CN109709182A - A kind of g-C3N4-MnO2The photic electrochemical process super sensitivity detection glutathione of nanocomposite - Google Patents
A kind of g-C3N4-MnO2The photic electrochemical process super sensitivity detection glutathione of nanocomposite Download PDFInfo
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- CN109709182A CN109709182A CN201910158921.3A CN201910158921A CN109709182A CN 109709182 A CN109709182 A CN 109709182A CN 201910158921 A CN201910158921 A CN 201910158921A CN 109709182 A CN109709182 A CN 109709182A
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Abstract
The invention discloses a kind of g-C3N4‑MnO2The photic electrochemical process super sensitivity detection glutathione of nanocomposite.By growing g-C on paper base3N4‑MnO2Nanocomposite, preparation g-C3N4‑MnO2- GSH sensor, utilizes MnO2To the specific selection and g-C of GSH3N4‑MnO2Nanocomposite and g-C3N4‑MnO2The sensitive photocurrent response of-GSH sensor, realizes the super sensitivity detection to GSH.The sensing system effectively reduces the detection limit of GSH compared with other conventional methods, and easy to operate, and detection efficiency is high.
Description
Technical field
The present invention relates to glutathione detection technique field, more specifically a kind of g-C3N4-MnO2Nanocomposite
Photic electrochemical process super sensitivity detection glutathione (GSH).
Background technique
Electrogenerated chemiluminescence (ECL) is one kind between electrochemistry and chemiluminescent method, since its is simple to operation, low
The characteristics of cost, high sensitivity, has become a kind of important strong analysis method in analysis and clinical medicine.More
Importantly, as a result ECL is presented on a simple instrument, low background because it does not need light source better than other analysis methods
Or zero background signal.
Nanocomposite is by two or more material of different nature, by method physically or chemically, in macroscopic view
Upper composition has the material of new capability.A variety of materials are mutually learnt from other's strong points to offset one's weaknesses in performance, are generated synergistic effect, are made composite material
Comprehensive performance is better than the performance of original various composition materials, thus meets a variety of different requirements.
Glutathione is a kind of tripeptides (L- gamma-glutamyl-L- cysteinyl-glycine) compound, it be distributed widely in animal,
In plant, cereal and oilseed, its one of function in cell is exactly to resist various toxin and carcinogen, there is research table
Bright: glutathione can be completely absorbed in small intestine, and certain epithelial cells can be using Exogenous Glutathione come detoxification, this says
Glutathione in bright diet decides the degree of cell damage in human body.In addition to as counterpoison, glutathione is also to some
Sulfydryl enzyme has activation, can be used as the antioxidant of protective enzyme He other protein sulfhydryls, biological oxidation, amino acid transport,
It plays a role during protection hemoglobin etc..In addition, research recently inhibits AIDS virus it has also been found that glutathione has
Effect.Therefore research glutathione has great importance to the Health and Living of the mankind.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of light that high sensitivity, high specificity are established in paper chip
Send a telegraph chemical analysis detection method, this method can be accomplished without complicated cumbersome big easily in most laboratories
Type equipment is supported.Specific solution is as follows:
(1) paper chip is designed: dredging using the micro-fluidic paper chip of Adobe Illustrator CS4 software design on computers
Water wax bulk print pattern, style is as shown in the picture, which includes hydrophobic region and the inside parent of outer wax printing
Water workspace, for individual unit having a size of 30 × 30mm, hydrophilic region diameter dimension is 10mm, and channel size is 6.5 × 8mm, institute
