CN114163676B - Liquid core hydrogel optical fiber, preparation method and application thereof, liquid core hydrogel optical fiber probe sensor and application thereof - Google Patents
Liquid core hydrogel optical fiber, preparation method and application thereof, liquid core hydrogel optical fiber probe sensor and application thereof Download PDFInfo
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- CN114163676B CN114163676B CN202111613423.7A CN202111613423A CN114163676B CN 114163676 B CN114163676 B CN 114163676B CN 202111613423 A CN202111613423 A CN 202111613423A CN 114163676 B CN114163676 B CN 114163676B
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- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention provides a liquid core hydrogel optical fiber, a preparation method and application thereof, a liquid core hydrogel optical fiber probe sensor and application thereof, and belongs to the technical field of optical fibers. The liquid core hydrogel optical fiber comprises a hollow hydrogel fiber core, a liquid core positioned in the hollow hydrogel fiber core and a hydrogel cladding coated on the surface of the hollow hydrogel fiber core; and UV (ultraviolet) glue seals are arranged at two ends of the hollow hydrogel fiber core. The light energy of the liquid core hydrogel optical fiber provided by the invention is mainly and intensively distributed in the liquid core, so that the liquid core hydrogel optical fiber has the advantages of good locality, low light transmission loss, high collection efficiency and high detection sensitivity; the liquid core can be repeatedly utilized by elution or replacement, and the repeated utilization rate is high; the detection of various substances can be realized by changing the types of the sensing liquid core or the light transmission liquid core in the liquid core, the flexibility is good, the expandability is strong, the application field is wide, and the method has good application prospect in the aspect of detection of metal ions, medicines and biotoxins.
Description
Technical Field
The invention relates to the technical field of optical fibers, in particular to a liquid core hydrogel optical fiber, a preparation method and application thereof, a liquid core hydrogel optical fiber probe sensor and application thereof.
Background
With the development of information technology, optical fiber sensing technology is rapidly activated. The optical fiber sensing is a novel sensing technology which takes light waves as a carrier and optical fibers as media and senses and transmits external measured signals. The optical fiber sensing technology has the advantages of small volume, light weight, strong chemical corrosion resistance, strong electromagnetic interference resistance, safe use, realization of remote detection and real-time monitoring and the like, and is widely applied to biochemical sample instant detection instruments. Most of the existing optical fiber materials are quartz optical fibers or plastic optical fibers, and although the bending property and the mechanical strength are good, the chemical properties of the materials are stable, so that the materials are not easy to combine with sensing materials, and certain limitations exist in the preparation of sensing probes.
The advent of hydrogel, a compound containing hydrophilic groups covalently linked as a three-dimensional network, has provided a new approach to the selection of optical fiber materials. Hydrogel optical fibers satisfying the total reflection condition can be prepared by using hydrogel materials with different refractive indexes. The hydrogel with high refractive index is used as a fiber core, and the hydrogel with low refractive index as a cladding is used as a cladding to realize the optical fiber optical path structure with total reflection. As the hydrogel crosslinked by covalent bonds has good mechanical strength and chemical stability, the prepared hydrogel optical fiber can be bent and is not easy to corrode compared with the traditional quartz optical fiber. In addition, the light transmitting optical fiber is directly embedded in the hydrogel optical fiber to realize coupling without expensive optical fiber fusion splicers and other instruments, so that the hydrogel optical fiber can be very conveniently compatible with the existing optical fiber devices. The hydrogel optical fiber structure prepared by the method has good optical performance and potential application prospect.
Chinese patent CN110724293A discloses a preparation method of a hydrogel optical fiber cladding, which comprises the following steps: s1, preparing a precursor solution A and a precursor solution B by using a hydrogel monomer, a photoinitiator and deionized water, wherein the concentration of the hydrogel monomer in the precursor solution A is higher than that in the precursor solution B; s2, injecting the precursor solution A into a mold, irradiating by using an ultraviolet lamp, carrying out photocrosslinking curing, and extruding to obtain a fiber core of the hydrogel optical fiber; s3: immersing the fiber core obtained in the step S2 in the precursor solution B, then immersing and pulling out the fiber core from the precursor solution B, irradiating the fiber core by using an ultraviolet lamp, and carrying out photocrosslinking and curing to obtain a clad optical fiber; and S4, observing whether the optical fiber after cladding in the S3 reaches the target diameter or not through a microscope. However, the solid hydrogel optical fiber prepared by the above prior art has high optical transmission loss when used as a light transmission optical fiber; when the optical fiber is used as a sensing optical fiber, the sensing material is fixed in the fiber core, so that the sensing material is insufficiently combined with a measured object and can react with the measured object, the sensing material and the measured object are not easy to elute, and the optical fiber probe is difficult to recycle.
Disclosure of Invention
In view of the above, the present invention aims to provide a liquid-core hydrogel optical fiber, a preparation method and an application thereof, a liquid-core hydrogel optical fiber probe sensor and an application thereof. The liquid core hydrogel optical fiber provided by the invention has the advantages of high reuse rate and low optical transmission loss.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a liquid core hydrogel optical fiber, which comprises a hollow hydrogel fiber core, a liquid core positioned in the hollow hydrogel fiber core and a hydrogel cladding coated on the surface of the hollow hydrogel fiber core; and two ends of the hollow hydrogel fiber core are UV glue sealing ends.
The preparation raw materials of the hollow hydrogel fiber core comprise a first hydrogel monomer, a photoinitiator and water;
the raw materials for preparing the hydrogel coating comprise a second hydrogel monomer, calcium chloride and water; the second hydrogel monomer has a refractive index less than the refractive index of the first hydrogel monomer;
the liquid core comprises a light transmitting liquid core or a sensing liquid core.
