CN111961462B - ZIF-8 coated gold nanocluster material and preparation method and application thereof - Google Patents
ZIF-8 coated gold nanocluster material and preparation method and application thereof Download PDFInfo
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- G01N21/64—Fluorescence; Phosphorescence
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Abstract
The invention discloses a ZIF-8 coated gold nanocluster material, which comprises the following specific components in percentage by weight: the metal organic framework ZIF-8 is used as an outer frame, AuNCs is coated in the outer frame, and in the gold nanocluster material coated with the ZIF-8, the ratio of Au to Zn is 0.01063112; the synthesis conditions of the ZIF-8 coated gold nanocluster material are mild, the obtained ZIF-8 coated gold nanocluster material can be used for detecting the content of vitamin C, and the detection limit of the vitamin C reaches 0.05-5 mu mol/L; compared with the existing detection means of the fluorescent probe, the fluorescent probe has the advantages of good fluorescence performance, long fluorescence life, longer service life and good practicability.
Description
Technical Field
The invention relates to the field of gold nanocluster materials. More specifically, the invention relates to a ZIF-8 coated gold nanocluster material as well as a preparation method and application thereof.
Background
Vitamin C (Vitamin C/ascorbyl acid, also known as L-ascorbic acid, also translated as Vitamin C) is an essential nutrient for higher primates and other minor organisms. Is a vitamin present in food and can be used as a nutritional supplement. Vitamin C is produced metabolically in most organisms, but with many exceptions, e.g. humans, vitamin C deficiency can lead to scurvy.
Therefore, the method for efficiently and rapidly detecting the vitamin C in the tablets is established, and is beneficial to quality monitoring of vitamin C health products.
In the prior art, the detection means for vitamin C mainly include: iodometry, titrimetry, high performance liquid chromatography, electrochemistry, spectrophotometry, fluorescence spectroscopy, and the like.
The fluorescence spectrum method is widely applied to the advantages of good selectivity, high efficiency, simple sample pretreatment, no damage to samples, low cost and the like.
Common vitamin fluorescence spectrum detection methods include: the method comprises the following steps of taking fluorescence resonance energy transfer or fluorescence internal filtering effect as a detection platform, constructing a probe by using two materials, and interrupting the fluorescence resonance energy transfer process or the fluorescence internal filtering effect by using the reducibility of vitamin to consume an energy receptor so as to realize the detection of vitamin C; therefore, it is highly desirable to construct a fluorescent probe with better selectivity and higher sensitivity.
Disclosure of Invention
It is an object of the present invention to address at least the above problems and to provide at least the advantages described hereinafter.
It is still another object of the present invention to provide a ZIF-8 coated gold nanocluster material, and a method for preparing the same and an application thereof, wherein the ZIF-8 coated gold nanocluster material can be obtained by using KMnO in an OFF-ON detection mode4Fluorescence of ZIF-8 coated gold nanoclusters is extinguished through fluorescence internal filtering effect, and KMnO is consumed by utilizing strong oxidizing property of vitamin C4The method has the advantages that the fluorescence internal filtering effect is reduced, the fluorescence of the ZIF-8 coated gold nanocluster is recovered, the simple and rapid sensitive detection of the vitamin C is realized, and the ZIF-8 coated gold nanocluster material has good fluorescence performance and long fluorescence life and has wide application prospect in the field of biomedicine.
To achieve these objects and other advantages in accordance with the present invention, there is provided a ZIF-8 coated gold nanocluster having a molecular formula AuNCs @ ZIF-8, in which a metal organic framework ZIF-8 is a frame in which AuNCs are embedded, and a ratio of Au/Zn content in the ZIF-8 coated gold nanocluster is 0.01063112.
A preparation method of ZIF-8 coated gold nanoclusters comprises the following steps:
s1, completely dissolving dimethyl imidazole in ultrapure water, adding zinc nitrate hexahydrate solution while stirring, stirring for 24 hours to obtain ZIF-8 mixed solution, centrifuging according to the volume ratio of the mixed solution to methanol of 1:1, and collecting precipitate; dispersing the collected precipitate in ultrapure water for later use, wherein the molar ratio of the dimethyl imidazole to the zinc nitrate hexahydrate is 65-85: 1;
s2, dissolving 11-mercaptoundecanoic acid in an aqueous solution of ZIF-8, adding dimethyl imidazole, glutathione, chloroauric acid and sodium hydroxide, stirring for 11 hours in the dark, adding absolute ethyl alcohol, centrifuging, and collecting precipitate to obtain AuNCs @ ZIF-8; wherein, dimethyl imidazole, 11-mercapto undecanoic acid, glutathione, HAuCl4The molar ratio of (A) is 99-101: 3-5: 1.