It is chromatographic paper with paper chip；
(2) it prepares flower-shaped gold nanoparticle: measuring 80 mL ultrapure waters and be heated to 90 DEG C, it is 1 that 0.8 mL mass fraction, which is added,
The chlorauric acid solution of % continues to be heated to 96 DEG C and keeps the temperature 1 min, the sodium citrate that 2.8 mL mass fractions of addition are 1 %, and 96
8 min are kept the temperature at DEG C and obtain gold seeds solution, are measured the gold seeds solution that 20 μ L are obtained and are added dropwise in working region, standing is dried,
In triplicate；Measure the ascorbic acid solution of 100 μ L, 200 mmol/L respectively at room temperature, 100 μ L mass fractions are 1 %'s
Chlorauric acid solution measures the 20 above-mentioned mixed solutions of μ L and is added drop-wise to the working region for being modified with gold seeds, stands 30 min, with super
Pure water rinsing 3 times；
(3) g-C is prepared3N4Nanometer sheet: 20 g melamines are weighed and are put into alumina crucible with cover and in 600 °C of Muffles
2 h are heated in furnace, the rate of heat addition is 3 °C of min-1, after completion of the reaction, generate yellow g-C3N4Powder；Weigh 50 mg yellow
g-C3N4Powder is scattered in 50 mL ultrapure waters, is ultrasonically treated 10 h；
(4) g-C is prepared3N4-MnO2Nanocomposite simultaneously carries out Photoelectric Detection:: measure 250 μ L g-C3N4Nanometer sheet solution
It is added to the 2-(N- morpholino of 2.5 mL, 0.1 M pH 6.0) mixed solution is obtained in ethanesulfonic acid buffer, measure 1 ml 10
The KMnO of mM4The ultrapure water of solution, 10 ml is added in mixed solution, is ultrasonically treated 30 min, forms brown colloid, centrifugation
Collect g-C3N4-MnO2Nanocomposite and with milli-Q water 3 times, will be centrifuged resulting product and is scattered in 10 mL ultrapure waters
In；It measures the 20 above-mentioned solution of μ L and is added drop-wise to the paper chip working region surface for containing flower-shaped gold nanoparticle obtained by step 2, it is quiet
30 min are set, with ultrapure water 3 times；G-C will be contained3N4-MnO2The paper chip of nanocomposite is connected with working electrode,
It is placed in the PBS solution of PH 7.4, the photo-signal generated is collected using three-electrode system；
(5) g-C is prepared3N4-MnO2- GSH sensor simultaneously carries out Photoelectric Detection: measuring the g-C of 10 μ L3N4-MnO2Nano-complex
Solution, 10 μ L GSH mixed in 1.5mL centrifuge tube, be incubated for 7min after, measure appropriate ultrapure water above-mentioned mixed solution is dilute
It releases to 250 μ L and is sufficiently mixed；It measures the 20 above-mentioned solution of μ L and is added drop-wise to the core for containing flower-shaped gold nanoparticle obtained by step 2
Piece working region surface stands 30 min, with ultrapure water 3 times；G-C will be contained3N4-MnO2- GSH nanocomposite
Paper chip is connected with working electrode, is placed in the PBS solution of PH 7.4, acquires photosignal using three-electrode system；
(6) photosignal is analyzed: in conjunction with step 4,5 resulting photosignals, the content of GSH in analytical calculation solution to be measured.
Beneficial effects of the present invention:
(1) present invention is low in cost, experimental implementation is simple, easy control of reaction conditions；
(2) compared to traditional glass-carbon electrode and glass electrode, paper base material abundant raw material, light weight, it is cheap, foldable, can drop
Solution；
(3) paper base sensor flexible is flexible, easy to carry, can cut out, be bent, folding and is plastic, and post-processing is simple, will not be right
Environment pollutes；
(4) paper is usually white, and background signal is low.
Detailed description of the invention
Fig. 1 is the paper chip design drawing of this paper.
Specific embodiment
Specific embodiment of the invention is illustrated below: a kind of g-C3N4-MnO2The photic electrification of nanocomposite
Method super sensitivity detection glutathione.
