CN114752378A - Preparation method and application of carbon quantum dots for detecting cephalosporin content in medicine - Google Patents
Preparation method and application of carbon quantum dots for detecting cephalosporin content 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
- 239000003814 drug Substances 0.000 title claims abstract description 24
- 229930186147 Cephalosporin Natural products 0.000 title claims abstract description 23
- 229940124587 cephalosporin Drugs 0.000 title claims abstract description 23
- 150000001780 cephalosporins Chemical class 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000007865 diluting Methods 0.000 claims abstract description 5
- 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 claims description 28
- 229960002727 cefotaxime sodium Drugs 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 25
- 238000005119 centrifugation Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 6
- 229940079593 drug Drugs 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- 239000010413 mother solution 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
- 238000002390 rotary evaporation Methods 0.000 claims description 6
- 230000005284 excitation Effects 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 239000007853 buffer solution Substances 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000007605 air drying Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000005485 electric heating Methods 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 239000012452 mother liquor Substances 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 claims 1
- 241000246044 Sophora flavescens Species 0.000 abstract description 6
- 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
- 239000002096 quantum dot Substances 0.000 description 8
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- 239000007850 fluorescent dye Substances 0.000 description 4
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- MFYSUUPKMDJYPF-UHFFFAOYSA-N 2-[(4-methyl-2-nitrophenyl)diazenyl]-3-oxo-n-phenylbutanamide Chemical compound C=1C=CC=CC=1NC(=O)C(C(=O)C)N=NC1=CC=C(C)C=C1[N+]([O-])=O MFYSUUPKMDJYPF-UHFFFAOYSA-N 0.000 description 2
- 241000219784 Sophora Species 0.000 description 2
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- 238000002474 experimental method Methods 0.000 description 2
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- 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
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B82Y40/00—Manufacture or treatment of nanostructures
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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- 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 a carbon quantum dot for detecting cephalosporin content in a medicament, wherein the preparation method of the carbon quantum dot comprises the steps of hydrothermal reaction, filtration and concentration of sophora flavescens powder. The application of the carbon quantum dots comprises the steps of diluting a carbon quantum dot solution step by step, preparing a solution to be detected and measuring the fluorescence intensity; the carbon quantum dot prepared from the sophora flavescens is used for detecting the content of cephalosporin in the medicine. The preparation method of the carbon quantum dots provided by the invention has the advantages of simple reaction steps and low preparation cost; the method for detecting the content of the cephalosporin in the medicament has the advantages of wide detection range, high accuracy and easiness in operation.
Description
Technical Field
The invention relates to the technical field of pharmaceutical analysis, and particularly relates to a preparation method and application of a carbon quantum dot.
Background
Carbon Quantum Dots (CQDs), also called Carbon Dots or Carbon nanodots, are zero-dimensional Carbon nanomaterials with significant fluorescent properties, and consist of ultrafine, dispersed, quasi-spherical Carbon nanoparticles with a size below 10 nm. As a new nano material, carbon quantum dots have excellent properties and great application value, and are being valued by more and more researchers. Compared with the traditional quantum dots (semiconductor and organic dye quantum dots), the quantum dots have the advantages of small size, good light resistance, simple preparation process, biocompatibility, environmental friendliness, good luminous performance, low biotoxicity and the like. Therefore, the quantum dots can replace the traditional quantum dots to play a better role in more fields.
The carbon quantum dots prepared by using the traditional Chinese medicine as a carbon source have the characteristics of wide raw materials, low price and the like. Meanwhile, the quantum dots have blue-green fluorescence, and when the quantum dots are combined with certain substances, the fluorescence can be enhanced or weakened. 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 solve the technical problem of providing a preparation method and application of a carbon quantum dot for detecting the content of cephalosporin in a medicament, 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 a carbon quantum dot for detecting the content of cephalosporin in a medicament comprises the following steps:
a 1: accurately weighing a certain amount of radix sophorae flavescentis powder, adding the radix sophorae flavescentis powder into a polytetrafluoroethylene reaction kettle, adding a certain amount of solvent, carrying out ultrasonic treatment for 15min, placing the mixture into an electric heating forced air drying oven, reacting for 4-12 h, and cooling to room temperature;
a 2: and c, placing the solution obtained in the step a1 into a high-speed centrifuge for centrifugation, passing the collected supernatant through a microfilm, and performing rotary evaporation on the filtrate to obtain the carbon quantum dots.