Preferably, the refractive index of the light transmission liquid core is higher than that of the hollow hydrogel core;
the sensing liquid core comprises a sensing material and water, and the sensing material comprises one or more of a fluorescent sensing material, a surface plasmon resonance material and a surface enhanced Raman scattering sensing material.
Preferably, the first hydrogel monomer and the second hydrogel monomer independently comprise one or more of polyethylene glycol diacrylate, alginic acid, polymethyl methacrylate, polyvinyl alcohol and polylactic acid-glycolic acid copolymer;
the photoinitiator comprises 2-hydroxy-2-methyl-1-phenyl-1-acetone and/or 2-hydroxy-4- (2-hydroxyethoxy) -2-methyl propiophenone;
the UV glue comprises one or more of epoxy acrylate, polyurethane acrylate, polyether acrylate, polyester acrylate and acrylic resin.
Preferably, the inner diameter of the hollow hydrogel fiber core is 0.5-1 mm;
the thickness of the hollow hydrogel fiber core is 1-3 mm;
the thickness of the hydrogel coating is 0.1-1 mm.
The invention provides a preparation method of the liquid core hydrogel optical fiber, which comprises the following steps:
mixing a first hydrogel monomer, a photoinitiator and water, injecting the obtained first hydrogel precursor solution into an annular region of a coaxial hollow silica gel sleeve, carrying out photocuring, and taking out the obtained gel from the coaxial hollow silica gel sleeve to obtain a hollow hydrogel fiber core;
adding a liquid core into the hollow hydrogel fiber core, and then carrying out liquid core packaging on two ends of the hollow hydrogel fiber core by using UV (ultraviolet) glue to obtain liquid core hydrogel; the liquid core comprises a light transmitting liquid core or a sensing liquid core;
and (3) soaking the liquid-core hydrogel in a second hydrogel monomer solution, then placing the soaked liquid-core hydrogel in a calcium chloride aqueous solution, and performing crosslinking and curing to obtain the liquid-core hydrogel optical fiber.
Preferably, the mass of the photoinitiator is 1 to 4% of the mass of the first hydrogel monomer.
Preferably, the light wavelength of the photocuring is 365-405 nm, and the illumination intensity is 12-30 mW/cm 2 The time is 3-6 min.
The temperature of the crosslinking curing is 20-28 ℃, and the time is 3-8 min.
Preferably, the optical fiber comprises a liquid core hydrogel optical fiber and a quartz optical fiber which is partially positioned at one end or two ends of a liquid core of the liquid core hydrogel optical fiber.
Preferably, the length of the silica optical fiber positioned in the liquid-core hydrogel optical fiber is 10-60% of the length of the liquid-core hydrogel optical fiber.
The invention provides application of the liquid core hydrogel optical fiber or the liquid core hydrogel optical fiber probe sensor in the technical scheme in detection of metal ions, medicines or biotoxins.
The invention provides a liquid core hydrogel optical fiber, which comprises a hollow hydrogel fiber core, a liquid core positioned in the hollow hydrogel fiber core and a hydrogel cladding coated on the surface of the hollow hydrogel fiber core; two ends of the hollow hydrogel fiber core are UV glue sealing ends; the preparation raw materials of the hollow hydrogel fiber core comprise a first hydrogel monomer, a photoinitiator and water; the raw materials for preparing the hydrogel coating comprise a second hydrogel monomer, calcium chloride and water; the second hydrogel monomer has a refractive index less than the refractive index of the first hydrogel monomer; the liquid core comprises a light transmitting liquid core or a sensing liquid core. Compared with solid hydrogel optical fibers and hollow hydrogel optical fibers, the liquid-core hydrogel optical fibers provided by the invention have high optical transmission efficiency; compared with the common quartz optical fiber, the liquid core hydrogel optical fiber provided by the invention has better flexibility, can be bent in a large range, and has a wide application range. The liquid core hydrogel optical fiber provided by the invention has the advantages that the light energy is mainly and intensively distributed in the liquid core, the locality is good, the light transmission loss is low, the collection efficiency is high, the full reaction of exciting light and a sensing material can be ensured, and the detection sensitivity is high. The liquid core hydrogel optical fiber provided by the invention can elute the sensing material and the detected object by directly extracting or changing the physical state of the hydrogel, and the preparation of a new probe can be completed by re-injecting the liquid core, so that the repeated utilization rate is high. The liquid core hydrogel optical fiber provided by the invention has the advantages that the contact area of the liquid phase sensing material and an object to be detected is larger, the reaction is more sufficient, the volume of the liquid core area is small, and the required amount of the sensing material is small. The liquid core hydrogel optical fiber provided by the invention improves the optical transmission efficiency by sealing different types of sensing materials, realizes the detection of a plurality of substances by different optical principles, has good flexibility, strong expandability and wide application field, and has good application prospect in the detection of metal ions, medicines and biotoxins.
The invention provides the liquid core hydrogel optical fiber obtained by the preparation method in the technical scheme. Compared with quartz optical fiber and plastic optical fiber, the preparation method provided by the invention does not need expensive optical fiber drawing equipment, and has low cost and simple preparation method. Moreover, the light transmission efficiency can be improved by replacing the sensing material, the flexibility is good, the liquid core can be repeatedly utilized by eluting or replacing, and the repeated utilization rate is high. Compared with solid hydrogel optical fibers, the liquid-core hydrogel optical fiber prepared by the method is mainly concentrated in the liquid-core area of the liquid-core hydrogel optical fiber for transmission, and has the advantages of good locality, low light transmission loss and high collection efficiency.
