CN108680566A - The new method of hydrogen peroxide is detected based on MoS2 nanometers of fermentoid luminescence systems - Google Patents
The new method of hydrogen peroxide is detected based on MoS2 nanometers of fermentoid luminescence systems Download PDFInfo
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- CN108680566A CN108680566A CN201810490582.4A CN201810490582A CN108680566A CN 108680566 A CN108680566 A CN 108680566A CN 201810490582 A CN201810490582 A CN 201810490582A CN 108680566 A CN108680566 A CN 108680566A
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/76—Chemiluminescence; Bioluminescence
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Abstract
The invention discloses a kind of new methods detecting hydrogen peroxide based on MoS2 nanometers of fermentoid luminescence systems, include the following steps:S1, MoS2 two-dimensional nano fermentoids are prepared;S2, the luminol mother liquor and Tris HCl buffer solutions for preparing 0.1mol/L;S3, the luminol mother liquor that will prepare gained are diluted to Tris HCl buffer solutions 5 mMs every liter of luminol solution, then the hydrogenperoxide steam generator of 40 microlitres of acquired solutions and 40 microlitres of various concentrations mixing in measuring cup is taken, 40 microlitres 1 mM every liter of MoS2 nanometer fermentoids are added thereto again, after reaction 30 seconds, entire reaction system is put into chemical luminescence detector, is collected by Chemiluminescence Apparatus and records optical signal caused by reaction.Invention enhances the intensity of luminous signal when detection hydrogen peroxide, shorten the reaction time.
Description
Technical field
The present invention relates to a kind of hydrogen peroxide detection methods, and in particular to one kind is examined based on MoS2 nanometers of fermentoid luminescence systems
Survey the new method of hydrogen peroxide.
Background technology
Hydrogen peroxide is a kind of oxidant, is a kind of common metabolite in life entity, is detected, monitors to it
It is known that whether vital metabolic normal, while one of certain disease symptoms are exactly that content of hydrogen peroxide is abnormal, therefore peroxidating
Hydrogen detection can be the metabolism of monitoring life entity, diagnose the illness the science that provides, objective evidence, have very important research and development value.
Generally acknowledge that special, sensitive detection hydrogen peroxide means are the catalases of organism at present, however hydrogen peroxide
The biology person's character of enzyme, purifying preserve, use condition harshness, with high costs, therefore the demand of fermentoid is extremely urgent.MoS2
Two-dimension nano materials are a kind of preferable nanometer fermentoids of hydroperoxide kind enzymatic activity, altogether with tetramethyl benzidine substrates (TMB)
Very good fermentoid characteristic is shown in hydrogen peroxide colorimetric detection method.But MoS2 nanometers of fermentoids are formed with TMB
Hydrogen peroxide detection architecture be to be aoxidized and change colour (colorimetric determination) based on tmb substrate, signal is weak, reaction relatively slowly, detection limit
Height needs further research to develop the better detection method of detection performance thus.
Invention content
To solve the above problems, detecting hydrogen peroxide based on MoS2 nanometers of fermentoid luminescence systems the present invention provides a kind of
New method enhances the intensity of luminous signal when detecting hydrogen peroxide, shortens the reaction time.
