CN115260521B - Ratio type palladium-methylene blue coordination polymer nano probe, preparation method and application - Google Patents
Ratio type palladium-methylene blue coordination polymer nano probe, preparation method and application Download PDFInfo
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Abstract
The invention discloses a ratio type palladium-methylene blue coordination polymer nano-probe (PdMBCPsNSs), which is synthesized by taking palladium chloride, sodium bromide and methylene blue as main raw materials and adopting a green photochemical synthesis method in a room temperature water phase. The invention also discloses a preparation method and application of the ratio type palladium-methylene blue coordination polymer nano probe. The invention has the beneficial effects that: high-selectivity and high-sensitivity detection of alkaline phosphatase (ALP) is realized, and the detection limit is 0.013U/L and 1.22U/L; the preparation process is simple and quick, and does not need heating and complex post-treatment steps; the palladium-methylene blue nano-sheet synthesized in the room temperature water phase is stable and has good dispersibility.
Description
Technical Field
The invention relates to the technical field of nano biosensing, in particular to a ratio type palladium-methylene blue coordination polymer nano probe (PdMBCPsNSs), a preparation method and application.
Background
Alkaline phosphatase (ALP) is widely used for diagnosis and treatment of human diseases as an important biomarker and an effective therapeutic target. ALP is distributed throughout the liver, kidney, bone, intestine, and other tissues and organs. ALP is involved in a variety of physiological processes in the organism, such as cell division, immune response, endotoxin detoxification, bone mineralization, etc., by catalyzing the phosphoester hydrolysis reaction of nucleic acids, proteins and other substrates under alkaline conditions. In recent years, ALP levels have been closely related to diseases of liver, bone tissue, prostate, endocrine system, etc., and thus can be a potential target for these diseases. Currently, the main etiology of ALP elevation clinically is: 1) Malignant tumors such as pancreatic head cancer, bile duct cancer, primary hepatocellular carcinoma, etc. 2) Gall stones, cholecystitis, sclerosing cholangitis, other inflammations, etc. In contrast, reduced ALP levels are mainly found in chronic glomerulonephritis, malnutrition, thyroid dysfunction, magnesium deficiency, severe anemia and other diseases. Therefore, establishing a highly sensitive and accurate ALP quantitative analysis method is important for early clinical diagnosis and prognosis of the above diseases.
In recent years, a variety of advanced ALP detection methods have been reported, including fluorescence, electrochemical, electrochemiluminescence, raman scattering analysis, inductively coupled plasma mass spectrometry, and the like. Although the above methods have high sensitivity and precision, they still have some limitations such as complex procedures, long detection times, large and expensive equipment, and the need for trained operators. This not only severely limits the detection applications in mobile work environments or in specific healthcare facilities, but the high detection costs can be prohibitive for some patients, especially in developing countries and resource-limited areas. In view of these problems, the point-of-care testing (POCT) method is a convenient, fast and practical technique, which can greatly remedy the shortcomings of the above analysis methods in the fields of disease diagnosis, health management, environmental monitoring, emergency response analysis, and the like. Therefore, there is an urgent need to develop new simple, portable, low cost, ALP point-of-care strategies to meet modern clinical diagnostic needs in resource-constrained environments.
New portable ALP analysis methods based on a few simple signals (e.g. color, temperature, pressure, weight, distance, etc.) are widely appreciated by researchers. Colorimetry is an analytical method based on color change signals. Colorimetric methods based on the formation of colored products from ALP-catalyzed substrates are widely used in clinical trials due to their simplicity and low cost. However, colorimetry is not sensitive due to its low color resolution and is susceptible to interference from other substances. Multimode detection is essential in order to build a more efficient POCT platform. The multi-mode detection method can realize accurate identification of a single target according to different detection methods. Because the detection mechanisms are different, the signal conversion is independent, so that the multi-mode detection method can combine the advantages of various detection modes, and further provides accurate quantitative detection results.
In view of the above, a simple, stable, high-sensitivity dual-mode ALP quantitative detection method needs to be developed.