The invention provides a liquid core hydrogel optical fiber probe sensor which comprises the liquid core hydrogel optical fiber and a quartz optical fiber, wherein the quartz optical fiber is partially positioned at one end or two ends of a liquid core of the liquid core hydrogel optical fiber. In the liquid core hydrogel optical fiber probe sensor provided by the invention, the liquid core hydrogel optical fiber has the advantages of high reuse rate, low optical transmission loss, high collection efficiency and good flexibility, and has good application prospects in the aspects of metal ion, medicine and biotoxin detection.
Drawings
FIG. 1 is a schematic diagram of fluorescence sensing of a liquid-core hydrogel optical fiber prepared in example 1;
FIG. 2 is a schematic diagram of fluorescence sensing of the reflective liquid-core hydrogel optical fiber fluorescence sensor prepared in example 2;
FIG. 3 is a schematic view of a surface plasmon resonance sensing apparatus of the transmission-type liquid-core hydrogel optical fiber fluorescence sensor prepared in example 3;
FIG. 4 shows the liquid-core hydrogel optical fiber fluorescence sensor prepared in example 2 and different Hg concentrations 2+ Reaction experiment results;
FIG. 5 shows the liquid-core hydrogel optical fiber fluorescence sensor prepared in example 2 and different Hg concentrations 2+ Reaction final strength test results;
FIG. 6 is a result of a repeated experiment after changing the liquid of the liquid core hydrogel optical fiber fluorescence sensor prepared in example 2;
FIG. 7 is a light transmission schematic diagram of a reflective liquid-core hydrogel optical fiber fluorescence sensor prepared in example 4;
FIG. 8 is a diagram of light-transmitting materials of example 4 and comparative examples 1 to 2, wherein (a) is comparative example 1, (b) is comparative example 2, and (c) is example 4.
Detailed Description
The invention provides a liquid core hydrogel optical fiber which is characterized by comprising a hollow hydrogel fiber core, a liquid core positioned in the hollow hydrogel fiber core and a hydrogel cladding coated on the surface of the hollow hydrogel fiber core; and two ends of the hollow hydrogel fiber core are UV glue sealing ends.
The preparation raw materials of the hollow hydrogel fiber core comprise a first hydrogel monomer, a photoinitiator and water;
the raw materials for preparing the hydrogel coating comprise a second hydrogel monomer, calcium chloride and water; the second hydrogel monomer has a refractive index less than the refractive index of the first hydrogel monomer;
the liquid core comprises a light transmitting liquid core or a sensing liquid core.
In the present invention, the first hydrogel monomer preferably includes one or more of polyethylene glycol diacrylate, alginic acid, polymethyl methacrylate, polyvinyl alcohol, and polylactic acid-glycolic acid copolymer. In the present invention, the photoinitiator preferably comprises 2-hydroxy-2-methyl-1-phenyl-1-propanone and/or 2-hydroxy-4- (2-hydroxyethoxy) -2-methylpropiophenone. In the present invention, the inner diameter of the hollow hydrogel core is 0.5 to 1mm, more preferably 0.6 to 0.9mm, and still more preferably 0.7 to 0.8mm; the thickness of the hollow hydrogel core is preferably 1 to 3mm, more preferably 1.5 to 2.5mm, and further preferably 2mm.
In the invention, the liquid core comprises a light-transmitting liquid core or a sensing liquid core. In the invention, the refractive index of the light transmission liquid core is higher than that of the hollow hydrogel core; the light transmission liquid core preferably comprises one or more of water, glycerol, turpentine, olive oil, a sucrose solution and a sodium chloride solution; the concentration of the sucrose solution is preferably 50 to 90wt%, more preferably 60 to 80wt%, and further preferably 70wt%; the concentration of the sodium chloride solution is preferably 30 to 35wt%, more preferably 32 to 35wt%, and further preferably 34 to 35wt%; the solvent in the sucrose solution and the sodium chloride solution independently preferably comprises one or more of water, glycerol, turpentine and olive oil.
In the invention, when the liquid core is a light transmission liquid core, the liquid core hydrogel optical fiber structure is a structure consisting of the liquid core, the hydrogel fiber core and the hydrogel cladding, and the refractive indexes of the liquid core, the hydrogel fiber core and the hydrogel cladding are sequentially reduced, so that the light can be transmitted forwards like in a quartz optical fiber by total reflection at the interface of the liquid core and the hydrogel fiber core after entering the liquid core.
In the present invention, the sensing liquid core preferably comprises a sensing material and water; the sensing material preferably comprises one or more of a fluorescent sensing material, a surface plasmon resonance material and a surface enhanced raman scattering sensing material. In the invention, the fluorescent sensing material comprises one or more of a fluorescent dye, a fluorescent dye-labeled nucleic acid and a fluorescent dye-labeled antibody, the fluorescent dye preferably comprises quantum dots or fluorescent microspheres, and the quantum dots preferably comprise one or more of cadmium selenide/zinc sulfide quantum dots (CdSe/ZnS QDs), carbon Quantum Dots (CQDs) and indium phosphide/zinc sulfide quantum dots (InP/ZnS QDs); the fluorescent microspheres preferably comprise; the fluorescent dye in the fluorescent dye-labeled nucleic acid and the fluorescent dye-labeled antibody independently comprises one or more of fluorescein thiocyanate (FITC), carboxyfluorescein (FAM) and tetrachlorofluorescein phosphoramidate (TET). In the present invention, the surface plasmon resonance material and the surface enhanced raman scattering sensing material independently comprise metal nanoparticles, preferably gold nanoparticles and/or silver nanoparticles. In the present invention, the particle size of the sensing material is preferably >20nm, more preferably 20 to 100nm, and further preferably 30 to 50nm. In the present invention, the concentration of the sensing material in the wick is preferably 30 to 100. Mu. Mol/L, more preferably 40 to 80. Mu. Mol/L, and still more preferably 50 to 60. Mu. Mol/L.
