CN117470806B - Polymer glucose sensor based on Mach-Zehnder structure - Google Patents
Polymer glucose sensor based on Mach-Zehnder structure Download PDFInfo
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- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 title claims abstract description 140
- 239000008103 glucose Substances 0.000 title claims abstract description 140
- 229920000642 polymer Polymers 0.000 title claims abstract description 67
- 230000003287 optical effect Effects 0.000 claims abstract description 52
- 230000035945 sensitivity Effects 0.000 claims abstract description 25
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 24
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 24
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 24
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims abstract description 23
- 238000005253 cladding Methods 0.000 claims abstract description 22
- 239000012792 core layer Substances 0.000 claims abstract description 18
- 239000010410 layer Substances 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000007822 coupling agent Substances 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 34
- 230000004044 response Effects 0.000 claims description 25
- 238000005452 bending Methods 0.000 claims description 23
- 239000007853 buffer solution Substances 0.000 claims description 8
- 238000001514 detection method Methods 0.000 claims description 8
- 108090000790 Enzymes Proteins 0.000 claims description 4
- 102000004190 Enzymes Human genes 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 4
- 230000008033 biological extinction Effects 0.000 claims description 4
- 238000010168 coupling process Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 229910000077 silane Inorganic materials 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- 230000008878 coupling Effects 0.000 claims description 3
- 238000005859 coupling reaction Methods 0.000 claims description 3
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 claims description 2
- NQTADLQHYWFPDB-UHFFFAOYSA-N N-Hydroxysuccinimide Chemical compound ON1C(=O)CCC1=O NQTADLQHYWFPDB-UHFFFAOYSA-N 0.000 claims description 2
- 239000003431 cross linking reagent Substances 0.000 claims description 2
- 238000005530 etching Methods 0.000 claims description 2
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 239000002861 polymer material Substances 0.000 claims description 2
- 238000006557 surface reaction Methods 0.000 claims description 2
- 230000008859 change Effects 0.000 abstract description 21
- 238000005259 measurement Methods 0.000 description 15
- 238000010586 diagram Methods 0.000 description 7
- 238000000691 measurement method Methods 0.000 description 5
- 230000001808 coupling effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 229940088598 enzyme Drugs 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000000872 buffer Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000013307 optical fiber Substances 0.000 description 2
- 239000011295 pitch Substances 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 229920002307 Dextran Polymers 0.000 description 1
- 108010015776 Glucose oxidase Proteins 0.000 description 1
- 239000004366 Glucose oxidase Substances 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000020940 control diet Nutrition 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000035558 fertility Effects 0.000 description 1
- 229940116332 glucose oxidase Drugs 0.000 description 1
- 235000019420 glucose oxidase Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000002444 silanisation Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
- G01N21/45—Refractivity; Phase-affecting properties, e.g. optical path length using interferometric methods; using Schlieren methods
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/24—Coupling light guides
- G02B6/26—Optical coupling means
- G02B6/28—Optical coupling means having data bus means, i.e. plural waveguides interconnected and providing an inherently bidirectional system by mixing and splitting signals
- G02B6/2804—Optical coupling means having data bus means, i.e. plural waveguides interconnected and providing an inherently bidirectional system by mixing and splitting signals forming multipart couplers without wavelength selective elements, e.g. "T" couplers, star couplers
- G02B6/2808—Optical coupling means having data bus means, i.e. plural waveguides interconnected and providing an inherently bidirectional system by mixing and splitting signals forming multipart couplers without wavelength selective elements, e.g. "T" couplers, star couplers using a mixing element which evenly distributes an input signal over a number of outputs
- G02B6/2813—Optical coupling means having data bus means, i.e. plural waveguides interconnected and providing an inherently bidirectional system by mixing and splitting signals forming multipart couplers without wavelength selective elements, e.g. "T" couplers, star couplers using a mixing element which evenly distributes an input signal over a number of outputs based on multimode interference effect, i.e. self-imaging
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
- G01N21/45—Refractivity; Phase-affecting properties, e.g. optical path length using interferometric methods; using Schlieren methods
- G01N2021/458—Refractivity; Phase-affecting properties, e.g. optical path length using interferometric methods; using Schlieren methods using interferential sensor, e.g. sensor fibre, possibly on optical waveguide
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Optics & Photonics (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a polymer glucose sensor based on a Mach-Zehnder structure, which comprises a PDMS lower cladding layer and a PMMA core layer arranged on the PDMS lower cladding layer, wherein the PMMA core layer is a Mach-Zehnder structure pattern, and GOD is fixed on a sensing arm of the PMMA core layer through an acid coupling agent to form three-dimensional rectangular contact. The polymer glucose sensor provided by the invention can sense glucose in a large concentration range by measuring the change of output optical power without external modulation means such as electro-optical, thermo-optical and the like, and has the characteristics of simple and compact device structure, high sensitivity and the like without a longer sensing arm and a complex microfluidic chip.