Disclosure of Invention
The invention discloses a ratio type palladium-methylene blue coordination polymer nano probe (PdMBCPsNSs), a preparation method and application thereof, wherein the ratio type PdMBCPsNSs with good stability can be prepared through mild synthesis conditions and simple synthesis steps, and the ratio type palladium-methylene blue coordination polymer nano probe is prepared through a ratio type absorbance value A 660 /A 808 Ratio-type temperature value T 660 /T 808 The linear relation with the concentration realizes the instant detection of ALP without complex instruments and operation programs, and can effectively solve the technical problems related to the background technology.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a ratio type palladium-methylene blue coordination polymer nano-probe is synthesized by taking palladium chloride, sodium bromide and methylene blue as main raw materials and adopting a green photochemical synthesis method in a room temperature water phase.
The invention also provides a preparation method of the ratio type palladium-methylene blue coordination polymer nano probe, which comprises the following steps:
step one, preparing a palladium chloride solution: adding a certain amount of palladium chloride solid powder and a certain volume of concentrated hydrochloric acid into deionized water to fix the volume, and slightly shaking until the solution is uniform to form a palladium chloride solution;
step two, preparing methylene blue solution: adding a certain amount of methylene blue solid powder into deionized water, fixing the volume, and slightly shaking to be uniform to form a methylene blue solution;
step three, synthesizing ratio type PdMBCPsNSs: a certain volume of palladium chloride solution, a certain weight of sodium bromide and a certain volume of methylene blue solution are sequentially added into an EP tube, and a xenon lamp is used for irradiating for a certain time to obtain the ratio type pdMBCPsNSs.
As a preferred modification of the present invention, in step one, 17.73mg of palladium chloride solid powder and 100. Mu.L of concentrated hydrochloric acid are added to deionized water to a volume of 100mL and gently shaken to homogeneity to form a palladium chloride solution.
As a preferred modification of the present invention, in step two, 37.39mg of methylene blue solid powder was added to deionized water and the volume was set to 100mL, and gently shaken to homogeneity to form a methylene blue solution.
As a preferred modification of the present invention, in step three, 10mL of a palladium chloride solution, 5mg of sodium bromide and 3.5mL of a methylene blue solution were sequentially added to an EP tube, and irradiated with a xenon lamp for 60 minutes to obtain ratiometric PdMBCPsNSs.
The invention also provides an application of the ratio type PdMBCPsNSs prepared by the preparation method of the ratio type palladium-methylene blue coordination polymer nano-probe, and the ratio type PdMBCPsNSs is used for colorimetric/temperature dual-mode detection of ALP.
As a preferred improvement of the present invention, the colorimetric/temperature dual mode detection specifically comprises the following detection steps:
(1) Adding ratio type PdMBCPsNSs and ascorbyl phosphate (AAP) into Tris-HCl buffer solution to obtain a detection reagent;
(2) Preparing a standard solution of ALP: preparing ALP solutions with the concentration of 0.5U/L, 1.0U/L, 1.5U/L, 2.0U/L, 2.5U/L, 3.0U/L, 5.0U/L, 7.5U/L, 10.0U/L and 12.5U/L respectively by taking Tris-HCl buffer solution as a solvent, and preserving at room temperature;
(3) Adding ALP solutions of different concentrations to the detection reagent of step (1), at 37 o Incubating for 10min under the water bath condition;
(4) Ultraviolet spectrum test is carried out by an ultraviolet spectrophotometer according to the ratioAbsorbance value a of the ratio 660 /A 808 Quantitative detection of ALP by the change;
(5) The temperature change was collected by a thermal infrared imager and the color change of the solution was observed by irradiating with a laser of 808nm or 660nm for 10 min.
The beneficial effects of the invention are as follows:
1. the colorimetric/temperature dual-mode detection method provided by the invention realizes the detection of ALP with high selectivity and high sensitivity, and the detection limit reaches 0.013U/L and 1.22U/L;
2. under the catalytic hydrolysis of ALP, AAP can be rapidly decomposed into Ascorbic Acid (AA), so that methylene blue is released by competitive substitution, different ultraviolet absorption peaks, photothermal effects and color changes are generated, and detection of ALP with different concentrations is realized;
3. palladium chloride, sodium bromide and methylene blue are used as raw materials, and a green photochemical synthesis method is used for reacting in a room-temperature water phase to generate blue-green ratio type PdMBCPsNSs, so that the preparation process is simple and quick, and heating and complex post-treatment steps are not needed;
4. the ratio type PdMBCPsNSs synthesized in the aqueous phase at room temperature is stable and has good dispersibility.