In the invention, when the liquid core is a sensing liquid core, the hydrogel fiber core restrains sensing materials (such as fluorescent recognition molecules with larger sizes) in the liquid core, and simultaneously, an object to be measured permeates into the liquid core to react.
In the present invention, the second hydrogel monomer preferably includes one or more of polyethylene glycol diacrylate, alginic acid, polymethyl methacrylate, polyvinyl alcohol, and polylactic acid-glycolic acid copolymer. In the present invention, the refractive index of the second hydrogel monomer is smaller than that of the first hydrogel monomer, and specifically, when the first hydrogel monomer is polyethylene glycol diacrylate, the second hydrogel monomer is preferably alginic acid. In the present invention, the thickness of the hydrogel coating is preferably 0.1 to 1mm, more preferably 0.2 to 0.5mm.
In the present invention, the UV glue preferably includes one or more of epoxy acrylate, urethane acrylate, polyether acrylate, polyester acrylate, and acrylic resin.
The invention provides a preparation method of the liquid core hydrogel optical fiber, which comprises the following steps:
mixing a first hydrogel monomer, a photoinitiator and water, injecting the obtained first hydrogel precursor solution into an annular region of a coaxial hollow silica gel sleeve, carrying out photocuring, and taking out the obtained gel from the coaxial hollow silica gel sleeve to obtain a hollow hydrogel fiber core;
adding a liquid core into the hollow hydrogel fiber core, and then carrying out liquid core packaging on two ends of the hollow hydrogel fiber core by using UV (ultraviolet) glue to obtain liquid core hydrogel; the liquid core comprises a light transmitting liquid core or a sensing liquid core;
and (3) soaking the liquid-core hydrogel in a second hydrogel monomer solution, then placing the soaked liquid-core hydrogel in a calcium chloride aqueous solution, and performing crosslinking and curing to obtain the liquid-core hydrogel optical fiber.
In the present invention, all the raw material components are commercially available products well known to those skilled in the art unless otherwise specified.
According to the invention, a first hydrogel monomer, a photoinitiator and water are mixed, the obtained hydrogel precursor solution is injected into an annular region of a coaxial hollow silica gel sleeve and then is subjected to photocuring, and the obtained gel is taken out of the coaxial hollow silica gel sleeve to obtain a hollow hydrogel fiber core.
In the present invention, the mass of the photoinitiator is preferably 1 to 4%, more preferably 1.5 to 3.5%, and still more preferably 2 to 3% of the mass of the first hydrogel monomer. The mixing method is not particularly limited, and the raw materials can be uniformly mixed. After the mixing, the invention preferably further comprises the step of performing ultrasonic degassing on the mixed solution obtained by the mixing to obtain the hydrogel precursor solution. In the invention, the temperature of the ultrasonic degassing is preferably room temperature, and the time of the ultrasonic degassing is preferably 20-40 min, and more preferably 30min; the ultrasonic degassing is preferably carried out in an ultrasonic cleaning machine. In the present invention, the concentration of the first hydrogel monomer in the hydrogel precursor solution is preferably 20 to 60wt%, more preferably 30 to 50wt%, and still more preferably 40wt%. In the present invention, the concentration of the photoinitiator in the hydrogel precursor solution is preferably 10 to 30g/L, more preferably 15 to 25g/L, and still more preferably 20g/L.
In the invention, the coaxial hollow silica gel sleeve is preferably formed by sleeving a small hollow silica gel tube into a large hollow silica gel tube, and the two hollow silica gel tubes are coaxial; the diameter of the small hollow silicone tube is preferably 0.5-1 mm, more preferably 0.6-0.9 mm, and further preferably 0.7-0.8 mm; the diameter of the large hollow silicone tube is preferably 2-3.5 mm, more preferably 2.2-3.2 mm, and further preferably 2.5-3 mm
In the invention, the light wavelength of the photocuring is preferably 365-405 nm, and the illumination intensity of the photocuring is preferably 12-30 mW/cm 2 More preferably 15 to 30mW/cm 2 More preferably 20 to 25mW/cm 2 (ii) a The photocuring time is preferably 3 to 6min, and more preferably 4 to 5min.
In the present invention, the manner of taking the obtained gel out of the coaxial hollow silica gel cannula is preferably to push out the coaxial hollow silica gel cannula with deionized water.
After a hollow hydrogel fiber core is obtained, liquid core is added into the hollow hydrogel fiber core, and then liquid core encapsulation is carried out on two ends by using UV (ultraviolet) glue, so that liquid core hydrogel is obtained; the liquid core comprises a light transmitting liquid core or a sensing liquid core. In the present invention, the light-transmitting liquid core or the sensing liquid core is preferably the same as the light-transmitting liquid core or the sensing liquid core, and the description thereof is omitted. In the present invention, the amount of the UV gel is preferably 20 to 40. Mu.L, more preferably 25 to 35. Mu.L, and still more preferably 30. Mu.L. The present invention is not particularly limited to the packaging, and a packaging operation known to those skilled in the art may be used.
After the liquid core hydrogel is obtained, the liquid core hydrogel is placed in a second hydrogel monomer solution for soaking, then placed in a calcium chloride aqueous solution, and subjected to crosslinking and curing to obtain the liquid core hydrogel optical fiber.