Embodiment 1(detects the GSH in aqueous solution)
(1) paper chip is designed: dredging using the micro-fluidic paper chip of Adobe Illustrator CS4 software design on computers
Water wax bulk print pattern, style is as shown in the picture, which includes hydrophobic region and the inside parent of outer wax printing
Water workspace, for individual unit having a size of 30 × 30 mm, hydrophilic region diameter dimension is 10 mm, and channel size is 6.5 × 8 mm,
Paper chip used is chromatographic paper；
(2) it prepares flower-shaped gold nanoparticle: measuring 80 mL ultrapure waters and be heated to 90 DEG C, it is 1 that 0.8 mL mass fraction, which is added,
The chlorauric acid solution of % continues to be heated to 96 DEG C and keeps the temperature 1 min, the sodium citrate that 2.8 mL mass fractions of addition are 1 %, and 96
8 min are kept the temperature at DEG C and obtain gold seeds solution, are measured the gold seeds solution that 20 μ L are obtained and are added dropwise in working region, standing is dried,
In triplicate；Measure the ascorbic acid solution of 100 μ L, 200 mmol/L respectively at room temperature, 100 μ L mass fractions are 1 %'s
Chlorauric acid solution measures the 20 above-mentioned mixed solutions of μ L and is added drop-wise to the working region for being modified with gold seeds, stands 30 min, with super
Pure water rinsing 3 times；
(3) g-C is prepared3N4Nanometer sheet: 20 g melamines are weighed and are put into alumina crucible with cover and in 600 °C of Muffles
2 h are heated in furnace, the rate of heat addition is 3 °C of min-1, after completion of the reaction, generate yellow g-C3N4Powder；Weigh 50 mg yellow
g-C3N4Powder is scattered in 50 mL ultrapure waters, is ultrasonically treated 10 h；
(4) g-C is prepared3N4-MnO2Nanocomposite simultaneously carries out Photoelectric Detection:: measure 250 μ L g-C3N4Nanometer sheet solution
It is added to the 2-(N- morpholino of 2.5 mL, 0.1 M pH 6.0) mixed solution is obtained in ethanesulfonic acid buffer, measure 0 respectively,
1, the KMnO of 2,3,4,5,6,7,8,9,10 mM4The ultrapure water of solution, 10 ml is added in mixed solution, ultrasonic treatment 30
Min forms brown colloid, g-C is collected by centrifugation3N4-MnO2Nanocomposite and with milli-Q water 3 times, will be centrifuged resulting
Product is scattered in 10 mL ultrapure waters；It measures the 20 above-mentioned solution of μ L and is added drop-wise to and contain flower-shaped gold nanoparticle obtained by step 2
Paper chip working region surface stands 30 min, with ultrapure water 3 times；G-C will be contained3N4-MnO2Nanocomposite
Paper chip is connected with working electrode, is placed in the PBS solution of PH 7.4, and the photoelectric current generated is collected using three-electrode system and is believed
Number；
(5) g-C is prepared3N4-MnO2- GSH sensor simultaneously carries out Photoelectric Detection: measuring the strongest g- of photosignal of 10 μ L
C3N4-MnO2Nano-complex solution, the GSH of 10 μ L, 0,0.05,0.1,0.15,0.2,0.25,0.5,1.0,1.5,2.0 mM
It is mixed in 1.5 mL centrifuge tubes, after being incubated for 7 min, measures appropriate ultrapure water and above-mentioned mixed solution is diluted to 250 μ L and is filled
Divide mixing；It measures the 20 above-mentioned solution of μ L and is added drop-wise to the paper chip working region table for containing flower-shaped gold nanoparticle obtained by step 2
Face stands 30 min, with ultrapure water 3 times；G-C will be contained3N4-MnO2The paper chip and work of-GSH nanocomposite
Electrode is connected, and is placed in the PBS solution of PH 7.4, acquires photosignal using three-electrode system；
(6) photosignal is analyzed: in conjunction with step 4,5 resulting photosignals, the content of GSH in analytical calculation solution to be measured.
Claims (7)
1. it is an object of the present invention to a kind of g-C3N4-MnO2The photic electrochemical process super sensitivity detection gluathione of nanocomposite
Peptide (GSH), it is characterized in that the following steps are included:
(1) paper chip is designed；
(2) flower-shaped gold nanoparticle is prepared；
(3) g-C is prepared3N4Nanometer sheet；
(4) g-C is prepared3N4-MnO2Nanocomposite simultaneously carries out Photoelectric Detection；
(5) g-C is prepared3N4-MnO2- GSH sensor simultaneously carries out Photoelectric Detection；
(6) photosignal is analyzed.
2. a kind of g-C according to claim 13N4-MnO2The photic electrochemical process super sensitivity detection of nanocomposite
GSH, design paper chip as described in step (1), it is characterized in that: it is soft using Adobe Illustrator CS4 on computers
Part designs the hydrophobic wax bulk print pattern of micro-fluidic paper chip, and style is as shown in the picture, which includes outside
The hydrophobic region of wax printing and inner hydrophilic workspace, for individual unit having a size of 30 × 30 mm, hydrophilic region diameter dimension is 10
Mm, channel size are 6.5 × 8 mm, and paper chip used is chromatographic paper.