Drawings
For a clearer description of the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly introduced below, it being obvious that the drawings in the description below are only some embodiments of the present invention, and that other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art, wherein:
FIGS. 1 (a) - (c) are schematic diagrams showing the synthetic routes and principles of the ratio-type PdMBCPsNSs of example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of the ratio-type pdMBCPsNSs in example 2 of the present invention;
FIG. 3 is an ultraviolet spectrum of ratio-type PdMBCPsNSs and MB in example 2 of the present invention;
FIG. 4 is an infrared spectrum of ratio-type PdMBCPsNSs and MB in example 2 of the present invention;
FIGS. 5 (a) - (d) are X-ray photoelectron spectra of ratio-type PdMBCPsNSs and MB in example 2 of the present invention;
FIG. 6 is an X-ray diffraction pattern of ratio-type PdMBCPsNSs and MB in example 2 of the present invention;
FIGS. 7 (a) - (d) are graphs showing the results of photo-thermal performance testing of the ratiometric PdMBCPsNSs of example 3 under 808nm laser light;
FIGS. 8 (a) - (c) are graphs showing the results of photo-thermal performance testing of the ratiometric PdMBCPsNSs of example 3 under 660nm laser light;
FIGS. 9 (a) - (c) are graphs showing UV spectra of different concentrations of ALP from the ratio-type pdMBCPsNSs of example 4 of the present invention;
FIGS. 10 (a) - (c) are graphs showing the results of the measurement of ALP at various concentrations by 808nm/660nm laser irradiation ratio type pdMBCPsNSs in example 4 of the present invention;
FIG. 11 is a graph showing the effect of different types of buffer solutions on ALP detection in example 5 of the present invention;
FIG. 12 is a graph showing the effect of pH of different buffer solutions on ALP detection in example 6 of the present invention;
FIG. 13 is a graph showing the effect of different ratio type pdMBCPsNSs concentrations on ALP detection effect in example 7 of the present invention;
FIG. 14 is a graph showing the effect of different AAP concentrations on ALP measurement in example 8 of the present invention;
FIG. 15 is a graph showing the effect of different enzyme catalysis times on ALP detection effect in example 9 of the present invention;
FIG. 16 is a graph showing the effect of different enzyme catalytic temperatures on ALP detection in example 10 of the present invention;
FIGS. 17 (a) and (b) are graphs showing the anti-interference ability and selectivity of ALP detection methods in examples 11 and 12, respectively, according to the present invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In addition, the technical solutions of the embodiments of the present invention may be combined with each other, but it is necessary to be based on the fact that those skilled in the art can implement the technical solutions, and when the technical solutions are contradictory or cannot be implemented, the combination of the technical solutions should be considered as not existing, and not falling within the scope of protection claimed by the present invention.
The invention provides a ratio type palladium-methylene blue coordination polymer nano-probe which is synthesized by taking palladium chloride, sodium bromide and methylene blue as main raw materials and adopting a green photochemical synthesis method in a room temperature water phase.
The ratio-type PdMBCPsNSs provided by the present invention will be described in detail below with reference to specific examples 1 to 11.
Example 1
Referring to fig. 1 (a), the present invention provides a preparation method of a ratio type palladium-methylene blue coordination polymer nano probe, which comprises the following steps:
step one, preparing a 1mM palladium chloride solution: 17.73mg of palladium chloride solid powder and 100 mu L of concentrated hydrochloric acid are added into deionized water to fix the volume to 100mL, and the mixture is gently shaken to be uniform, so that a palladium chloride solution (1 mM) is formed;
step two, preparing a 1mM methylene blue solution: 37.39mg of methylene blue solid powder was added to deionized water and the volume was set to 100mL, and gently shaken to homogeneity to form a methylene blue solution (1 mM);
step three, synthesizing ratio type PdMBCPsNSs: to the EP tube, 10mL of a palladium chloride solution, 5mg of sodium bromide and 3.5mL of a methylene blue solution were sequentially added, and the mixture was irradiated with a xenon lamp for 60 minutes to obtain ratiometric PdMBCPsNSs.
Example 2
Characterization of ratio pdmbcpsss:
(1) And taking a certain amount of ratio type PdMBCPsNSs for vacuum drying, and using a scanning electron microscope for characterization, wherein the nano-sheet growth is completed when the illumination time is 5 min. As shown in FIG. 2, it can be seen from a scanning electron microscope that the prepared coordination polymer PdMBCPsNSs has a leaf-shaped structure with uniform size and monodisperse distribution and is approximately two-dimensional lamellar.