Description
Technical Field
The invention relates to a glucose sensor device, in particular to a polymer glucose sensor based on a Mach-Zehnder structure, which can be used for measuring the concentration of glucose in a large range.
Background
A glucose sensor is an instrument for measuring the glucose concentration in an environment that can help people understand the glucose concentration in an environment to better control diet and lifestyle. Compared with the traditional measuring method, the glucose sensor has the advantages of high response speed, high sensitivity, good stability and the like, and is widely applied to the fields of food safety, biotechnology, medical detection and the like. For example, in food processing and manufacturing, glucose sensors may be used to detect glucose content in food products to ensure the quality and safety of the food products; in the agricultural field, glucose sensors can be used to detect glucose content in soil to assess soil fertility and crop growth; in addition, in environmental monitoring, glucose sensors can also be used to detect glucose content in a body of water to assess the pollution level of the body of water and the health of the ecological environment.
Glucose monitoring instruments can be classified into wavelength measurement methods and light intensity measurement methods according to sensing measurement methods. Wavelength measurement is based on the absorption or reflection spectral characteristics of a glucose solution at a specific wavelength to determine its concentration, which requires not only the use of complex optical elements such as filters, gratings or interferometers, but also the incorporation of accurate wavelength measurement equipment to achieve accurate measurements, which greatly increases the complexity and cost of the system. Wavelength measurement methods may have small wavelength shifts at certain concentrations, and thus sensitivity is susceptible to spectrometer measurement accuracy. The light intensity measuring method is a method for measuring the intensity change of the output light power, and the measuring scheme does not need a spectrometer, so that the measuring cost is greatly reduced. Some of the currently reported sensors based on the light intensity detection method have the defects of limited sensitivity, complex structure, insufficient compactness in structure, high requirements on light sources and the like, and have certain defects on the interaction of a fast-response substance to be detected and the sensor and a wider dynamic range.
Therefore, how to explore an optical glucose measurement method and obtain a glucose sensor with high sensitivity, high linearity, high stability and low detection limit detection on the premise of measuring glucose concentration with high precision is a technical problem to be solved in the field.
Term interpretation: PDMS: polydimethyl siloxane; PMMA: polymethyl methacrylate; GOD: glucose oxidase; MMI: a multimode interference coupler; PBS: phosphate.
Disclosure of Invention
The invention aims to provide a polymer glucose sensor based on a Mach-Zehnder structure, which has the advantages of high sensitivity, good linearity, strong stability, easiness in integration and capability of effectively measuring a large range of glucose concentration.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the invention provides a polymer glucose sensor based on a Mach-Zehnder structure, which comprises a PDMS lower cladding layer, a PMMA core layer and a PDMS upper cladding layer from bottom to top; the PMMA core layer comprises an input waveguide, an output waveguide, a 1×2MMI coupler, a 2×1MMI coupler, a curved waveguide, a sensing arm and a reference arm; the sensing arm and the reference arm are equal in length and parallel, and are symmetrically arranged by taking the central line as an axis; fixing GOD on a sensing arm of the PMMA core layer through an acid coupling agent at the temperature of 40 ℃ to form a three-dimensional rectangular contact structure, wherein the upper surface of the three-dimensional rectangular contact structure is lower than the upper surface of the PDMS upper cladding layer and higher than the upper surface of the sensing arm;
the refractive index change range of the GOD is 1.3352-1.3400, the arm length of the sensing arm is 1740 mu m, and the arm distance between the sensing arm and the reference arm is 130 mu m; the bending radius of the bending waveguide is 800 mu m, the transverse length of the bending waveguide is 430 mu m, and the deflection angle of the bending waveguide is 0.28rad;
the loss of the polymer glucose sensor based on the Mach-Zehnder structure is controlled within 1.6dB, and the sensitivity is 2.67 mW/(mg/mL).