In the present invention, the concentration of the second hydrogel monomer solution is preferably 30 to 60wt%, more preferably 40 to 60wt%, and further preferably 40 to 50wt%; the second hydrogel monomer preferably comprises one or more of alginic acid, polymethyl methacrylate and polylactic acid-glycolic acid copolymer. In the present invention, the temperature of the soaking is preferably room temperature, and the time of the soaking is preferably 2 to 5min, more preferably 2 to 4min, and further preferably 2 to 3min. In the present invention, the concentration of the calcium chloride aqueous solution is preferably 0.5 to 3mol/L, more preferably 1 to 2.5mol/L, and still more preferably 1.5 to 2mol/L. In the present invention, the temperature of the crosslinking curing is preferably 20 to 28 ℃, more preferably 23 to 27 ℃, and further preferably 24 to 26 ℃; the time for the crosslinking and curing is preferably 3 to 8min, more preferably 4 to 7min, and still more preferably 5 to 6min.
The invention provides a liquid core hydrogel optical fiber probe sensor which comprises a liquid core hydrogel optical fiber and a quartz optical fiber partially positioned at one end or two ends of a liquid core of the liquid core hydrogel optical fiber.
In the invention, when the quartz optical fiber is positioned at one end of the liquid core, the liquid core hydrogel optical fiber probe sensor is a reflection type liquid core hydrogel optical fiber fluorescence sensor, and when the quartz optical fiber is positioned at two ends of the liquid core, the liquid core hydrogel optical fiber probe sensor is a transmission type liquid core hydrogel optical fiber fluorescence sensor. In the present invention, the lengths of the silica optical fibers located at one end and both ends in the liquid core are independently preferably 10 to 60%, more preferably 15 to 50%, and still more preferably 20 to 30% of the length of the liquid core hydrogel optical fiber.
In the present invention, the method for preparing the liquid core hydrogel optical fiber probe sensor preferably comprises the following steps:
mixing a first hydrogel monomer, a photoinitiator and water, injecting the obtained hydrogel precursor solution into an annular area of a coaxial hollow silica gel sleeve, carrying out photocuring, and taking the obtained gel out of the coaxial hollow silica gel sleeve to obtain a hollow hydrogel fiber core;
injecting a liquid core into the hollow hydrogel fiber core, then inserting a quartz optical fiber into one end or two ends of the hollow hydrogel fiber core, and performing liquid core packaging by using UV (ultraviolet) glue to obtain the hydrogel containing the quartz optical fiber liquid core; the liquid core comprises a light transmitting liquid core or a sensing liquid core;
and (3) soaking the quartz-containing optical fiber liquid core hydrogel in a second hydrogel monomer solution, then placing the soaked quartz-containing optical fiber liquid core hydrogel in a calcium chloride aqueous solution, and performing crosslinking curing to obtain the liquid core hydrogel optical fiber probe sensor.
In the invention, no special limitation is imposed on the insertion of the quartz optical fiber at one end or two ends of the hollow hydrogel fiber core, and the length of the inserted quartz optical fiber can be ensured to be 10-30% of the length of the liquid core hydrogel fiber probe sensor; the silica optical fiber is preferably fixed by the UV glue. In the present invention, other preparation conditions of the liquid core hydrogel optical fiber probe sensor are preferably the same as those of the liquid core hydrogel optical fiber, and are not described herein again.
The invention provides application of the liquid core hydrogel optical fiber or the liquid core hydrogel optical fiber probe sensor in the technical scheme in detection of metal ions, medicines or biotoxins.
In the present invention, the metal ions preferably include one or more of mercury ions, iron ions, copper ions, and lead ions. In the invention, the medicament is preferably an animal medicament, and more preferably comprises one or more of profenofos, ciprofloxacin, oxytetracycline and amitraz. In the invention, the biotoxin preferably comprises one or more of aflatoxin, saxitoxin, gymnodinium breve toxin and 1/4 of gonyautoxin.
In the present invention, the method for applying the liquid core hydrogel optical fiber preferably comprises the following steps: and exciting the liquid core hydrogel optical fiber by using a bulk optical element, and immersing the liquid core hydrogel optical fiber into a solution to be detected for detection. In the present invention, the bulk optical element preferably comprises an LED, photodetector, filter or lens.
In the present invention, the method for applying the liquid core hydrogel optical fiber fluorescence sensor preferably comprises the following steps: and (3) immersing the liquid core hydrogel optical fiber fluorescence sensor into a solution to be detected for detection.
In the invention, the excitation and the collection of the signals of the reflective liquid core hydrogel optical fiber fluorescence sensor are both completed by quartz optical fibers. In the invention, the quartz optical fiber at one end of the transmission-type liquid core hydrogel optical fiber fluorescence sensor is used for excitation, and the quartz optical fiber at the other end is used for collection.
In the detection process, the sensing material is restrained in the fiber core by the porous structure of the liquid core hydrogel optical fiber, and meanwhile, the peripheral small molecule object to be detected permeates into the liquid core to react with the sensing material, so that the detection is realized.
In the present invention, the method for recycling a liquid-core hydrogel optical fiber preferably includes the steps of: and processing the detected liquid core hydrogel optical fiber and then using the processed liquid core hydrogel optical fiber for detection. In the present invention, the treatment preferably comprises a physical treatment or a chemical treatment, the physical treatment preferably comprising a heat treatment or extraction of a wick; the temperature of the heating treatment is preferably 200-400 ℃, and more preferably 300-350 ℃; the time of the heat treatment is preferably 5 to 10 seconds, and more preferably 5 to 7 seconds. In the present invention, the drawing is preferably performed using a syringe. In the present invention, the chemical treatment preferably comprises soaking in a debonder, which preferably comprises an organic solvent; the organic solvent preferably comprises acetone or ethyl acetate; the soaking time is not particularly limited, and the soaking time is only required to be 5-7 min, and more preferably 5-6 min until the packaging UV glue is decomposed. In the invention, the recycling method of the liquid core hydrogel optical fiber fluorescence sensor is the same as that of the liquid core hydrogel optical fiber, and is not described in detail herein.