Preferably, the molar ratio of dimethylimidazole to zinc nitrate in S1 is 70: 1.
Preferably, dimethylimidazole, 11-mercaptoundecanoic acid, glutathione, HAuCl are mentioned as S24In a molar ratio of 100:4:4: 1.
An application of a ZIF-8 coated gold nanocluster material as a fluorescent probe for detecting the content of vitamin C in tablets.
Preferably, the specific detection steps are: dispersing the gold nanocluster storage solution coated with ZIF-8 in an N-2-hydroxyethylpiperazine-N' -2-ethanesulfonic acid buffer solution to obtain a gold nanocluster dispersion solution coated with ZIF-8; the ZIF-8 coated gold nanocluster solution is divided into a plurality of equal parts, and KMnO with the same concentration is added into each part4Incubating to obtain an empty sample; adding vitamin C standard solutions with different gradient volumes into each empty sample, reacting at room temperature, and measuring the fluorescence intensity of the mixed reaction system to obtain a standard curve; and taking an empty sample, adding the empty sample into the sample to be detected, reacting at room temperature, measuring the fluorescence intensity of the mixed reaction system, and contrasting with the standard curve to obtain the concentration of the vitamin C in the sample to be detected.
The invention at least comprises the following beneficial effects:
the ZIF-8 coated gold nanocluster material is obtained, the preparation method is simple, and the obtained gold nanocluster material is good in fluorescence performance and long in fluorescence life;
meanwhile, the ZIF-8 coated gold nanocluster material is applied to detection of vitamin C content by using KMnO4Fluorescence quenching of ZIF-8 coated gold nanoclusters by fluorescence internal filtering effect, and consumption of KMn by strong oxidizing property of vitamin CO4The fluorescence inner filtering effect is reduced, and the fluorescence recovery of the ZIF-8 coated gold nanocluster is an OFF-ON detection mode.
The vitamin C detection method has good fluorescence performance and long fluorescence life of the fluorescent probe, takes the stable ZIF-8 coated gold nanocluster as a detection platform, and uses KMnO4The method is used for regulating and controlling to realize simple, quick and sensitive detection of the vitamin C, and has lower detection limit compared with most of the conventional vitamin C detection methods.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is a graph of the fluorescence spectrum, UV-VIS absorption spectrum of ZIF-8 coated gold nanoclusters prepared in accordance with the present invention;
FIG. 2 is a transmission electron micrograph of ZIF-8 coated gold nanoclusters prepared according to the present invention;
FIG. 3 shows a ZIF-8 coated gold nanocluster-KMnO of an embodiment of the present invention4Standard curve diagram for vitamin C assay.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
< example 1>
A preparation method of ZIF-8 coated gold nanoclusters comprises the following steps:
s1, completely dissolving dimethyl imidazole in ultrapure water, adding zinc nitrate hexahydrate solution while stirring, stirring for 24 hours to obtain ZIF-8 mixed solution, centrifuging according to the volume ratio of the mixed solution to methanol of 1:1, and collecting precipitate; and dispersing the collected precipitate in ultrapure water for standby, wherein the molar ratio of dimethyl imidazole to zinc nitrate hexahydrate is 65: 1;
s2, dissolving 11-mercaptoundecanoic acid in ZIF-8 water solution, adding dimethyl imidazole, glutathione, chloroauric acid and sodium hydroxide, stirring in the dark for 11 hr, adding ethanol, and stirringCarrying out ethanol extraction, centrifuging and collecting the precipitate to obtain AuNCs @ ZIF-8; wherein, dimethyl imidazole, 11-mercapto undecanoic acid, glutathione, HAuCl4In a molar ratio of 99:3:3:3: 1.
< example 2>
A preparation method of ZIF-8 coated gold nanoclusters comprises the following steps:
s1, completely dissolving dimethyl imidazole in ultrapure water, adding zinc nitrate hexahydrate solution while stirring, stirring for 24 hours to obtain ZIF-8 mixed solution, centrifuging according to the volume ratio of the mixed solution to methanol of 1:1, and collecting precipitate; dispersing the collected precipitate in ultrapure water for standby, wherein the molar ratio of the dimethylimidazole to the zinc nitrate hexahydrate is 85: 1;
s2, dissolving 11-mercaptoundecanoic acid in a ZIF-8 aqueous solution, adding dimethyl imidazole, glutathione, chloroauric acid and sodium hydroxide, stirring for 11 hours in a dark place, adding absolute ethyl alcohol, centrifuging, and collecting a precipitate to obtain AuNCs @ ZIF-8; wherein, dimethyl imidazole, 11-mercapto undecanoic acid, glutathione, HAuCl4In a molar ratio of 101:5:5:5: 1.