To achieve the above object, the technical solution that the present invention takes is:
The new method that hydrogen peroxide is detected based on MoS2 nanometers of fermentoid luminescence systems, is included the following steps:
S1, MoS2 two-dimensional nano fermentoids are prepared
50mgMoS2 is added in the 10ml aqueous solutions containing 10mg bovine serum albumins (BSA), gun-type ultrasonic probe is used
After being ultrasonically treated 6h under conditions of power is 240W, the speed centrifugation 45min with 5000r/min is placed in supercentrifuge,
Ultrasound disperses 10min again in general purpose ultrasound cleaner bath, then centrifuges 45min with 15000r/min speed, collects supernatant,
It is saved backup under 4 degree;
S2, luminol solution and Tris-HCl buffer solutions are prepared
Prepare luminol solution
It weighs 7.08mg luminol reagents and is dissolved in the sodium hydroxide solution of a concentration of 0.1mol/L of 4ml and be configured to
The luminol mother liquor of 0.1mol/L, and be kept in dark place at 4 deg. celsius;
It is equipped with Tris-HCl buffer solutions
1.211mg trishydroxymethylaminomethanes are weighed, are dissolved in the ultra-pure water of 75ml, it is molten with the hydrochloric acid of 1mol/L
Liquid adjusts pH to 11 respectively, and 25mg ethylenediamine tetra-acetic acids are added, and ultra-pure water is settled to 1000ml, for use;
The measurement of S3, hydrogen peroxide
The luminol that luminol mother liquor obtained by preparing is diluted to 5 mMs every liter with Tris-HCl buffer solutions is molten
Then liquid takes the hydrogenperoxide steam generator of 40 microlitres of acquired solutions and 40 microlitres of various concentrations mixing in measuring cup, then thereto
40 microlitres 1 mM every liter of MoS2 nanometer fermentoids are added, after reacting 30 seconds, are put into chemical luminescence detector, passes through chemistry and sends out
Light instrument is collected and records optical signal caused by reaction, and the characteristic signal frequency peak and peak intensity composed by optical signal quantify peroxide
Change hydrogen.
In said program, the detection architecture of hydrogen peroxide is done using luminol/MoS2 nanometers of fermentoid, can significantly improve production
Raw light signal strength and reduction hydrogen peroxide detection limit, concentration of hydrogen peroxide can be detected by, which making, further decreases, and is highly sensitive micro-
The detection of trace hydrogen peroxide provides new method.
Description of the drawings
Fig. 1 is the UV-vis spectrophotometric spectra figures of the MoS2 centrifuged supernatants of ultrasound stripping in the embodiment of the present invention.
Fig. 2 is the two-dimentional MoS removed in the embodiment of the present invention2The TEM of nanometer sheet schemes.
Specific implementation mode
In order to make objects and advantages of the present invention be more clearly understood, the present invention is carried out with reference to embodiments further
It is described in detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this hair
It is bright.
Embodiment
S1, MoS2 two-dimensional nano fermentoids are prepared
50mgMoS2 is added in the 10ml aqueous solutions containing 10mg bovine serum albumins (BSA), gun-type ultrasonic probe is used
After being ultrasonically treated 6h under conditions of power is 240W, the speed centrifugation 45min with 5000r/min is placed in supercentrifuge,
Ultrasound disperses 10min again, then centrifuges 45min with 15000r/min speed, collects supernatant, is saved backup under 4 degree;
S2, luminol solution and Tris-HCl buffer solutions are equipped with
It is equipped with luminol solution
It weighs 7.08mg luminol reagents and is dissolved in the sodium hydroxide solution of a concentration of 0.1mol/L of 4ml and be configured to
The luminol mother liquor of 0.1mol/L, and be kept in dark place at 4 deg. celsius;Needed for being diluted to Tris-HCl buffer solutions when use
The concentration wanted.
It is equipped with Tris-HCl buffer solutions
1 part of 1.211mg trishydroxymethylaminomethanes are weighed using electronic balance, are dissolved in the ultra-pure water of 75ml respectively
In, pH to 11 is adjusted respectively with the hydrochloric acid solution of 1mol/L, and 25mg ethylenediamine tetrems are added into each buffer solution mixed up respectively
Acid is settled to 1000ml, for use using ultra-pure water.
It is equipped with hydrogenperoxide steam generator
It using a concentration of 30% hydrogenperoxide steam generator as mother liquor, is positioned under 4 degrees Celsius and is kept in dark place, using super when use
Pure water is diluted to required concentration.
The measurement of S3, hydrogen peroxide
The luminol that luminol mother liquor obtained by configuring is diluted to 5 mMs every liter with Tris-HCl buffer solutions is molten
Then liquid takes the hydrogenperoxide steam generator of 40 microlitres of 5 mMs every liter of luminol solutions and 40 microlitres of various concentrations (can be with
Detection limit is determined by its concentration) mixing in measuring cup, then the MoS2 nanometer classes of 40 microlitres 1 mM every liter of addition thereto
Enzyme is put into chemical luminescence detector after reacting 30 seconds.It is collected by Chemiluminescence Apparatus and records optical signal caused by reaction.