Preferably, the loss of the polymer glucose sensor based on the Mach-Zehnder structure is 1.58dB, and the extinction ratio is 41.43dB.
When the input optical power is 10mW and the glucose solution concentration is 0mg/mL, the maximum output optical power is 6.95mW, and when the glucose solution concentration is 2.6mg/mL, the minimum output optical power is 0.0005mW, the sensor realizes linear response of the glucose concentration in the range of 0-2.6mg/mL, and the glucose concentration sensing range is 0-2.6mg/mL.
The relative standard deviation of the polymer glucose sensor based on the Mach-Zehnder structure is (1.5-2.5) multiplied by 10 -3 The minimum detection limit was 0.1mg/mL.
The thickness of the PDMS lower cladding and the thickness of the PDMS upper cladding are 10 mu m, and the refractive index is 1.4040; the thickness of the PMMA core layer is 1 mu m, and the refractive index is 1.4880; the distance from the upper surface of the sensing arm to the upper surface of the three-dimensional rectangular contact structure is 2-3 mu m.
Preferably, the waveguide width of the curved waveguide is 1.5 μm and the height is 1 μm.
The GOD solution was obtained in the following manner: dissolving GOD powder in PBS buffer solution with pH of 5.5 to form GOD solution with mass concentration of 30 mg/mL;
and (3) dropwise adding GOD solution on the sensing arm of the PMMA core layer, and curing to form a three-dimensional rectangular contact structure on the sensing arm.
Compared with the prior art, the invention has the beneficial effects that:
1. the input optical power of the polymer glucose sensor based on the Mach-Zehnder structure is 10mW, and the output optical power of the polymer glucose sensor is changed between 0.0005mW and 6.9500mW when the concentration of a glucose solution is 0mg/mL to 2.6mg/mL. The arm length of the sensing arm is 1740 mu m, the size of the device is greatly reduced, the structure is simple and compact, and the measurement of the concentration of the glucose solution in a large range can be realized without a long sensing arm and a complex microfluidic chip.
2. In the preparation of the glucose sensor, the GOD can be kept at the optimal activity by controlling the temperature of the GOD to 40 ℃ and the pH to 5.5, so that the output optical power of the polymer glucose sensor with the Mach-Zehnder structure reaches the maximum value, the sensitivity is 2.67 mW/(mg/mL), the loss is controlled within 1.6dB, and the glucose sensor has high stability (the relative standard deviation is about (1.5-2.5) multiplied by 10) -3 ) Low detection limit (0.1 mg/mL).
Drawings
FIG. 1 is a schematic diagram of a polymeric glucose sensor based on a Mach-Zehnder structure of the present invention;
FIG. 2 is a schematic diagram of a curved waveguide structure and parameters of a polymer glucose sensor based on a Mach-Zehnder structure of the present invention; wherein (a) is an influence graph of the transverse length on the output light power variation under different deflection angles; (b) Is a graph of the influence of the bending radius on the variation of the output optical power at a deflection angle of 0.28rad;
FIG. 3 is a graph of the output optical power versus different arm spacing for a polymer glucose sensor based on a Mach-Zehnder structure of the present invention; wherein (a) is the arm spacing (left graph) and the corresponding output light power condition (right graph) when the coupling effect occurs between the reference arm and the sensing arm; (b) The distance between the reference arm and the sensing arm when no coupling effect occurs (left graph) and the corresponding output light power condition (right graph); (c) A comparison chart of the change condition of output light power along with the refractive index under different arm pitches;
FIG. 4 is a graph showing the comparison of the output optical power response of the polymer glucose sensor of the present invention at different sensor arm lengths based on Mach-Zehnder structures;
FIG. 5 is a graph of the optical field of a polymeric glucose sensor based on a Mach-Zehnder structure of the present invention;
FIG. 6 is a schematic diagram of a measurement system of a polymer glucose sensor based on a Mach-Zehnder structure of the present invention;
FIG. 7 is a graph showing the response of the variation in output optical power of a polymer glucose sensor based on Mach-Zehnder structures obtained at different temperatures and pH; wherein (a) is an influence diagram of different temperatures on output optical power; (b) is an influence graph of different pH values on output optical power;