According to the invention, after physical treatment or chemical treatment, hydrogel meshes in the liquid-core hydrogel optical fiber or the liquid-core hydrogel optical fiber fluorescence sensor become larger, so that a sensing material and a detected object after detection reaction are eluted, or the sensing material and the detected object after reaction are directly extracted in an injector extraction mode; thereby realizing the reutilization.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
1081.2 μ L polyethylene glycol diacrylate, 55.7 μ L2-hydroxy-2-methyl-1-phenyl-1-propanone photoinitiator and 1863.1 μ L deionized water were mixed, and degassed by ultrasound with an ultrasonic cleaner for 20min to obtain 3mL hydrogel precursor solution.
Sleeving a hollow silicone tube with the inner diameter of 0.50mm into a hollow silicone tube with the inner diameter of 2mm to obtain a coaxial sleeve, injecting a hydrogel precursor solution into an annular area of the coaxial sleeve by using an injector, then placing the coaxial sleeve under an ultraviolet lamp light source of 365-405 nm for irradiating for 5min, and pushing out the coaxial hollow silicone sleeve by using deionized water to obtain a hollow hydrogel fiber core;
and injecting an aqueous solution of a molecular beacon and a nucleic acid aptamer into the fiber core of the hollow hydrogel (the concentration of the molecular beacon is 1 mu mol/L, the concentration of the nucleic acid aptamer is 1 mu mol/L), and sealing two ends of the hollow hydrogel fiber core by using UV (ultraviolet) glue to obtain the liquid-core hydrogel fiber core.
And (3) immersing the fiber core of the liquid-core hydrogel into a sodium alginate solution with the concentration of 1mol/L, standing for 2min, taking out, then placing into a calcium chloride solution with the concentration of 1mol/L, and performing crosslinking curing at 25 ℃ for 5min to obtain the reflective liquid-core hydrogel optical fiber fluorescence sensor (the thickness of the hydrogel cladding is 0.5 mm).
Fig. 1 is a schematic diagram of fluorescence sensing of the liquid-core hydrogel optical fiber prepared in example 1, and it can be seen from fig. 1 that the aptamer is a hairpin structure and is constrained in the liquid-core sensing region, and when there is no analyte in the liquid core, the fluorescent material and the quencher do not emit light due to fluorescence resonance energy transfer. Mercury ions enter the liquid core sensing area through osmosis and are specifically combined with the aptamer, so that the hairpin of the aptamer is opened, and the distance between the fluorescent material and the quenching group is increased to recover fluorescence. The fluorescence intensity is in direct proportion to the concentration of the mercury ions, so that the relation between the fluorescence intensity and the concentration of the mercury ions can be obtained, and the quantitative detection of the concentration of the mercury ions is realized.
Example 2
1081.2 μ L polyethylene glycol diacrylate, 55.7 μ L2-hydroxy-2-methyl-1-phenyl-1-propanone photoinitiator and 1863.1 μ L deionized water were mixed, and degassed by ultrasound with an ultrasonic cleaner for 20min to obtain 3mL hydrogel precursor solution.
Sleeving a hollow silicone tube with the inner diameter of 0.50mm into a hollow silicone tube with the inner diameter of 2mm to obtain a coaxial sleeve, injecting a hydrogel precursor solution into an annular area of the coaxial sleeve by using an injector, then placing the coaxial sleeve under an ultraviolet lamp light source with the wavelength of 365-405 nm for irradiating for 5min, and pushing out the coaxial hollow silicone sleeve by using deionized water to obtain a hollow hydrogel fiber core;
and (2) inserting a CdSe/ZnS QDs aqueous solution (with the particle size of 10-12 nm and the concentration of 1 mu mol/L) into the core of the hollow hydrogel, then inserting a quartz optical fiber with the core diameter of 105 mu m into one end of the aqueous solution, sealing and fixing the quartz optical fiber by using UV glue, and sealing the other end of the quartz optical fiber by using the UV glue to obtain the liquid-core hydrogel.
And (3) immersing the liquid core hydrogel into a sodium alginate solution with the concentration of 1mol/L, standing for 2min, taking out, then placing into a calcium chloride solution with the concentration of 1mol/L, and performing crosslinking curing at 25 ℃ for 2min to obtain the reflective liquid core hydrogel optical fiber fluorescence sensor (the thickness of the hydrogel cladding is 0.5).
Fig. 2 is a schematic diagram of fluorescence sensing of the reflective liquid core hydrogel optical fiber fluorescence sensor prepared in example 2, and it can be seen from fig. 2 that an excitation light source is transmitted into the liquid core through the quartz optical fiber of the reflective liquid core hydrogel optical fiber fluorescence sensor to excite the fluorescent material to emit light, and then the emitted light is collected by the quartz optical fiber and transmitted to the photodetector through the optical fiber coupler.
Example 3
Mixing 1351.5 mu L of polyethylene glycol diacrylate, 55.7 mu L of 2-hydroxy-2-methyl-1-phenyl-1-acetone photoinitiator and 1592.8 mu L of deionized water, and ultrasonically degassing for 20min by an ultrasonic cleaner to obtain 3mL of hydrogel precursor solution.