Chemiluminescence Apparatus measures high pressure and is set as -900V, measures detection and is set as 0.05s, the integrated signal of 10s is gone to record.
As a result our detection limit is shown in 37 every liter of nanomoles, and than high 1 order of magnitude based on TMB, (it is in micromole
Every liter of 0.08 every liter of micromole of the order of magnitude-bibliography is that " Guo Xinrong, Ni Yongnian are based on molybdenum disulfide color developing detection peroxidating
Hydrogen ").
Fig. 1 can be with the stripping of secondary proof MoS2, it is clear that it typical case occurs near 430nm, 610nm, 670nm wavelength
Single layer or few layer MoS2 characteristic peaks, it was demonstrated that the presence of MoS2 two-dimensional nano fermentoids.Fig. 2 is typical MoS2 two-dimensional nanos fermentoid shape
Looks figure, the left side are for few layer of structure, and the right is single layer structure, very close with base color, indicate that lamella is thinner, closer
Single layer structure.
2) fluorometric investigation result data
When MoS2 two-dimensional nano fermentoids detection hydrogen peroxide is not added and addition MoS2 two-dimensional nano fermentoids detect peroxide
It is being to show glow peak at 450nm spectrum in wavelength when changing hydrogen, it is meant that MoS2/ luminols luminescence system can detect really
Hydrogen oxide, while being added when MoS2 two-dimensional nano fermentoids detect hydrogen peroxide and shining peak intensity at 2000 units, without adding
Intensity is only 500 units when entering MoS2 two-dimensional nano fermentoids detection hydrogen peroxide, it is clear that MoS2 two-dimensional nano fermentoid energy pole is added
Big enhancing luminous signal intensity.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (1)
1. detecting the new method of hydrogen peroxide based on MoS2 nanometers of fermentoid luminescence systems, it is characterised in that:Include the following steps:
S1, MoS2 two-dimensional nano fermentoids are prepared
50mgMoS2 is added in the 10ml aqueous solutions containing 10mg bovine serum albumins (BSA), using gun-type ultrasonic probe in work(
After rate is ultrasonically treated 6h under conditions of being 240W, the speed centrifugation 45min with 5000r/min is placed in supercentrifuge, logical
Be cleaned by ultrasonic bathe in ultrasound disperse 10min again, then with 15000r/min speed centrifuge 45min, collect supernatant, 4 degree
Under save backup;
S2, luminol solution and Tris-HCl buffer solutions are prepared
Prepare luminol solution
It weighs 7.08mg luminol reagents and is dissolved in the sodium hydroxide solution of a concentration of 0.1mol/L of 4ml and be configured to 0.1mol/L's
Luminol mother liquor, and be kept in dark place at 4 deg. celsius;
Prepare Tris-HCl buffer solutions
1.211mg trishydroxymethylaminomethanes are weighed, are dissolved in the ultra-pure water of 75ml, with the hydrochloric acid solution point of 1mol/L
Not Tiao pH to 11,25mg ethylenediamine tetra-acetic acids are added, ultra-pure water is settled to 1000ml, for use;
The measurement of S3, hydrogen peroxide
Luminol mother liquor obtained by preparing is diluted to 5 mMs every liter of luminol solution with Tris-HCl buffer solutions, so
The hydrogenperoxide steam generator of 40 microlitres of acquired solutions and 40 microlitres of various concentrations mixing in measuring cup is taken afterwards, then 40 are added thereto
Microlitre 1 mM every liter of MoS2 nanometer fermentoids are put into chemical luminescence detector, are received by Chemiluminescence Apparatus after reaction 30 seconds
Collect and record optical signal caused by reaction, the characteristic signal frequency peak and peak intensity composed by optical signal quantify hydrogen peroxide.
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Cited By (1)
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CN115779965A (en) * | 2022-11-15 | 2023-03-14 | 陕西科技大学 | MoS with antibacterial property and potential tumor inhibition property 2 Preparation method and application of nano enzyme |
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