FIG. 8 is a graph showing the response of the output optical power of the polymer glucose sensor according to the present invention based on Mach-Zehnder structure as a function of glucose concentration;
FIG. 9 is a graph of the specific response of a polymer glucose sensor based on a Mach-Zehnder structure of the present invention;
FIG. 10 is a graph of the stability response of a polymer glucose sensor based on a Mach-Zehnder structure of the present invention;
FIG. 11 is a graph of the durability response of a polymer glucose sensor based on a Mach-Zehnder structure of the present invention; wherein (a) is a graph of the output optical power of the same polymer glucose sensor at different times and different glucose concentrations; (b) The sensitivity and loss of the same polymer glucose sensor at different times and different glucose concentrations are compared with each other;
reference numerals:
1. PDMS lower cladding, 2, PMMA core, 3, PDMS upper cladding, 4, 1×2MMI coupler, 5, 2×1MMI coupler, 6, curved waveguide, 7, sensor arm, 8, reference arm, 9, input waveguide, 10, output waveguide, 11, centerline.
Detailed Description
The technical scheme of the invention is described in detail below with reference to the accompanying drawings and specific embodiments.
The described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be obtained by persons skilled in the art without making any creative effort, based on the embodiments of the present invention are included in the protection scope of the present invention, and the embodiments described below by referring to the drawings are exemplary only for explaining the technical scheme of the present invention and should not be construed as limiting the present invention.
The structure of the polymer glucose sensor based on the mach-zehnder structure (referred to as polymer glucose sensor for short) of this embodiment is shown in fig. 1. Comprises a PDMS lower cladding layer 1, a PMMA core layer 2 and a PDMS upper cladding layer 3 from bottom to top. The PMMA core layer 2 comprises an input waveguide 9, an output waveguide 10, a 1×2MMI coupler 4, a 2×1MMI coupler 5, a curved waveguide 6, a sensing arm 7 and a reference arm 8, wherein the sensing arm 7 and the reference arm 8 are arranged in an axisymmetric way by taking a central line 11 as an axis, the PDMS upper cladding 3 is etched near the area where the sensing arm 7 is positioned, all the upper, left and right sides of the sensing arm 7 are exposed, GOD is filled in the etched area and is fixed on the sensing arm 7 of the PMMA core layer 2 through an acid coupling agent, a three-dimensional rectangular contact structure is formed, and the upper surface of the three-dimensional rectangular contact structure is lower than the upper surface of the PDMS upper cladding 3 and higher than the upper surface of the sensing arm 7.
In the embodiment, the thickness of the PDMS lower cladding and the thickness of the PDMS upper cladding are both 10 mu m, and the refractive index is 1.4040; the thickness of the PMMA core layer is 1 mu m, and the refractive index is 1.4880; the distance from the upper surface of the sensing arm to the upper surface of the three-dimensional rectangular contact structure is 2-3 mu m.
The curved waveguide structure and parameters of the polymer glucose sensor based on the mach-zehnder structure of this embodiment are shown in fig. 2. When the bending waveguide 6 is selected, a rectangular waveguide with the waveguide width of 1.5 mu m and the waveguide height of 1 mu m is selected to be coupled and butted with the 1X 2MMI coupler 4 at the front end. The bending radius, the lateral length and the deflection angle of the bending waveguide 6 are three important factors which have a great influence on the optical loss, and the graph (a) in fig. 2 shows the influence of the lateral length on the output optical power variation under different deflection angles, and the output optical power loss is smaller and more stable under the deflection angle of 0.28 rad. Fig. 2 (b) shows the effect of the bending radius on the output optical power variation at a deflection angle of 0.28rad, and the output optical power loss is minimum and stable at a deflection angle of 0.28rad and a transverse length of 430 μm and a bending radius of 800 μm. The invention selects the bending radius of the bending waveguide 6 to be 800 mu m, the transverse length to be 430 mu m and the deflection angle to be 0.28rad after comprehensive consideration, at this time, the waveguide loss of the bending waveguide 6 reaches a minimum value, and the normalized output light power is 0.96a.u..