< example 3>
A preparation method of ZIF-8 coated gold nanoclusters comprises the following steps:
s1, completely dissolving dimethyl imidazole in ultrapure water, adding zinc nitrate hexahydrate solution while stirring, stirring for 24 hours to obtain ZIF-8 mixed solution, centrifuging according to the volume ratio of the mixed solution to methanol of 1:1, and collecting precipitate; dispersing the collected precipitate in ultrapure water for standby, wherein the molar ratio of the dimethylimidazole to the zinc nitrate hexahydrate is 70: 1;
s2, dissolving 11-mercaptoundecanoic acid in an aqueous solution of ZIF-8, adding dimethyl imidazole, glutathione, chloroauric acid and sodium hydroxide, stirring for 11 hours in the dark, adding absolute ethyl alcohol, centrifuging, and collecting precipitate to obtain AuNCs @ ZIF-8; wherein, dimethyl imidazole, 11-mercapto undecanoic acid, glutathione, HAuCl4In a molar ratio of 100:4:4:4: 1.
< example 4> application to vitamin C content measurement
The AuNCs @ ZIF-8 obtained in the embodiment 3 is used as a fluorescent probe to detect the content of vitamin C in a sample to be detected;
the method comprises the following specific steps:
firstly, preparing an empty sample;
dispersing the gold nanoclusters coated with the ZIF-8 obtained in the embodiment 3 in ultrapure water, and storing to obtain a gold nanocluster storage solution coated with the ZIF-8;
dispersing the ZIF-8 coated gold nanocluster storage solution in an N-2-hydroxyethylpiperazine-N '-2-ethanesulfonic acid buffer solution, wherein the pH of the N-2-hydroxyethylpiperazine-N' -2-ethanesulfonic acid buffer solution is 7.4, and thus obtaining a ZIF-8 coated gold nanocluster dispersion solution with the concentration of 10-20 mmol/L; dividing the gold nanocluster solution coated with ZIF-8 into a plurality of parts, and adding KMnO with equal concentration to each part4Incubating the solution to obtain an empty sample;
wherein KMnO4The adding amount of the solution is 10-20 μ L, wherein 16 μ L is taken, the concentration is 0.1-1.5mmol/L, 0.5mmol/L is taken in the embodiment, the incubation time is 1-5min, and 5min is taken in the embodiment;
secondly, drawing a standard curve;
taking a plurality of empty samples, adding vitamin C standard solutions with different gradient volumes into each of the other empty samples except the first empty sample, reacting at room temperature for 8-15min, measuring the fluorescence intensity of the mixed reaction system at 595nm, taking the concentration of the vitamin C in the mixed reaction system as an abscissa, and comparing the recovered fluorescence intensity (F) of the mixed reaction system with the fluorescence intensity (F) of the probe0) As ordinate, AA-F/F was obtained0A standard curve;
wherein, the concentration of vitamin C in the mixed system is as follows in sequence:
0μmol/L、0.05μmol/L、0.1μmol/L、0.5μmol/L、1μmol/L、2μmol/L、3μmol/L、4μmol/L、5μmol/L、6μmol/L、7μmol/L、8μmol/L、9μmol/L、10μmol/L；
detecting the recovered fluorescence intensity (F) of the mixed reaction system and the fluorescence intensity (F) of the probe0) After the fluorescence intensity, the concentration of vitamin C in the mixed system was plotted on the abscissa, and the ratio of the recovered fluorescence intensity (F) of the mixed reaction system was calculatedFluorescence intensity (F) of the Probe0) As ordinate, AA-F/F was obtained0The standard curve is shown in FIG. 3;
preparing a sample solution to be detected, detecting the fluorescence intensity, and obtaining the detection concentration by contrasting a standard curve;
dispersing the gold nanocluster stock solution coated with ZIF-8 in hepes buffer solution with pH 7.4, adding 16 mu L0.5mmol/L KMnO into 2mL of the dispersion solution4Incubating for 5min, adding 2 μ L of solution obtained by dissolving 46.3mg Bulbus Lilii KANGPAVvitamin C buccal tablet in 5.26mL ultrapure water and diluting 25 times with 0.22 μm filter head, and detecting recovered fluorescence intensity (F) of mixed reaction system and fluorescence intensity of probe (F)0) After the fluorescence intensity, the recovered fluorescence intensity (F) of the mixed reaction system and the fluorescence intensity (F) of the probe were obtained0) The concentration of the vitamin C in the mixed system is obtained by contrasting the standard curve, and the average recovery rate is calculated; specific results are shown in tables 1 and 2;
TABLE 1
| Content of sample to be tested (mg) | Actual detection (mg) | Recovery (%) |
| 46.3 | 47.27 | 102.10 |
| 46.3 | 43.59 | 94.15 |
| 46.3 | 45.17 | 97.56 |
| 46.3 | 48.05 | 103.78 |
Examples of the experiments
Detection of fluorescence spectrum and ultraviolet-visible absorption spectrogram
The AuNCs @ ZIF-8 obtained in the example 3 is subjected to detection of a fluorescence spectrum and an ultraviolet-visible absorption spectrogram, and the detection result is shown in figure 1; it can be seen that the ultraviolet absorption peak is at 250nm, and the fluorescence intensity reaches the maximum value at 595nm, which is close to 860a.u.