(2) Taking a certain amount of ratio type PdMBCPsNSs and MB for ultraviolet absorption spectrum test, and finding that the coordination polymer has absorption at near infrared 808nm, as shown in figure 3; an infrared absorption spectrum test was performed by taking a certain amount of ratio type pdmbcpssss and MBs, as shown in fig. 4. It was found that the ratio type PdMBCPsNSs was 407cm compared to MB -1 And a new absorption peak appears, which indicates that the palladium ion is successfully coordinated with the N atom in MB, and the primary synthesis of the ratio type PdMBCPsNSs is successful.
(3) X-ray photoelectron spectroscopy is carried out by taking a certain amount of ratio type PdMBCPsNSs and MB, and corresponding sulfur, palladium and nitrogen elements are confirmed to exist in the X-ray photoelectron spectroscopy of the ratio type PdMBCPsNSs, as shown in fig. 5 (a) - (d).
(4) X-ray diffraction pattern analysis was performed on a certain amount of ratio type PdMBCPsNSs and MBs, confirming that the ratio type PdMBCPsNSs were successfully synthesized, as shown in fig. 6.
Example 3
Photo-thermal performance test of ratiometric pdmbcpssss:
(1) Different amounts of ratio type PdMBCPsNSs were added to deionized water to prepare ratio type PdMBCPsNSs aqueous dispersion with different concentrations. After uniform dispersion, detection was performed at room temperature using an ultraviolet spectrophotometer.
(2) Under the irradiation of 808nm or 660nm lasers with different optical power densities, the aqueous dispersion of the ratio type PdMBCPsNSs (30 mug/mL) is respectively irradiated for 10min, and a thermal infrared imager is used for collecting temperature change and drawing a time-temperature change curve. It can be observed that the temperature increases with the increase of the power density of a 808nm or 660nm laser after the irradiation of the ratio type PdMBCPsNSs for 10min, has good photo-thermal conversion effect, and finally selects 1.5W/cm 2 、0.4W/cm 2 The optimal optical power densities of the laser experiments are 808nm and 660nm respectively.
(3) PdMBCPsNS with different concentration ratiosThe s-aqueous dispersion was laser light at 808nm (optical power density 1.5W/cm 2 ) And 660nm laser (optical power density of 0.4W/cm) 2 ) Time-temperature profile under irradiation. It can be observed that the temperature increases with the increase of the concentration of the aqueous dispersion of the ratio-type PdMBCPsNSs after 5min of the ratio-type PdMBCPsNSs under the irradiation of 808nm or 660nm laser, and 30 μg/mL is finally selected as the optimal concentration for the test of the photo-thermal property.
(4) To investigate the photo-thermal stability of the ratiometric PdMBCPsNSs coordination polymer, the light power density was measured at 808nm (1.5W/cm 2 ) Or 660nm laser (optical power density of 0.4W/cm) 2 ) The heating-cooling curve was obtained after three cycles of irradiation of the aqueous dispersion of PdMBCPsNSs (30. Mu.g/mL), and it was concluded that the coordination polymer had better stability.
Fig. 7 (a) - (d) are graphs of various results of photo-thermal performance tests of ratiometric PdMBCPsNSs under 808nm laser light.
Fig. 8 (a) - (c) are graphs of various results of photo-thermal performance tests of ratiometric PdMBCPsNSs under 660nm laser light.
Example 4
The invention also provides an application of the ratio type PdMBCPsNSs prepared by the preparation method of the ratio type palladium-methylene blue coordination polymer nano-probe, and the ratio type PdMBCPsNSs is used for colorimetric/temperature dual-mode detection of ALP.
The colorimetric/temperature dual-mode detection specifically comprises the following detection steps:
(1) Adding ratio type PdMBCPsNSs and AAP into Tris-HCl buffer solution to obtain a detection reagent;
(2) Preparing a standard solution of ALP: preparing ALP solutions with the concentration of 0.5U/L, 1.0U/L, 1.5U/L, 2.0U/L, 2.5U/L, 3.0U/L, 5.0U/L, 7.5U/L, 10.0U/L and 12.5U/L respectively by taking Tris-HCl buffer solution as a solvent, and preserving at room temperature;
(3) Adding ALP solutions of different concentrations to the detection reagent of step (1), at 37 o Incubating for 10min under the water bath condition;
(4) Ultraviolet spectrum test is carried out by an ultraviolet spectrophotometer according to the ratio typeAbsorbance value a 660 /A 808 Quantitative detection of ALP by the change, the results are shown in FIGS. 9 (a) - (c);
(5) With 808nm (optical power density of 1.5W/cm) 2 ) Or 660nm laser (optical power density of 0.4W/cm) 2 ) Irradiating for 10min, and collecting temperature change and observing color change of the solution by using a thermal infrared imager.
