, and the light that sends by optical lens 30 collimations, for improving the collimation effect, is placed an aperture 29 in the focusing along after two optical lenses 27,28 focus on; The collimation directional light through linear polarizer 24, adjustable diaphragm 25, long burnt optical lens 26, obtains the little angle of p polarization converging beam 8 more at last.Converging beam 8 is through 4 incidents of fluid prism and focus on the optical clear substrate 14 of sensing chip 6 and the interface of sensing membrane 15.
Said reflected light detecting unit 3 is made up of as signal collection element and spectrum resolution device 33 optical lens 31; In the present embodiment, reflected light 9 focuses on through optical collection lens 31 and is coupled in optical fiber 32, carries out spectrum resolution by spectrum resolution device 33 independently.Spectrum resolution device 33 is to be detected by photomultiplier behind the monochromator splitting.
The little angle of the broadband polychrome p polarization converging beam 8 of said broadband polychromatic source and 1 output of incident beam shaping unit; Optical clear substrate 14 through fluid prism 4, sensing chip; Receive but attenuated total internal reflection at the interface of optical clear substrate 14 with sensing membrane 15; Reflected light 9 carries out spectrum resolution through optical clear substrate 14, the fluid prism 4 of sensing chip by reflected light detecting unit 3, obtains wavelength resonances surface plasma body resonant vibration curve.In the present embodiment, the incident direction of incident light is fixed, and angle is about 73 degree between the normal of sensing chip.
A kind of sensitivity and the adjustable surface plasma body resonant vibration system of dynamic range that adopt present embodiment to set up are sample with the aqueous sucrose solution of various concentration, have carried out experimental analysis.
At first sucrose concentration is respectively 0% (refractive index n
0%=1.3330), 1% (refractive index n
1%=1.3342) 2 samples; Selecting refractive index for use is 1.4502 cedar oil aqueous isopropanol (mass ratio of cedar oil and isopropyl alcohol is 1.28: the 1) fluid media (medium) as the fluid prism; Carried out high-sensitivity surface plasma resonance analysis (as shown in Figure 5), corresponding surface plasma body resonant vibration wavelength is respectively λ
0%=776.60nm, λ
1%=792.30nm, the calculating wavelength sensitivity is (λ
1%-λ
0%)/(n
1%-n
0%)=13083.3nm/RIU; Then the fluid media (medium) of fluid prism being changed to refractive index is 1.5174 cedar oil, and sucrose concentration is respectively 0% (refractive index n
0%=1.3330), 1% (refractive index n
1%=1.3342), 5% (refractive index n
5%=1.3401), 13% (refractive index n
13%=1.3529), 18% (refractive index n
18%=1.3605) 5 samples have carried out surface plasma body resonant vibration analysis (like Fig. 6, shown in 7), and corresponding surface plasma body resonant vibration wavelength is respectively λ
0%=593.44nm, λ
1%=595.62nm, λ
5%=603.03nm, λ
13%=623.48nm, λ
18%=637.58nm, it is 1816.7nm/RIU that 2 samples by 0% and 1% calculate wavelength sensitivity.Can find out that by analysis result the refractive index of fluid prism is that 1.4502 o'clock sensitivity is that the refractive index of fluid prism is 1.5174 o'clock 7 times, and dynamic range narrows down.Thus, only pass through the refractive index of the fluid media (medium) of regulated fluid prism, promptly can carry out the optimization of sensitivity and dynamic range to testing sample.Because the refractive index of fluid media (medium) can be regulated through the concentration ratio of mixed solution continuously, so can guarantee to carry out the high-sensitivity detection analysis under the condition that dynamic range is met.
Said embodiment has adopted half-cylindrical fluid prism, also can adopt other shapes such as triangle.
Said embodiment has adopted monochromator to carry out the spectrum unscrambling analysis by the optical fiber coupling, also can adopt spectrograph through spectrum unscrambling analytical equipments such as CCD, also can directly analyze without the optical fiber coupling.
Described embodiment has set up a kind of sensitivity and the adjustable surface plasma body resonant vibration system of dynamic range, and the present invention is equally applicable to the sensitivity and the dynamic range adjustment of surface plasma resonance image-forming.
