CN114752378B - Preparation method and application of carbon quantum dot for detecting content of cefotaxime sodium in medicine - Google Patents
Preparation method and application of carbon quantum dot for detecting content of cefotaxime sodium in medicine Download PDFInfo
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 229960002727 cefotaxime sodium Drugs 0.000 title claims abstract description 42
- AZZMGZXNTDTSME-JUZDKLSSSA-M cefotaxime sodium Chemical compound [Na+].N([C@@H]1C(N2C(=C(COC(C)=O)CS[C@@H]21)C([O-])=O)=O)C(=O)\C(=N/OC)C1=CSC(N)=N1 AZZMGZXNTDTSME-JUZDKLSSSA-M 0.000 title claims abstract description 42
- 239000003814 drug Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000007865 diluting Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 238000007664 blowing Methods 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 230000005284 excitation Effects 0.000 claims description 5
- 239000010413 mother solution Substances 0.000 claims description 5
- 239000007853 buffer solution Substances 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000002390 rotary evaporation Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 8
- 239000002096 quantum dot Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 239000007850 fluorescent dye Substances 0.000 description 5
- 239000012528 membrane Substances 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- OIGNJSKKLXVSLS-VWUMJDOOSA-N prednisolone Chemical compound O=C1C=C[C@]2(C)[C@H]3[C@@H](O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 OIGNJSKKLXVSLS-VWUMJDOOSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011852 carbon nanoparticle Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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Abstract
The invention discloses a preparation method and application of carbon quantum dots for detecting cefotaxime sodium content in a medicine, wherein the preparation method of the carbon quantum dots comprises the steps of hydrothermal reaction of kuh-seng powder, filtering and concentrating. The application of the carbon quantum dot comprises the steps of diluting the carbon quantum dot solution step by step, preparing a liquid to be measured and measuring the fluorescence intensity; the carbon quantum dots prepared from the kuh-seng are used for detecting the content of cefotaxime sodium in the medicine. The preparation method of the carbon quantum dot provided by the invention has the advantages of simple reaction steps and low preparation cost; the method for detecting the content of the cefotaxime sodium in the medicine has the advantages of wide detection range, high accuracy and easiness in operation.
Description
Technical Field
The invention relates to the technical field of medicine analysis, in particular to a preparation method and application of carbon quantum dots.
Background
Carbon quantum dots (Carbon Quantum Dots, CQDs), also known as carbon dots or carbon nanodots, are a class of zero-dimensional carbon nanomaterials with remarkable fluorescent properties consisting of ultrafine, dispersed, quasi-spherical carbon nanoparticles with dimensions below 10 nm. As a novel nanomaterial, carbon quantum dots have excellent properties and great application value, and are being paid attention to by more and more researchers. Compared with the traditional quantum dots (semiconductor and organic dye quantum dots), the fluorescent dye has a plurality of outstanding advantages, such as small size, good light resistance, simple preparation process, biocompatibility, environmental friendliness, good luminous performance, low biotoxicity and the like. Therefore, the quantum dot can replace the traditional quantum dot to play a better role in more fields.
The traditional Chinese medicine is used as a carbon source to prepare the carbon quantum dots, and has the characteristics of wide raw materials, low price and the like. Meanwhile, the quantum dots have blue-green fluorescence, and when combined with certain substances, the quantum dots can increase or decrease the fluorescence. By utilizing the characteristic, the quantum dot can be used as a fluorescent probe to detect the content of a substance. However, the existing detection method has the defects of complex operation and high cost.
Disclosure of Invention
The invention aims to provide a preparation method and application of carbon quantum dots for detecting the content of cefotaxime sodium in a medicine, so as to solve the problems of complex operation and high cost of the existing detection method and simplify the operation steps.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows.
A preparation method of carbon quantum dots for detecting content of cefotaxime sodium in a medicine comprises the following steps:
a1: accurately weighing a certain amount of radix Sophorae Flavescentis powder, adding into polytetrafluoroethylene reaction kettle, adding a certain amount of solvent, performing ultrasonic treatment for 15min, placing into electrothermal blowing drying oven, reacting for 4-12 hr, and cooling to room temperature;
a2: and c, putting the solution obtained in the step a1 into a high-speed centrifugal machine for centrifugation, and enabling the collected supernatant to pass through a microfilm and obtaining the carbon quantum dots after rotary evaporation of the filtrate.
Further optimizing the technical scheme, wherein the quality of the kuh-seng powder in the step a1 is 1.000g-3.000g; the solvent is any one of hydrochloric acid solution, sulfuric acid solution, phosphoric acid solution and water, and the volume of the solvent is any one of 10mL, 15mL, 20mL and 25 mL.