For this step (5), it should be further explained that, referring to fig. 1 (b) - (c), the principle of the ratio PdMBCPsNSs for colorimetric/temperature dual-mode detection of ALP in the present invention is as follows:
the ratio type PdMBCPsNSs has two characteristic absorption peaks at 808nm and 660nm, and MB has a strong characteristic absorption peak at 660 nm. ALP, when present, is capable of catalyzing dephosphorylation of AAP to produce AA. The generated AA can compete for replacing MB in the ratio type PdMBCPsNSs, so that the MB is released into the solution, and therefore the absorption at 808nm is weakened, and the absorption at 660nm is enhanced; at the same time, the color of the solution system is changed from the initial grey green to deep blue. The temperature of the system is correspondingly reduced/increased when the 808nm/660nm laser is used for irradiation. Therefore, the absorbance value A is based on the absorption and color transition of the ratiometric PdMBCPsNSs 660 /A 808 Ratio-type temperature value T 660 /T 808 And the color change can rapidly and sensitively detect ALP. By utilizing the obvious color and photo-thermal signal change generated in the process, an ALP ultrasensitive colorimetric/temperature dual-mode detection method based on coordination competition is constructed.
The concentration of ALP solution is taken as the abscissa, and the absorbance value A is taken as the ratio 660 /A 808 Drawing a standard curve for the ordinate, and a regression equation of the standard curve: y=0.15669x+0.84103, correlation coefficient R 2 0.99898 the ALP solution concentration is taken as abscissa and the temperature T is measured as the ratio 660 /T 808 Drawing a standard curve for the ordinate, and a regression equation of the standard curve: y=0.30733x+0.79431, correlation coefficient R 2 = 0.99179. The detection limits were 0.013U/L and 1.22U/L, respectively.
Fig. 10 (a) - (c) are graphs of the detection results of ALP standard solutions of different concentrations (thermal infrared imager as signal acquisition).
Example 5:
examine the effect of different kinds of buffer solutions on the detection effect:
the ratio of PdMBCPsNSs and AAP were added to phosphate buffer (10 mM, pH 7.4), tris-HCl buffer (10 mM, pH 7.4) and HAc/NaAc buffer (0.2M, pH 7.4), respectively, and the assay was performed as in example 4.
The detection results are shown in fig. 11: the absorbance change was the largest and the signal was the strongest in Tris-HCl buffer. Therefore, tris-HCl buffer was chosen as the optimal buffer in the subsequent examples.
Example 6:
examine the effect of buffer solution pH on detection effect:
ratio type PdMBCPsNSs and AAP were added to Tris-HCl buffer (10 mM) and Tris-HCl pH was 6.8, 7.0, 7.2, 7.4, 7.6, 7.8 and 8.0, respectively, and tested as in example 4. The detection results are shown in fig. 12: the absorbance change was greatest and the signal was strongest when the Tris-HCl buffer pH was 7.4-. Thus, tris-HCl buffer (pH 7.4) was selected as the optimal pH in the subsequent examples.
Example 7:
the effect of the ratio-type PdMBCPsNSs concentration on the detection effect was examined:
the ratio type PdMBCPsNSs and AAP were added to Tris-HCl buffer to prepare detection reagents with different concentrations, wherein the concentrations of the ratio type PdMBCPsNSs were 0 mug/mL, 16.7 mug/mL, 33.3 mug/mL, 50.0 mug/mL, 66.7 mug/mL and 83.3 mug/mL, respectively, and the concentrations of AAP were 0.55mM. The test was carried out as described in example 4. The detection results are shown in fig. 13: the absorbance change was appropriate at a ratio-type PdMBCPsNSs concentration of 50.0 μg/mL. Thus, 50.0. Mu.g/mL was chosen as the concentration of PdMBCPsNSs for the UV spectrum test in the subsequent examples.