Secondly, detection and detection of a transmission electron microscope
The AuNCs @ ZIF-8 obtained in the embodiment 3 is subjected to transmission electron microscope detection to obtain a TEM image, and the detection result is shown in FIG. 2; it can be seen that AuNCs @ ZIF-8 has a constant particle size and is uniformly loaded.
Third, atomic emission spectroscopy detection
Atomic emission spectroscopy detection is carried out on AuNCs @ ZIF-8 obtained in example 3, and detection elements are Au and Zn, so that the Au content is 44.9563mg/mL and the Zn content is 4228.745 mg/mL.
Sensitivity of four, ZIF-8 coated gold nanoclusters to vitamin C detection
The method is used for evaluating the detection linear range of the gold nano-material cluster material in the embodiment 3 by detecting the content of the vitamin C with different concentrations; the detection results are shown in Table 2;
TABLE 2
| Item | Content of sample to be tested (mg/g) | Detection concentration (M) | Mean. + -. SD (mg/g) | Average recovery. + -. SD (%) |
| 1 | 38.58mg/g | 5 | 41.56±0.33 | 107.72±0.86 |
| 2 | 38.58mg/ |
2 | 38.35±1.69 | 99.40±4.38 |
| 3 | 38.58mg/g | 0.5 | 38.00±2.17 | 99.17±6.71 |
The detection limit and the detection range of different types of fluorescent probes in different references for detecting the content of the vitamin C are compared, the detection means are fluorescence chromatograms, the specific result is shown in table 3, and the table 3 shows that the detection limit of the ZIF-8 coated gold nanocluster material of the invention for detecting the content of the vitamin C is relatively lower;
TABLE 3
Among them, references 1 to 8 are:
1、"Switch-On"Fluorescent Sensing of Ascorbic Acid in Food Samples Based on Carbon Quantum Dots–MnO2 Probe[J].Journal of Agricultural&Food Chemistry,2016,64(1):371.
2、A rapid microwave synthesis of nitrogen–sulfur co-doped carbon nanodots as highly sensitive and selective fluorescence probes for ascorbic acid[J].Talanta,2016,153:332-339.
3、Efficient Two-Photon Fluorescence Nanoprobe for Turn-On Detection and Imaging of Ascorbic Acid in Living Cells and Tissues[J].Analytical Chemistry,2016:6057.
4、A near-infrared luminescent Mn2+-doped NaYF4:Yb,Tm/Fe3+upconversion nanoparticles redox reaction system for the detection of GSH/Cys/AA[J].Talanta,2017,172:95.
5、Near Infrared Graphene Quantum Dots-Based Two-Photon Nanoprobe for Direct Bioimaging of Endogenous Ascorbic Acid in Living Cells[J].Analytical Chemistry,2017,89(7):4077-4084.
6、A dual-mode sensor for colorimetric and"turn-on"fluorescent detection of ascorbic acid[J].Dyes and Pigments,2018.
7、A Metal-Organic Framework as Selectivity Regulator for Fe3+and Ascorbic Acid Detection[J].Analytical Chemistry,2019,91(19).
8、A label-free nano-probe for sequential and quantitative determination of Cr(VI)and ascorbic acid in real samples based on S and N dual-doped carbon dots[J].Spectrochimica Acta Part A:Molecular and Biomolecular Spectroscopy,2019,215:58-68.