Further optimizing the technical scheme, wherein the temperature in the electrothermal blowing drying oven in the step a1 is set to be 100-180 ℃.
Further optimizing the technical scheme, wherein the centrifugal speed of the centrifugal machine in the step a2 is 10000-18000r/min, and the centrifugal time is 10-15min.
Further optimizing the technical scheme, wherein the aperture of the micro-membrane in the step a2 is 0.45 mu m.
The invention also provides an application of the preparation method of the carbon quantum dot for detecting the content of the cefotaxime sodium in the medicine, which adopts the carbon quantum dot prepared from the kuh-seng powder to detect the content of the cefotaxime sodium in the medicine, and specifically comprises the following steps:
b1, preparing a carbon quantum dot solution of 0.5mg/mL or 1.0mg/mL or 5.0mg/mL or 10.0mg/mL in a volumetric flask as a mother solution, and then gradually diluting;
b2, accurately transferring the carbon quantum dot solution and the BR buffer solution with the volume ratio of 1:2, transferring 10mL of cefotaxime sodium to be tested, placing all the materials into a volumetric flask, and adding water to dilute to a scale;
b3, measuring the fluorescence intensity of the carbon quantum dot containing the cefotaxime sodium prepared in the step b2 and the fluorescence intensity of the reagent blank on a fluorescence spectrophotometer.
Further optimizing the technical scheme, the concentration of the mother solution is one of 0.5mg/mL, 1.0mg/mL, 5.0mg/mL and 10.0 mg/mL.
Further optimizing the technical scheme, the excitation wavelength of the fluorescence spectrophotometer is 340nm, the emission wavelength is 450nm, and the slit width is 5nm.
By adopting the technical scheme, the invention has the following technical progress.
The invention provides a preparation method of carbon quantum dots for detecting cefotaxime sodium content in a medicine, which is characterized in that kuh-seng powder is used as a starting material, and the carbon quantum dots are obtained after hydrothermal reaction, high-speed centrifugation, micro-membrane filtration, concentration and drying; has the advantages of simple reaction steps and low preparation cost. The application of the carbon quantum dot for detecting the content of the cefotaxime sodium in the medicine provided by the invention is that the carbon quantum dot is used for detecting the cefotaxime sodium, and has the advantages of wide detection range, high accuracy and easiness in operation.
Drawings
FIG. 1 is a graph showing the effect of time on fluorescence of generated carbon quantum dots in the preparation of carbon quantum dots in example 1 of the present invention;
FIG. 2 is a graph showing the effect of temperature on fluorescence of generated carbon quantum dots in the preparation of carbon quantum dots in example 1 of the present invention;
FIG. 3 is an infrared spectrum of the carbon quantum dots prepared in example 1 of the present invention;
FIG. 4 is an X-ray diffraction pattern of the carbon quantum dots prepared in example 1 of the present invention;
FIG. 5 is a fluorescence spectrum of the carbon quantum dots prepared in example 1 of the present invention at different excitation wavelengths;
FIG. 6 shows fluorescence intensities at different pH values for the carbon quantum dots prepared in example 1 of the present invention;
FIG. 7 is the effect of different ionic strength on carbon quantum dots during preparation in example 1 of the present invention;
FIG. 8 is a graph showing the effect of time on CQDs-CFTM system in the case of cefotaxime sodium in example 1 of the present invention;
FIG. 9 is a graph showing the effect of the concentration of cefotaxime sodium in cefotaxime sodium on the fluorescence spectrum of carbon quantum dots in example 1;
FIG. 10 is a linear relationship between the concentration of cefotaxime sodium and fluorescence quenching value in the case of detecting cefotaxime sodium in example 1 according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments.
A preparation method of carbon quantum dots for detecting content of cefotaxime sodium in a medicine comprises the following steps:
a1: accurately weighing 1.000g-3.000g of radix sophorae flavescentis powder, adding the powder into a polytetrafluoroethylene reaction kettle, and then adding 10mL or 15mL or 20mL or 25mL of solvent, wherein the solvent is selected from any one of hydrochloric acid solution, sulfuric acid solution, phosphoric acid solution and water. After ultrasonic treatment for 15min, the mixture is placed in an electrothermal blowing drying oven, the temperature is set to be 100-180 ℃, and after 4-12 h of reaction, the mixture is cooled to room temperature. In practical experiments, the temperature is set to be one of 100 ℃, 120 ℃, 140 ℃, 160 ℃ and 180 ℃ and the reaction time is one of 4 hours, 6 hours, 8 hours, 10 hours and 12 hours, so that trend can be observed conveniently and charts can be prepared.
a2: and c, putting the solution obtained in the step a1 into a high-speed centrifugal machine to be centrifuged for 10-15min, setting the centrifugal speed of the centrifugal machine to 10000-18000r/min, collecting supernatant and passing through a micro-membrane with the aperture of 0.45 mu m to remove unreacted organic parts and large particles, and performing spin evaporation on the filtrate to obtain the carbon quantum dots.