The comparison of the output optical power of different arm pitches of the polymer glucose sensor based on the Mach-Zehnder structure in the embodiment is shown in fig. 3. Too close an arm spacing of the sensor arm 7 and the reference arm 8 can lead to coupling effects (the energy input to the left waveguide is gradually coupled into the right waveguide with increasing propagation distance) and can also affect the sensing performance of the sensor. When the arm spacing is not more than 4 mu m, as can be seen from the graph (a) in fig. 3, the arm spacing is too close, and the sensing performance of the sensor is seriously affected; considering the combined action of the bending radius, the transverse length and the deflection angle of the bending waveguide 6 and the arm spacing, it is determined that when the arm spacing is 130 mu m, the coupling effect between the waveguides is not generated between the sensing arm 7 and the reference arm 8, as shown in the graph (b) of fig. 3, the output optical power can reach the maximum value, and the device loss is minimum at this time, as shown in the graph (c) of fig. 3.
Sensitivity of the Mach-Zehnder structure-based polymer glucose sensorSCan be expressed as:
，
in the middle ofλAs a function of the wavelength(s),Lin order to sense the arm length of the arm,n c for the refractive index of the liquid to be measured,N eff for the effective refractive index of the sensor arm,is the change relation of the effective refractive index of the sensing arm along with the concentration of glucose. From the analysis of the formula, it can be seen that not only the effective refractive index of the sensor armN eff Can affect the sensitivity of the glucose sensor and the arm length of the sensing armLThe sensitivity of the sensor can be influenced, and meanwhile, the transmission power analysis of the polymer glucose sensor with the refractive index and Mach-Zehnder structure is combined, so that the sensing sensitivity of the sensor can be improved by increasing the evanescent field range of the optical field in contact with the object to be measured. Polymer glucose for light intensity Mach-Zehnder structureThe sensor, the light intensity of which repeatedly appears twice in a change period, thus only consider the light intensity response change of 1/2 period.
After specific catalytic glucose reaction, the refractive index of GOD is reduced, and after catalytic reaction with enzyme, the refractive index of glucose solution with different concentrations is also reduced. In addition, the sensitivity and the sensing range of the polymer glucose sensor having the mach-zehnder structure are a pair of mutually restricted amounts. In the embodiment, the refractive index change range of GOD is 1.3352-1.3400, the arm length of the sensing arm 7 is 1740 mu m, if the arm length continues to be increased, the detected glucose concentration range is reduced, and in the interval of the refractive index change range of GOD of 1.3352-1.3400, the output light power is not monotonous; also, if the arm length is increased again, this will lead to a decrease in the sensitivity of the detected glucose, and when the sensing arm 7 is a rectangular waveguide structure with three faces all contacting the object to be detected, the arm spacing is 130 μm, the bending radius of the bending waveguide 6 is 800 μm, the lateral length is 430 μm and the deflection angle is 0.28rad, which has a higher sensitivity and linearity over this refractive index interval, and the device is minimized while guaranteeing the maximum sensing range.
The comparison of the output optical power response of the polymer glucose sensor based on Mach-Zehnder structure at different arm lengths is shown in FIG. 4. When the refractive index variation range of GOD is in the interval 1.3352-1.3400, the difference of the output light power of the end points of the interval is maximum and monotonic in the interval, the sensitivity is maximum. Only when the arm length of the sensing arm 7 is 1740 mu m, the GOD refractive index variation range is in the interval 1.3352-1.3400, and the output optical power is monotonous in the interval; when the arm length of the sensing arm is smaller than 1740 mu m, the sensitivity of the GOD refractive index change range in the 1.3352-1.3400 interval is reduced, and the glucose detection requirement cannot be met.