Sleeving a hollow silicone tube with the inner diameter of 0.80mm into a hollow silicone tube with the inner diameter of 2.5mm to obtain a coaxial sleeve, injecting a hydrogel precursor solution into an annular area of the coaxial sleeve by using an injector, then placing the coaxial sleeve under an ultraviolet lamp light source with the wavelength of 365-405 nm for irradiating for 6min, and pushing out the coaxial hollow silicone sleeve by using deionized water to obtain a hollow hydrogel fiber core;
and (2) injecting gold nanoparticle sol (the particle size is 30nm and the concentration is 50 mu M) into the fiber core of the hollow hydrogel, respectively inserting quartz optical fibers with the core diameter of 200 mu M into the two ends of the hollow hydrogel, and sealing and fixing the quartz optical fibers by using UV (ultraviolet) glue to obtain the liquid-core hydrogel.
And (3) immersing the liquid core hydrogel into a sodium alginate solution with the concentration of 1mol/L, standing for 2min, taking out, then placing into a calcium chloride solution with the concentration of 1mol/L, and performing crosslinking curing at 25 ℃ for 2min to obtain the transmission type liquid core hydrogel optical fiber fluorescence sensor (the thickness of a hydrogel cladding is 0.5 mm).
Fig. 3 is a schematic view of a surface plasmon resonance sensing apparatus of the transmission-type liquid core hydrogel optical fiber fluorescence sensor prepared in example 3. As can be seen from fig. 3, the white light source and the optical fiber spectrometer connected with the pigtail are respectively connected to two ends of the transmission-type liquid-core hydrogel optical fiber fluorescence sensor, and the transmission-type liquid-core hydrogel optical fiber fluorescence sensor is placed in glucose solutions with different concentrations. The liquid core area of the transmission-type liquid core hydrogel optical fiber fluorescence sensor is gold nanoparticles, the gold nanoparticles can form a surface plasma resonance peak, and the position of the peak can generate displacement along with the change of the refractive index of the particle surface. The white light source is transmitted into the liquid core through the optical fiber and excites the gold nanoparticles to generate surface plasma resonance peaks, glucose solutions with different concentrations penetrate into the liquid core and can lead the refractive index of the surface of the gold particles to change, so that the displacement of the resonance peaks is generated, and the optical signals are transmitted into the spectrometer through the subsequent optical fiber to be detected.
FIG. 4 shows the liquid-core hydrogel optical fiber fluorescence sensor prepared in example 2 and different Hg concentrations 2+ As shown in fig. 4, the liquid core hydrogel optical fiber fluorescence sensor prepared in example 2 can distinguish mercury ions with a series of concentration gradients.
FIG. 5 shows the liquid-core hydrogel optical fiber fluorescence sensor prepared in example 2 and different Hg concentrations 2+ And (5) reaction final strength experiment results. As can be seen from fig. 5, the liquid core hydrogel optical fiber fluorescence sensor prepared in example 2 has specificity for detecting mercury ions.
Fig. 6 is a result of repeated experimental tests after the liquid core of the liquid core hydrogel optical fiber fluorescence sensor prepared in example 2 is replaced. As can be seen from FIG. 6, the liquid core hydrogel optical fiber fluorescence sensor prepared by the invention can be recycled by changing the liquid.
Example 4
1081.2 μ L of polyethylene glycol diacrylate, 55.7 μ L of 2-hydroxy-2-methyl-1-phenyl-1-propanone photoinitiator and 1863.1 μ L of deionized water were mixed, and subjected to ultrasonic degassing for 20min by an ultrasonic cleaner to obtain 3mL of hydrogel precursor solution.
Sleeving a hollow silicone tube with the inner diameter of 0.40mm into a hollow silicone tube with the inner diameter of 2mm to obtain a coaxial sleeve, injecting a hydrogel precursor solution into an annular area of the coaxial sleeve by using an injector, then placing the coaxial sleeve under an ultraviolet lamp light source of 365-405 nm for irradiating for 5min, and pushing out the coaxial hollow silicone sleeve by using deionized water to obtain a hollow hydrogel fiber core;
and injecting a sodium chloride aqueous solution with the concentration of 80wt% into the core of the hollow hydrogel, then inserting a quartz optical fiber with the core diameter of 105 mu m into one end of the hollow hydrogel, sealing and fixing the quartz optical fiber by using UV glue, and sealing the other end of the hollow hydrogel by using the UV glue to obtain the liquid-core hydrogel.
And immersing the liquid core hydrogel into a sodium alginate solution with the concentration of 1mol/L, standing for 2min, taking out, then placing into a calcium chloride solution with the concentration of 1mol/L, and performing crosslinking curing at 25 ℃ for 2min to obtain the reflective liquid core hydrogel optical fiber fluorescence sensor (the thickness of a hydrogel cladding is 0.5 mm).
Comparative example 1
Injecting the hydrogel precursor solution into a hollow silica gel tube with the inner diameter of 2mm by using an injector, irradiating for 5min under an ultraviolet lamp light source with the wavelength of 365-405 nm, and pushing out the coaxial hollow silica gel sleeve by using deionized water to obtain the solid hydrogel optical fiber.
Comparative example 2
1081.2 μ L of polyethylene glycol diacrylate, 55.7 μ L of 2-hydroxy-2-methyl-1-phenyl-1-propanone photoinitiator and 1863.1 μ L of deionized water were mixed, and subjected to ultrasonic degassing for 20min by an ultrasonic cleaner to obtain 3mL of hydrogel precursor solution.
And sleeving a hollow silicone tube with the inner diameter of 0.50mm into a hollow silicone tube with the inner diameter of 2mm to obtain a coaxial sleeve, injecting a hydrogel precursor solution into an annular area of the coaxial sleeve by using an injector, then placing the coaxial sleeve under an ultraviolet lamp light source of 365-405 nm for irradiating for 5min, and pushing out the coaxial hollow silicone sleeve by using deionized water to obtain the hollow hydrogel optical fiber.