The application of the preparation method of the carbon quantum dot for detecting the content of cefotaxime sodium in the medicine takes the carbon quantum dot of kuh-seng powder as a fluorescent probe, and the method for detecting the cefotaxime sodium is established and concretely comprises the following steps:
b1, preparing a carbon quantum dot solution with the concentration of 0.5mg/mL or 1.0mg/mL or 5.0mg/mL or 10.0mg/mL in a volumetric flask as a mother solution, and then gradually diluting. The volumetric flask is one of 25mL, 50mL, 100mL, and 250 mL.
b2, accurately transferring the carbon quantum dot solution and the BR buffer solution with the volume ratio of 1:2, transferring 10mL of cefotaxime sodium to be tested, placing the cefotaxime sodium to be tested into a volumetric flask, adding water to dilute to a scale, and shaking uniformly.
b3, setting the excitation wavelength of the fluorescence spectrophotometer to 340nm, the emission wavelength to 450nm and the slit width to 5nm. The fluorescence intensity of the carbon quantum dots containing cefotaxime sodium prepared in step b2 and the fluorescence intensity of the reagent blank were measured on a fluorescence spectrophotometer.
Example 1:
the invention provides a preparation method of carbon quantum dots for detecting the content of cefotaxime sodium in a drug, which comprises the following steps of:
a1: accurately weighing 2.000g of radix sophorae flavescentis powder, adding the powder into a polytetrafluoroethylene reaction kettle, and then adding 20mL of water. After 15min of ultrasonic treatment, the mixture is placed in an electrothermal blowing drying oven, the temperature is set at 180 ℃, and after 10h of reaction, the mixture is cooled to room temperature.
a2: and c, putting the dark brown solution obtained in the step a1 into a high-speed centrifugal machine for centrifugation for 15min, setting the centrifugation speed of the centrifugal machine to 10000r/min, collecting supernatant and passing through a micro-membrane with the pore diameter of 0.45 mu m to remove unreacted organic parts and large particles, and performing rotary evaporation on the filtrate to obtain the carbon quantum dots.
Example 2:
the invention provides a preparation method of carbon quantum dots for detecting the content of cefotaxime sodium in a drug, which comprises the following steps of:
a1: 1.000g of kuh-seng powder is accurately weighed, added into a polytetrafluoroethylene reaction kettle, and then 10mL of sulfuric acid solution is added. After 15min of ultrasonic treatment, the mixture is placed in an electrothermal blowing drying oven, the temperature is set to 140 ℃, and after 4h of reaction, the mixture is cooled to room temperature.
a2: and c, putting the dark brown solution obtained in the step a1 into a high-speed centrifugal machine for centrifugation for 12min, setting the centrifugation speed of the centrifugal machine to be 18000r/min, collecting supernatant and passing through a micro-membrane with the pore diameter of 0.45 mu m to remove unreacted organic parts and large particles, and performing spin evaporation on the filtrate to obtain the carbon quantum dots.
Example 3:
the invention provides a preparation method of carbon quantum dots for detecting the content of cefotaxime sodium in a drug, which comprises the following steps of:
a1: 3.000g of kuh-seng powder is accurately weighed, added into a polytetrafluoroethylene reaction kettle, and then 25mL of hydrochloric acid solution is added. After 15min of ultrasonic treatment, the mixture is placed in an electrothermal blowing drying oven, the temperature is set to be 100 ℃, and after 12h of reaction, the mixture is cooled to room temperature.
a2: and c, putting the dark brown solution obtained in the step a1 into a high-speed centrifugal machine for centrifugation for 10min, setting the centrifugation speed of the centrifugal machine to be 14000r/min, collecting supernatant and passing through a micro-membrane with the pore diameter of 0.45 mu m to remove unreacted organic parts and large particles, and performing spin evaporation on the filtrate to obtain the carbon quantum dots.
The method for establishing the detection of the cefotaxime sodium by using the carbon quantum dots prepared in the embodiment 1 as fluorescent probes specifically comprises the following steps:
b1, preparing a carbon quantum dot solution with the concentration of 1.0mg/mL in a volumetric flask with the concentration of 100mL as a mother solution, and then gradually diluting.
b2, accurately transferring 1mL of the carbon quantum dot solution and 2mL of the BR buffer solution, transferring 10mL of cefotaxime sodium to be detected, placing all the materials into a volumetric flask, adding water to dilute to a scale, and shaking uniformly.
b3, setting the excitation wavelength of the fluorescence spectrophotometer to 340nm, the emission wavelength to 450nm and the slit width to 5nm. The fluorescence intensity of the carbon quantum dots containing cefotaxime sodium prepared in step b2 and the fluorescence intensity of the reagent blank were measured on a fluorescence spectrophotometer.