The optical field diagram of the polymer glucose sensor based on the mach-zehnder structure of this embodiment is shown in fig. 5. When the arm length of the sensing arm 7 is 1740 mu m, and the sensing arm 7 is of a rectangular waveguide structure with three surfaces all contacting an object to be measured, under the conditions that the arm distance is 130 mu m, the bending radius of the bending waveguide 6 is 800 mu m, the transverse length is 430 mu m, and the deflection angle is 0.28rad, the light field is effectively limited in the PMMA core layer 2 area, and the extinction ratio of the glucose sensor is 41.43dB.
The measurement system of the polymer glucose sensor based on the mach-zehnder structure of this embodiment is shown in fig. 6. And the glucose solution is dripped into the polymer glucose sensor based on the Mach-Zehnder structure after GOD is modified by silanization coupling for sensing measurement, light with the wavelength of 1550nm emitted by the tunable laser passes through the polarization controller and is coupled and input into an input waveguide 9 of the polymer glucose sensor based on the Mach-Zehnder structure through a tapered optical fiber, the input light generates interference phenomenon through a sensing arm 7 and a reference arm 8, and the output waveguide 10 is coupled and output into an optical power meter through the tapered optical fiber, so that the relation between the concentration and the output optical power of the polymer glucose sensor based on the Mach-Zehnder structure is obtained.
In this embodiment, when the GOD is fixed, the temperature and pH at which the GOD is located need to be controlled, and the optimal activity of the GOD is maintained, and meanwhile, the performance of the polymer glucose sensor based on the Mach-Zehnder structure is optimized.
The embodiment adopts a covalent coupling method to realize simple, efficient and stable fixation of GOD. Firstly, carrying out surface functionalization modification on the surface of the sensing arm 7 by using a silane solution, and supporting a 'molecular bridge' between an interface of enzyme and a polymer material through silane; then, further coupling treatment is carried out on the surface of the sensor arm 7 by using a cross-linking agent formed by 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide;
and (3) dissolving GOD powder in PBS buffer solution with pH of 5.5 to form 30mg/mL GOD solution, placing the device after etching the PDMS upper cladding layer 3 in a high-low temperature test box, controlling the temperature to 40 ℃, dripping the GOD solution and solidifying, forming a three-dimensional rectangular contact structure on the sensing arm, and flushing the non-fixed GOD on the surface of the sensing arm 7 by the PBS buffer solution to finish the fixation of the GOD.
The response graphs of the output optical power variation amounts of the polymer glucose sensor based on the mach-zehnder structure obtained at different temperatures and pH in this example are shown in fig. 7. According to the invention, the temperature is controlled to be changed between 35 ℃ and 45 ℃ through a high-low temperature test box, and glucose solutions with the same concentration, the same volume and different temperatures are adopted for experiments, so that the change condition of an optical transmission characteristic curve corresponding to a polymer glucose sensor based on a Mach-Zehnder structure along with the temperature is analyzed. As shown in fig. 7 (a), when the temperature of the GOD is increased to 40 ℃, the specific catalytic reaction occurs most strongly on the surface of the sensor arm 7, and the effective refractive index of the sensor arm 7 changes most, so that the output optical power variation reaches the maximum; further increasing the temperature of the PBS buffer, the effective refractive index change of the sensor arm 7 will be reduced, and the output optical power change of the polymer glucose sensor based on the Mach-Zehnder structure is reduced.
The invention selects PBS buffer solution with pH=4.0 and pH=8.0 to mix with HCl and NaOH, controls the pH value to be in a certain range, measures the pH value by a pH meter, and then reduces the pH range at intervals of 0.5 and pH to find the optimal pH value. Glucose solutions of the same concentration, the same volume and different pH values were used for the dropwise addition measurement. The effect of the pH of the solution on the optical transmission characteristics is shown in fig. 7 (b), and when the pH of the PBS buffer is increased to 5.5, the active group on the GOD molecule is in a dissociated state, and after a specific catalytic reaction occurs on the surface of the sensor arm 7, the effective refractive index of the sensor arm 7 will change the most, so that the output optical power reaches the maximum change amount. Further improve the pH value of PBS buffer solution, the dissociation state of active group on GOD molecule is restrained, is unfavorable for enzyme and glucose to combine, and the change of effective refractive index of sensor arm 7 will reduce, and then leads to the output light power variation of polymer glucose sensor based on Mach-Zehnder structure to reduce.