Claims (8)
1. sensitivity and the adjustable surface plasma body resonant vibration system of dynamic range are made up of the adjustable surface plasma body resonant vibration coupling unit of refractive index, broadband polychromatic source, incident beam shaping unit and reflected light detecting unit; Wherein, the adjustable surface plasma body resonant vibration coupling unit of said refractive index comprises the adjustable fluid prism of a refractive index, is positioned at the sensing chip on the said fluid prism and is positioned at the sample flow cell on the said sensing chip; Said sensing chip comprises an optical clear substrate and on it sensing membrane of position, and said optical clear substrate contacts with fluid media (medium) in the said fluid prism, and said sensing membrane constitutes a bottom surface of said sample flow cell.
2. surface plasma body resonant vibration according to claim 1 system is characterized in that: said fluid prism is made up of cavity and the fluid media (medium) that is positioned at the chamber; The cavity of wherein said fluid prism is provided with two apertures and a macropore, and two apertures are respectively as the input port and the delivery outlet of said fluid media (medium), and macropore is as the installing port of said sensing chip.
3. surface plasma body resonant vibration according to claim 2 system, it is characterized in that: the cavity of said fluid prism is processed by optically transparent material;
The fluid media (medium) of said fluid prism is optically transparent liquid, gas or supercritical fluid.
4. according to each described surface plasma body resonant vibration system among the claim 1-3, it is characterized in that: the material that surface plasma body resonant vibration can take place of serving as reasons of the sensing membrane in the said sensing chip is processed.
5. according to each described surface plasma body resonant vibration system among the claim 1-4; It is characterized in that: the light that said incident beam shaping unit sends the broadband polychromatic source is shaped as adjustable p polarization parallel light of bulk or the little angle of p polarization converging beam, is incident in sensing chip through said fluid prism.
6. according to each described surface plasma body resonant vibration system among the claim 1-5, it is characterized in that: said incident beam shaping unit comprises optical alignment element, linear polarizer, adjustable diaphragm and lens.
7. according to each described surface plasma body resonant vibration system among the claim 1-6, it is characterized in that: said reflected light detecting unit is made up of signal collection element and spectrum resolution device; Said spectrum resolution device is the spectrograph that is equipped with the monochromator of photo-electric conversion element or is equipped with the linear array photo-electric conversion element; Said signal collection element and spectrum resolution device directly are coupled or are coupled through optical fiber.
8. a method of utilizing among the claim 1-7 each described surface plasma body resonant vibration system to detect comprises the steps:
1) selects to realize the refractive index of the fluid prism of surface plasma body resonant vibration according to the refractive index of testing sample;
2) testing sample is joined among the claim 1-7 in the sample flow cell of each described surface plasma body resonant vibration system;
3) utilize among the claim 1-7 each described surface plasma body resonant vibration system to detect, obtain wavelength resonances surface plasma body resonant vibration curve.
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| CN103698304A (en) * | 2014-01-15 | 2014-04-02 | 中国科学院化学研究所 | Shear type liquid core coupled surface plasma resonance imaging analyzer |
| CN103698306A (en) * | 2014-01-15 | 2014-04-02 | 中国科学院化学研究所 | Liquid core coupling surface plasma resonance imaging analyzer |
| CN103728280A (en) * | 2014-01-15 | 2014-04-16 | 中国科学院化学研究所 | Surface plasma resonance coupling optical element |
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| CN104237169A (en) * | 2013-06-07 | 2014-12-24 | 国家纳米科学中心 | Detection method of SPR detection system based on external field modulation |
| CN103698304A (en) * | 2014-01-15 | 2014-04-02 | 中国科学院化学研究所 | Shear type liquid core coupled surface plasma resonance imaging analyzer |
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| CN108680558A (en) * | 2018-08-09 | 2018-10-19 | 江苏师范大学 | Optical path converter, micro Raman spectra test system, water pollution detecting system |
| CN108919393A (en) * | 2018-08-09 | 2018-11-30 | 江苏师范大学 | A kind of easy-operating optical path converter |
| CN108919393B (en) * | 2018-08-09 | 2020-12-08 | 江苏师范大学 | Light path converter easy to operate |
| CN110174374A (en) * | 2019-06-28 | 2019-08-27 | 湖南师范大学 | A kind of SPR index sensor of infrared band |
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| CN113777079A (en) * | 2021-09-09 | 2021-12-10 | 北京化工大学 | Integrated surface plasma resonance chip and preparation method thereof |
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| CN116026760B (en) * | 2022-11-23 | 2023-10-31 | 广东工业大学 | Wavelength type SPR sensing system and method |
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