3. a kind of g-C according to claim 13N4-MnO2The photic electrochemical process super sensitivity detection of nanocomposite
GSH, step prepare flower-shaped gold nanoparticle described in (2), it is characterized in that: it measures 80 mL ultrapure waters and is heated to 90 DEG C,
The chlorauric acid solution that 0.8 mL mass fraction is 1 % is added, continue to be heated to 96 DEG C and keeps the temperature 1 min, 2.8 mL mass are added
Score is the sodium citrate of 1 %, and 8 min are kept the temperature at 96 DEG C and obtain gold seeds solution, measures the gold seeds solution that 20 μ L are obtained
It is added dropwise in working region, standing is dried, in triplicate；The ascorbic acid for measuring 100 μ L, 200 mmol/L respectively at room temperature is molten
Liquid, 100 μ L mass fractions are the chlorauric acid solution of 1 %, and the 20 above-mentioned mixed solutions of μ L of measurement, which are added drop-wise to, is modified with gold seeds
Working region stands 30 min, with ultrapure water 3 times.
4. a kind of g-C according to claim 13N4-MnO2The photic electrochemical process super sensitivity detection of nanocomposite
GSH, preparation g-C described in step (3)3N4Nanometer sheet, it is characterized in that: it weighs 20 g melamines and is put into aluminium oxide with cover
In crucible and in heating 2 h in 600 °C of Muffle furnaces, the rate of heat addition is 3 °C of min-1, after completion of the reaction, generate yellow g-
C3N4Powder；Weigh 50 mg yellow g-C3N4Powder is scattered in 50 mL ultrapure waters, is ultrasonically treated 10 h.
5. a kind of g-C according to claim 13N4-MnO2The photic electrochemical process super sensitivity detection of nanocomposite
GSH, preparation g-C described in step (4)3N4-MnO2Nanocomposite simultaneously carries out Photoelectric Detection, it is characterized in that: measure 250
μL g-C3N4Nanometer sheet solution is added to the 2-(N- morpholino of 2.5 mL, 0.1 M pH 6.0) it is mixed in ethanesulfonic acid buffer
Solution is closed, the KMnO of 1 ml, 10 mM is measured4The ultrapure water of solution, 10 ml is added in mixed solution, ultrasonic treatment 30
Min forms brown colloid, g-C is collected by centrifugation3N4-MnO2Nanocomposite and with milli-Q water 3 times, will be centrifuged resulting
Product is scattered in 10 mL ultrapure waters；It measures the 20 above-mentioned solution of μ L and is added drop-wise to and contain flower-shaped gold nanoparticle obtained by step (2)
Paper chip working region surface, stand 30 min, with ultrapure water 3 times；G-C will be contained3N4-MnO2Nanocomposite
Paper chip be connected with working electrode, be placed in the PBS solution of PH 7.4, utilize three-electrode system collect generate photoelectric current letter
Number.
6. a kind of g-C according to claim 13N4-MnO2The photic electrochemical process super sensitivity detection of nanocomposite
GSH, preparation g-C described in step (5)3N4-MnO2- GSH sensing material simultaneously carries out Photoelectric Detection, it is characterized in that: measure 10 μ
The g-C of L3N4-MnO2Nano-complex solution, 10 μ L GSH mixed in 1.5 mL centrifuge tubes, after being incubated for 7 min, measure suitable
Above-mentioned mixed solution is diluted to 250 μ L and is sufficiently mixed by amount ultrapure water；It measures the 20 above-mentioned solution of μ L and is added drop-wise to step (2) institute
The paper chip working region surface containing flower-shaped gold nanoparticle is obtained, 30 min are stood, with ultrapure water 3 times；G- will be contained
C3N4-MnO2The paper chip of-GSH nanocomposite is connected with working electrode, is placed in the PBS solution of PH 7.4, utilizes three electricity
Polar body system acquires photosignal.
7. a kind of g-C according to claim 13N4-MnO2The photic electrochemical process super sensitivity detection of nanocomposite
GSH, the analysis of photosignal described in step (6), it is characterized in that: in conjunction with step (4), (5) resulting photosignal, analysis meter
Calculate the content of GSH in solution to be measured.
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