In order to detect the sensing range and sensitivity of the polymer glucose sensor based on the Mach-Zehnder structure, glucose solutions of different concentrations of 0-3mg/mL are prepared, glucose solutions of different concentration gradients are respectively prepared at concentration changes of 0.1mg/mL concentration intervals, for example, glucose solutions of 1mg/mL concentration are prepared, 10mg of glucose powder is added into 10mL of PBS buffer solution with pH of 5.5, and the mixture is stirred uniformly by using a magnetic stirrer.
The present embodiment is based onA response plot of the output optical power of the polymer glucose sensor of mach-zehnder structure as a function of glucose concentration is shown in fig. 8. The glucose concentration sensing range of the polymer glucose sensor based on Mach-Zehnder structure was measured using 10mW of input optical power in experimental measurementC L And their ability to respond to different concentrations of glucose. To eliminate the interference caused by each different concentration of glucose solution, the sensor arm 7 needs to be rinsed with deionized water before each independent measurement. Fig. 8 shows the optical output characteristics of a polymer glucose sensor based on a mach-zehnder structure at different glucose concentrations, with the change in output optical power in the direction of decreasing power as the concentration of the glucose solution increases. The experimental results show that when the glucose solution concentration is 0mg/mL, the maximum output optical power is 6.95mW, and when the glucose solution concentration is 2.6mg/mL, the minimum output optical power is 0.0005mW, and the device realizes linear response within the glucose concentration range of 0-2.6mg/mL. The extinction ratio of the polymer glucose sensor based on the mach-zehnder structure was 41.43dB,C L 0-2.6mg/mL, sensitivity 2.67 mW/(mg/mL).
The specific response diagram of the polymer glucose sensor based on the mach-zehnder structure of this embodiment is shown in fig. 9. The intensity responses of the sensor to three different solutions (PBS, naCl and glucose) are compared, wherein the maximum output optical power response variation of the polymer glucose sensor based on the Mach-Zehnder structure to glucose is 6.95mW, the maximum output optical power response variation of the sensor to PBS and NaCl is 0.16mW and 0.11mW respectively, and the result shows that the GOD on the sensor arm 7 can specifically identify the glucose, so the polymer glucose sensor based on the Mach-Zehnder structure has good selectivity to the glucose.
The stability response diagram of the polymer glucose sensor based on the mach-zehnder structure of this embodiment is shown in fig. 10. Stability is another important performance indicator of polymer glucose sensors and is also an important indicator of the accuracy of the measurement. The stability of a polymer glucose sensor can be expressed as: under the same experimental environment (same concentration, temperature, pH and volume of dextran)Glucose solution) to the output optical power, and the fluctuation condition of the output optical power is characterized, the stability of the polymer glucose sensor based on the Mach-Zehnder structure can be measured by using the relative standard deviation. The glucose solutions with concentrations of 1mg/mL and 2mg/mL were repeatedly measured 10 times, and the measured results were recorded every 5 minutes, and the measured output light power was fluctuated with time as shown in FIG. 10, and the experimental results showed that although the output light power measured by the sensor fluctuated with time to varying degrees, it fluctuated within a very small range, and the relative standard deviation of the concentration single point measurement was about 2X 10 -3 Therefore, the polymer glucose sensor based on the Mach-Zehnder structure has better stability for measuring the concentration of glucose solution.
The durability response graph of the polymer glucose sensor based on the mach-zehnder structure of this embodiment is shown in fig. 11. Durability refers to the fact that the light intensity response to glucose solutions of different concentrations can maintain good consistency and accuracy, and excellent durability is a necessary precondition for long-term use of the sensor. The response test was performed on a polymer glucose sensor stored for different times in a room temperature environment, and the specific experimental procedure was as follows: after the same polymer glucose sensor was stored in a room temperature environment for 15 days and 40 days, respectively, it was measured using glucose solutions of different concentrations, and the optical output characteristic curves at different glucose concentrations at different times were as shown in fig. 11 (a), and the change trend was shown in accordance with the initial measurement results after 15 days and 40 days, with the output optical power significantly moving in a decreasing direction with increasing concentration, and the change rates after 15 days and 40 days were 2.2% and 3.2%, respectively. Meanwhile, two main performance parameters of sensitivity and loss are also examined, and it can be seen that after 15 days and 40 days, the measurement results are shown in a graph (b) in fig. 11, the loss and the sensitivity of the polymer glucose sensor based on the Mach-Zehnder structure are not obviously changed, the loss change range is 2.36-2.50dB, and the sensitivity change range is 2.67-2.53 mW/(mg/mL). Although the response intensity, loss and sensitivity of the device after being placed for a period of time are slightly reduced relative to the performance of the device when tested immediately after processing, the sensing interval of the glucose by the polymer glucose sensor based on the Mach-Zehnder structure is not changed obviously, which shows that the response of the polymer glucose sensor to glucose after being stored for different periods of time at room temperature still maintains high consistency.