Example 8:
and (3) examining the influence of the concentration of the AAP solution on the detection effect:
AAP is dissolved in Tris-HCl buffer solution to prepare AAP solutions with different concentrations: 0.1mM, 0.2mM, 0.3mM, 0.4mM, 0.45mM, 0.5mM, 0.55mM, 0.6mM and 0.65mM. The procedure of example 4 was followed, and AAP solutions of different concentrations were added for detection. The detection results are shown in fig. 14: the absorbance change was greatest and the signal was strongest at an AAP concentration of 0.55mM in the detection reagent. Thus, 0.55mM was chosen as the optimal AAP solution concentration in the subsequent examples.
Example 9:
and (3) examining the influence of enzyme catalytic reaction time on the detection effect:
the test solution was added to Tris-HCl buffer containing ratio type pdMBCPsNSs and AAP according to the procedure of example 4, and reacted for 0min, 5min, 10min, 15min, 20min and 25min, respectively, and the influence of enzyme catalytic reaction time on the detection result was examined. The detection results are shown in fig. 15: the absorbance change value gradually rises along with the extension of the reaction time, and reaches an ideal state when reaching 10 min. Therefore, 10min was chosen as the optimal enzyme catalytic reaction time in the subsequent examples.
Example 10:
and (3) observing the influence of the enzyme catalytic reaction temperature on the detection effect:
the test solution was added to Tris-HCl buffer containing ratio-type PdMBCPsNSs and AAP according to the procedure of example 4 at a reaction temperature of 22, respectively o C、27 o C、32 o C、37 o C、42 o C and 47 o And C, examining the influence of the enzyme catalytic reaction temperature on the detection result. The detection results are shown in fig. 16: with the increase of the reaction temperature, the absorbance change value gradually increases to 37 o At the temperature C, the absorbance change value reaches the maximum. Thus choose 37 o The temperature C is the optimal enzyme catalytic reaction temperature in the subsequent examples.
Example 11:
investigation of anti-interference capability of the method:
1.5. Mu.L of ratio type PdMBCPsNSs (10 mg/mL) was added to 268.5. Mu.L of Tris-HCl buffer (10 mM, pH=7.4), and after mixing well, the same concentration of ALP solution and AAP solution was added to the mixed solution. Shaking up at 37 o After the reaction of C for 10min, comparing the reaction products by an ultraviolet spectrophotometerAnd (5) detecting the rate type absorbance. Several common enzymes (e.g. bovine serum albumin, glucose oxidase, horseradish peroxidase, trypsin, lysozyme), reducing biomolecules (e.g. glutathione, dopamine, cysteine), metal ions (e.g. K) were examined + 、Na + 、Ca 2+ 、Mg 2+ 、CO 3 2- 、SO 4 2- ) Interference level to ALP. The result shows that the method has good anti-interference capability on ALP. All enzymes were 20 times ALP, 50 μm in concentration of reducing biomolecules and 0.1mM in concentration of ions. The results are shown in FIG. 17 (a).
Example 12:
the selectivity of the method is examined:
1.5. Mu.L of ratio-type PdMBCPsNSs (10 mg/mL) was added to 268.5. Mu.L of Tris-HCl buffer (10 mM, pH=7.4), and after mixing well, the AAP solution at the same concentration was added to the mixed solution. Shaking up at 37 o After 10mins of reaction C, the absorbance of the sample was measured by a ratio type ultraviolet spectrophotometer. Several common enzymes (e.g. bovine serum albumin, glucose oxidase, horseradish peroxidase, trypsin, lysozyme), reducing biomolecules (e.g. glutathione, dopamine, cysteine), metal ions (e.g. K) were examined + 、Na + 、Ca 2+ 、Mg 2+ 、CO 3 2- 、SO 4 2- ) Interference level to ALP. The results show that the method has higher selectivity to ALP. All enzymes were 20 times ALP, 50 μm in concentration of reducing biomolecules and 0.1mM in concentration of ions. The results are shown in FIG. 17 (b).
The beneficial effects of the invention are as follows:
1. the colorimetric/temperature dual-mode detection method provided by the invention realizes the detection of ALP with high selectivity and high sensitivity, and the detection limit is 0.013U/L and 1.22U/L;
2. under the catalytic hydrolysis of ALP, AAP can be rapidly decomposed into AA, so that methylene blue is released by competitive substitution, different ultraviolet absorption peaks, photothermal effects and color changes are generated, and detection of ALP with different concentrations is realized, and the results are shown in figures 9 and 10;
3. palladium chloride, sodium bromide and methylene blue are used as raw materials, and a green photochemical synthesis method is used for reacting in a room-temperature water phase to generate blue-green ratio type PdMBCPsNSs, so that the preparation process is simple and quick, and heating and complex post-treatment steps are not needed;
4. the ratio type PdMBCPsNSs synthesized in the aqueous phase at room temperature is stable and has good dispersibility.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown and described, it is well suited to various fields of use for which the invention would be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the specific details and illustrations shown and described herein, without departing from the general concepts defined in the claims and their equivalents.