Dual-Response Detection of Oxidized Glutathione,Ascorbic Acid,and Cell Imaging Based on pH/Redox Dual-Sensitive Fluorescent Carbon Dots[J].ACS Omega 2020,5,9,4482–4489.
while embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable to various fields of endeavor for which the invention may be embodied with additional modifications as would be readily apparent to those skilled in the art, and the invention is therefore not limited to the details given herein and to the embodiments shown and described without departing from the generic concept as defined by the claims and their equivalents.
Claims (5)
1. A preparation method of a ZIF-8 coated gold nanocluster material is characterized by comprising the following steps of:
s1, dissolving dimethyl imidazole in ultrapure water completely, adding zinc nitrate hexahydrate solution while stirring, stirring for 24 hours to obtain ZIF-8 mixed solution, centrifuging the mixed solution and methanol according to the volume ratio of 1:1, and collecting precipitate; dispersing the collected precipitate in ultrapure water for later use, wherein the molar ratio of dimethyl imidazole to zinc nitrate hexahydrate is 65-85: 1;
s2, dissolving 11-mercaptoundecanoic acid in an aqueous solution of ZIF-8, adding dimethyl imidazole, glutathione, chloroauric acid and sodium hydroxide, stirring for 11 hours in the dark, adding absolute ethyl alcohol, centrifuging, and collecting precipitate to obtain AuNCs @ ZIF-8; wherein, dimethyl imidazole, 11-mercapto undecanoic acid, glutathione, HAuCl4The molar ratio of (1) to (2) is 99-101: 3-5: 1;
the molecular formula of the ZIF-8 coated gold nanocluster material is AuNCs @ ZIF-8, the ZIF-8 coated gold nanocluster material takes a metal organic framework ZIF-8 as an outer frame, AuNCs are coated in the outer frame, and the Au/Zn ratio in the ZIF-8 coated gold nanocluster material is 0.01063112.
2. The method of preparing a ZIF-8 coated gold nanocluster material of claim 1, wherein a molar ratio of dimethylimidazole to zinc nitrate in S1 is 70: 1.
3. The method of preparing a ZIF-8 coated gold nanocluster material of claim 1, wherein S2 is dimethyl imidazole, 11-mercaptoundecanoic acid, glutathione, HAuCl4In a molar ratio of 100:4:4: 1.
4. The use of the ZIF-8 coated gold nanocluster material obtained by the method for preparing a ZIF-8 coated gold nanocluster material as claimed in claim 1 as a fluorescent probe for detecting the vitamin C content in a tablet, wherein the detection limit of vitamin C is 0.05-5 μmol/L.
5. The use of claim 4, wherein the specific detection steps are: dispersing the gold nanocluster storage solution coated with ZIF-8 in an N-2-hydroxyethylpiperazine-N' -2-ethanesulfonic acid buffer solution to obtain a gold nanocluster dispersion solution coated with ZIF-8; the gold nanocluster solution coated with ZIF-8 is divided into several equal parts, and KMnO with the same concentration is added into each part4Incubating to obtain an empty sample; adding vitamin C standard solutions with different gradient volumes into each empty sample, reacting at room temperature, and measuring the fluorescence intensity of the mixed reaction system to obtain a standard curve; and taking an empty sample, adding the empty sample into the sample to be detected, reacting at room temperature, measuring the fluorescence intensity of the mixed reaction system, and contrasting with the standard curve to obtain the concentration of the vitamin C in the sample to be detected.
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| CN110628042B (en) * | 2019-10-29 | 2022-03-22 | 西北工业大学 | Preparation method and application of fluorescence enhanced metal nanocluster/zeolite imidazolate framework composite nanomaterial |
| CN111118111A (en) * | 2019-12-11 | 2020-05-08 | 山东农业大学 | Rapid detection method of glucose |
| CN110981896B (en) * | 2019-12-17 | 2022-07-01 | 南宁师范大学 | Preparation method and application of 11-mercaptoundecanoic acid modified gold nanocluster |
| CN111390161B (en) * | 2020-04-14 | 2021-08-03 | 中国科学院生态环境研究中心 | Core-shell type nano gold rod-metal organic framework nano material and preparation method thereof |
| CN111921543B (en) * | 2020-07-23 | 2023-05-09 | 天津大沽化工股份有限公司 | Preparation method and application of efficient acetylene hydrochlorination catalyst |
| CN112133929B (en) * | 2020-09-18 | 2021-08-10 | 济南大学 | Preparation method of ZIF-8-derived Au-N-C oxygen reduction electrocatalyst |
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