The invention is applicable to the prior art where it is not described.
Claims (2)
1. A polymer glucose sensor based on Mach-Zehnder structure comprises a PDMS lower cladding layer, a PMMA core layer and a PDMS upper cladding layer from bottom to top; the PMMA core layer is characterized by comprising an input waveguide, an output waveguide, a 1×2MMI coupler, a 2×1MMI coupler, a curved waveguide, a sensing arm and a reference arm; the sensing arm and the reference arm are equal in length and parallel, and are symmetrically arranged by taking the central line as an axis; fixing GOD on a sensing arm of the PMMA core layer through an acid coupling agent at the temperature of 40 ℃ to form a three-dimensional rectangular contact structure, wherein the upper surface of the three-dimensional rectangular contact structure is lower than the upper surface of the PDMS upper cladding layer and higher than the upper surface of the sensing arm;
the refractive index variation range of the GOD is 1.3352-1.3400, the arm length of the sensing arm is 1740 mu m, and the arm distance between the sensing arm and the reference arm is 130 mu m; the bending radius of the bending waveguide is 800 mu m, the transverse length of the bending waveguide is 430 mu m, and the deflection angle of the bending waveguide is 0.28rad;
the loss of the polymer glucose sensor based on the Mach-Zehnder structure is controlled within 1.6dB, and the sensitivity is 2.67 mW/(mg/mL);
when the input optical power is 10mW and the glucose solution concentration is 0mg/mL, the maximum output optical power is 6.95mW, and when the glucose solution concentration is 2.6mg/mL, the minimum output optical power is 0.0005mW, the sensor realizes the linear response of the glucose concentration in the range of 0-2.6mg/mL, and the glucose concentration sensing range is 0-2.6mg/mL;
the relative standard deviation of the polymer glucose sensor based on the Mach-Zehnder structure is (1.5-2.5) multiplied by 10 -3 The lowest detection limit is 0.1mg/mL;
the GOD is fixed on the sensing arm of the PMMA core layer through an acid coupling agent at the temperature of 40 ℃ to form a three-dimensional rectangular contact structure, which comprises the following steps: firstly, carrying out surface functionalization modification on the surface of a sensing arm by using a silane solution, and erecting a 'molecular bridge' between an interface of enzyme and a polymer material through silane; then, further coupling treatment is carried out on the surface of the sensing arm by using a cross-linking agent formed by 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide;
dissolving GOD powder in PBS buffer solution with pH of 5.5 to form 30mg/mL GOD solution, placing the device after etching the PDMS upper cladding in a high-low temperature test box, controlling the temperature to 40 ℃, dripping the GOD solution and solidifying, forming a three-dimensional rectangular contact structure on the sensing arm, flushing unfixed GOD on the surface of the sensing arm by the PBS buffer solution, and thus finishing the fixation of the GOD;
the thickness of the PDMS lower cladding and the thickness of the PDMS upper cladding are 10 mu m, and the refractive index is 1.4040; the PMMA core layer has a thickness of 1 mu m and a refractive index of 1.4880; the distance from the upper surface of the sensing arm to the upper surface of the three-dimensional rectangular contact structure is 2-3 mu m;
the curved waveguide has a waveguide width of 1.5 μm and a height of 1 μm.
2. A mach-zehnder structure based polymer glucose sensor according to claim 1, wherein the mach-zehnder structure based polymer glucose sensor has a loss of 1.58dB and a extinction ratio of 41.43dB.
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