Claims (7)
1. The ratio type palladium-methylene blue coordination polymer nano probe is characterized in that the ratio type palladium-methylene blue coordination polymer nano probe is synthesized by adopting palladium chloride, sodium bromide and methylene blue as main raw materials and adopting a photochemical synthesis method of irradiating a xenon lamp for a certain time in a room temperature water phase.
2. A preparation method of a ratio type palladium-methylene blue coordination polymer nano probe is characterized by comprising the following steps: the preparation method comprises the following steps:
step one, preparing a palladium chloride solution: adding a certain amount of palladium chloride solid powder and a certain volume of concentrated hydrochloric acid into deionized water to fix the volume, and slightly shaking until the solution is uniform to form a palladium chloride solution;
step two, preparing methylene blue solution: adding a certain amount of methylene blue solid powder into deionized water, fixing the volume, and slightly shaking to be uniform to form a methylene blue solution;
step three, synthesizing a ratio type palladium-methylene blue coordination polymer nano probe: and sequentially adding a certain volume of palladium chloride solution, a certain weight of sodium bromide and a certain volume of methylene blue solution into an EP tube, and irradiating for a certain time by using a xenon lamp to obtain the palladium-methylene blue coordination polymer nano probe.
3. The method for preparing the ratio-type palladium-methylene blue coordination polymer nano probe according to claim 2, which is characterized in that: in step one, 17.73mg of palladium chloride solid powder and 100 μl of concentrated hydrochloric acid were added to deionized water to fix the volume to 100mL, and gently shaken to uniformity to form a palladium chloride solution.
4. The method for preparing the ratio-type palladium-methylene blue coordination polymer nano probe according to claim 2, which is characterized in that: in step two, 37.39mg of methylene blue solid powder was added to deionized water and the volume was set to 100mL, and gently shaken to homogeneity to form a methylene blue solution.
5. The method for preparing the ratio-type palladium-methylene blue coordination polymer nano probe according to claim 2, which is characterized in that: in the third step, 10mL of palladium chloride solution, 5mg of sodium bromide and 3.5mL of methylene blue solution are sequentially added into an EP tube, and the mixture is irradiated by a xenon lamp for 60min to obtain the ratio type palladium-methylene blue coordination polymer nano probe.
6. Use of a ratio-type palladium-methylene blue coordination polymer nanoprobe prepared by the preparation method of the ratio-type palladium-methylene blue coordination polymer nanoprobe according to any one of claims 2 to 5, which is characterized in that: the ratio type palladium-methylene blue coordination polymer nano-probe is used for carrying out colorimetric/temperature dual-mode detection on alkaline phosphatase.
7. The use of a ratio-based palladium-methylene blue coordination polymer nanoprobe according to claim 6, wherein: the colorimetric/temperature dual-mode detection specifically comprises the following detection steps:
(1) Adding a ratio type palladium-methylene blue coordination polymer nano probe and ascorbyl phosphate into Tris-HCl buffer solution to obtain a detection reagent;
(2) Preparing a standard solution of alkaline phosphatase: preparing alkaline phosphatase solutions with the concentration of 0.5U/L, 1.0U/L, 1.5U/L, 2.0U/L, 2.5U/L, 3.0U/L, 5.0U/L, 7.5U/L, 10.0U/L and 12.5U/L respectively by taking Tris-HCl buffer solution as a solvent, and preserving at room temperature;
(3) Adding alkaline phosphatase solutions of different concentrations to the detection reagent of step (1), at 37 o Incubating for 10min under the water bath condition;
(4) Ultraviolet spectrum test is carried out by an ultraviolet spectrophotometer, and the absorbance value A is according to the ratio 660 /A 808 Quantitative detection of alkaline phosphatase by change;
(5) The temperature change was collected by a thermal infrared imager and the color change of the solution was observed by irradiating with a laser of 808nm or 660nm for 10 min.
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