The reflective liquid-core hydrogel optical fiber fluorescence sensor prepared in example 4, the solid-core hydrogel optical fiber prepared in comparative example 1 and the hollow-core hydrogel optical fiber prepared in comparative example 2 were respectively connected to a 520nm laser.
Fig. 7 is a light transmission schematic diagram of a reflection type liquid core hydrogel optical fiber fluorescence sensor prepared in example 4, wherein light rays (1) and (2) represent light rays with different incident angles. As can be seen from fig. 7, the refractive index of the liquid core > the refractive index of the hydrogel cladding, which meets the basic condition of total reflection, and light is locally transmitted in the liquid core region.
FIG. 8 is a diagram of light-transmitting substances of example 4 and comparative examples 1 to 2, wherein (a) is comparative example 1, (b) is comparative example 2, and (c) is example 4. As can be seen from fig. 8, although the solid hydrogel optical fiber can see the total reflection transmission trace of light, the light is relatively dispersed as a whole; the hollow hydrogel fiber core generates more leakage light; the liquid core hydrogel optical fiber can well localize light in the liquid core, and the transmission efficiency is high.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The liquid core hydrogel optical fiber is characterized by comprising a hollow hydrogel fiber core, a liquid core positioned in the hollow hydrogel fiber core and a hydrogel cladding coated on the surface of the hollow hydrogel fiber core; two ends of the hollow hydrogel fiber core are UV adhesive sealing ends;
the preparation raw materials of the hollow hydrogel fiber core comprise a first hydrogel monomer, a photoinitiator and water;
the raw materials for preparing the hydrogel coating comprise a second hydrogel monomer, calcium chloride and water; the second hydrogel monomer has a refractive index less than the refractive index of the first hydrogel monomer;
the liquid core comprises a light transmitting liquid core or a sensing liquid core.
2. The liquid-core hydrogel optical fiber according to claim 1, wherein the refractive index of the light-transmitting liquid core is higher than the refractive index of the hollow hydrogel core;
the sensing liquid core comprises a sensing material and water, and the sensing material comprises one or more of a fluorescent sensing material, a surface plasmon resonance material and a surface enhanced Raman scattering sensing material.
3. The liquid-core hydrogel optical fiber according to claim 1, wherein the first hydrogel monomer and the second hydrogel monomer independently comprise one or more of polyethylene glycol diacrylate, alginic acid, polymethyl methacrylate, polyvinyl alcohol, and polylactic acid-glycolic acid copolymer;
the photoinitiator comprises 2-hydroxy-2-methyl-1-phenyl-1-acetone and/or 2-hydroxy-4- (2-hydroxyethoxy) -2-methyl propiophenone;
the UV glue comprises one or more of epoxy acrylate, polyurethane acrylate, polyether acrylate and polyester acrylate.
4. The liquid core hydrogel optical fiber according to claim 1 or 3, wherein the inner diameter of the hollow hydrogel fiber core is 0.5 to 1mm;
the thickness of the hollow hydrogel fiber core is 1 to 3mm;
the thickness of the hydrogel coating is 0.1-1mm.
5. The method for preparing the liquid core hydrogel optical fiber according to any one of claims 1 to 4, which is characterized by comprising the following steps:
mixing a first hydrogel monomer, a photoinitiator and water, injecting the obtained first hydrogel precursor solution into an annular region of a coaxial hollow silica gel sleeve, carrying out photocuring, and taking out the obtained gel from the coaxial hollow silica gel sleeve to obtain a hollow hydrogel fiber core;
adding a liquid core into the hollow hydrogel fiber core, and then performing liquid core packaging on two ends of the hollow hydrogel fiber core by using UV (ultraviolet) glue to obtain liquid core hydrogel; the liquid core comprises a light transmitting liquid core or a sensing liquid core;
and (3) soaking the liquid-core hydrogel in a second hydrogel monomer solution, then placing the soaked liquid-core hydrogel in a calcium chloride aqueous solution, and performing crosslinking and curing to obtain the liquid-core hydrogel optical fiber.
6. The preparation method according to claim 5, wherein the mass of the photoinitiator is 1 to 4% of the mass of the first hydrogel monomer.
7. The method according to claim 5, wherein the photocuring light has a wavelength of 365 to 405nm and an illumination intensity of 12 to 30mW/cm 2 The time is 3 to 6min；
The temperature of the crosslinking curing is 20 to 28 ℃, and the time is 3 to 8min.
8. The liquid core hydrogel optical fiber probe sensor is characterized by comprising a liquid core hydrogel optical fiber and a quartz optical fiber, wherein the quartz optical fiber is partially positioned at one end or two ends of a liquid core of the liquid core hydrogel optical fiber;
the liquid core hydrogel optical fiber is the liquid core hydrogel optical fiber according to any one of claims 1 to 4 or the liquid core hydrogel optical fiber prepared by the preparation method according to any one of claims 5 to 7.
9. The liquid core hydrogel optical fiber probe sensor according to claim 8, wherein the length of the quartz optical fiber in the liquid core hydrogel optical fiber is 10 to 60% of the length of the liquid core hydrogel optical fiber.
10. The use of the liquid core hydrogel optical fiber according to any one of claims 1 to 4, the liquid core hydrogel optical fiber prepared by the preparation method according to any one of claims 5 to 7, or the liquid core hydrogel optical fiber probe sensor according to any one of claims 8 to 9 in the detection of metal ions, drugs or biotoxins.
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