According to the experimental optimization condition, the fluorescence quenching intensity delta F of the carbon quantum dots and the concentration c of the corresponding cefotaxime sodium are in a linear relation, and the linear equation is delta F=1.374c+41.617; the fluorescence quenching strength of the carbon quantum dots and the concentration of cefotaxime sodium show a good linear relation between 20 and 400 mug/mL, and the correlation coefficient R=0.993. Therefore, the detection of the cefotaxime sodium based on the carbon quantum dot fluorescent probe is realized.
Claims (7)
1. The preparation method of the carbon quantum dot for detecting the content of cefotaxime sodium in the medicine is characterized by comprising the following steps of:
a1: accurately weighing radix Sophorae Flavescentis powder, adding into polytetrafluoroethylene reaction kettle, adding solvent, ultrasonic treating for 15min, placing into electrothermal blowing drying oven, reacting for 4-12 hr, and cooling to room temperature;
a2: and c, putting the solution obtained in the step a1 into a high-speed centrifugal machine for centrifugation, and enabling the collected supernatant to pass through a microfilm and obtaining the carbon quantum dots after rotary evaporation of the filtrate.
2. The method for preparing the carbon quantum dot for detecting the content of cefotaxime sodium in a medicine according to claim 1, which is characterized in that: the quality of the kuh-seng powder in the step a1 is 1.000g-3.000g; the solvent is any one of hydrochloric acid solution, sulfuric acid solution, phosphoric acid solution and water, and the volume of the solvent is any one of 10mL, 15mL, 20mL and 25 mL.
3. The method for preparing the carbon quantum dot for detecting the content of cefotaxime sodium in a medicine according to claim 1, which is characterized in that: the temperature in the electrothermal blowing drying oven in the step a1 is set to be 100-180 ℃.
4. The method for preparing the carbon quantum dot for detecting the content of cefotaxime sodium in a medicine according to claim 1, which is characterized in that: and c, the centrifugal speed of the centrifugal machine in the step a2 is 10000-18000r/min, and the centrifugal time is 10-15min.
5. The method for preparing the carbon quantum dot for detecting the content of cefotaxime sodium in a medicine according to claim 1, which is characterized in that: the pore size of the microfilm in step a2 is 0.45 μm.
6. The application of the carbon quantum dot prepared by the preparation method according to any one of claims 1 to 5, wherein the carbon quantum dot prepared by the kuh-seng powder is used for detecting the content of cefotaxime sodium in the medicine, and the application specifically comprises the following steps:
b1, preparing a carbon quantum dot solution of 0.5mg/mL or 1.0mg/mL or 5.0mg/mL or 10.0mg/mL in a volumetric flask as a mother solution, and then gradually diluting;
b2, accurately transferring the carbon quantum dot solution and the BR buffer solution with the volume ratio of 1:2, transferring 10mL of cefotaxime sodium to be tested, placing all the materials into a volumetric flask, and adding water to dilute to a scale;
b3, measuring the fluorescence intensity of the carbon quantum dot containing the cefotaxime sodium prepared in the step b2 and the fluorescence intensity of the reagent blank on a fluorescence spectrophotometer.
7. The use according to claim 6, characterized in that: the fluorescence spectrophotometer had an excitation wavelength of 340nm, an emission wavelength of 450nm, and a slit width of 5nm.
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| CN112920797A (en) * | 2021-03-25 | 2021-06-08 | 广东工业大学 | N, S-doped water-soluble carbon quantum dot and application thereof |
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| CN110155984B (en) * | 2019-06-12 | 2021-02-02 | 浙江科技学院 | Method for synthesizing biomass fluorescent carbon dots by hydrothermal method with soybean dregs as raw material and application |
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| CN111573652A (en) * | 2020-05-19 | 2020-08-25 | 四川农业大学 | Preparation of chicken feather nitrogen-doped carbon quantum dot and fluorescent probe and paraquat detection method |
| CN112174111A (en) * | 2020-09-30 | 2021-01-05 | 湖南科技大学 | Preparation method and application of near-infrared light-emitting carbon dots with p-phenylenediamine as carbon source |
| CN112375565A (en) * | 2020-10-13 | 2021-02-19 | 山西大学 | Carbon quantum dot for rapidly and sensitively detecting azithromycin, and preparation method and application thereof |
| CN112920797A (en) * | 2021-03-25 | 2021-06-08 | 广东工业大学 | N, S-doped water-soluble carbon quantum dot and application thereof |
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| CN114752378A (en) | 2022-07-15 |
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