Further optimizing the technical scheme, wherein the mass of the radix sophorae flavescentis in the step a1 is 1.000g-3.000 g; 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.
The technical scheme is further optimized, and the temperature in the electrothermal blowing drying oven in the step a1 is set to be 100-180 ℃.
Further optimizing the technical scheme, the centrifugation speed of the centrifuge in the step a2 is 10000-.
In the technical scheme, the pore diameter of the micro-membrane in the step a2 is 0.45 μm.
The invention also provides application of the carbon quantum dot for detecting the cephalosporin content in the medicament, the carbon quantum dot prepared from the sophora flavescens is adopted to detect the cephalosporin content in the medicament, and the method specifically comprises the following steps:
b1, preparing a carbon quantum dot solution with a certain concentration in a volumetric flask as a mother solution, and diluting step by step;
b2, accurately transferring a carbon quantum dot solution and a BR buffer solution in a volume ratio of 1:2, transferring a proper amount of cefotaxime sodium to be detected, placing the cefotaxime sodium in a volumetric flask, and adding water to dilute the cefotaxime sodium to a scale;
b3, measuring the fluorescence intensity of the carbon quantum dots containing cefotaxime sodium prepared in the step b2 and the fluorescence intensity of the reagent blank on a fluorescence spectrophotometer.
The technical scheme is further optimized, and the concentration of the mother solution is one of 0.5mg/mL, 1.0mg/mL, 5.0mg/mL and 10.0 mg/mL.
The technical scheme is further optimized, wherein the excitation wavelength of the fluorescence spectrophotometer is 340nm, the emission wavelength is 450nm, and the slit width is 5 nm.
Due to the adoption of the technical scheme, the technical progress of the invention is as follows.
The invention provides a preparation method of carbon quantum dots for detecting cephalosporin content in a drug, which takes lightyellow sophora root as a starting raw material and obtains the carbon quantum dots after hydrothermal reaction, high-speed centrifugation, micro-membrane filtration, concentration and drying; has the advantages of simple reaction steps and low preparation cost. The carbon quantum dot for detecting the content of the cephalosporin in the medicament is applied to the detection of 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 the fluorescence of the 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 the fluorescence of the resulting carbon quantum dots in the preparation of carbon quantum dots in example 1 according to the present invention;
FIG. 3 is an IR spectrum of carbon quantum dots prepared in example 1 of the present invention;
FIG. 4 is an X-ray diffraction pattern of carbon quantum dots prepared in example 1 of the present invention;
FIG. 5 shows fluorescence spectra of carbon quantum dots prepared in example 1 of the present invention at different excitation wavelengths;
FIG. 6 shows fluorescence intensities of carbon quantum dots prepared in example 1 of the present invention at different pH values;
FIG. 7 is a graph showing the effect of different ionic strengths on carbon quantum dots in the preparation process in example 1 of the present invention;
FIG. 8 is a graph showing the effect of time in cefotaxime sodium on CQDs-CFTM system in example 1 of the present invention;
FIG. 9 shows the effect of detecting cefotaxime sodium concentration in cefotaxime sodium on the fluorescence spectrum of carbon quantum dots in example 1 of the present invention;
FIG. 10 is a linear relationship between the concentration of cefotaxime sodium in cefotaxime sodium and the fluorescence quenching value in the example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments.
A preparation method of a carbon quantum dot for detecting the content of cephalosporin in a medicament comprises the following steps:
a 1: accurately weighing 1.000-3.000 g of radix Sophorae Flavescentis powder, adding into a polytetrafluoroethylene reaction kettle, and adding 10mL or 15mL or 20mL or 25mL of solvent selected from hydrochloric acid solution, sulfuric acid solution, phosphoric acid solution, and water. After the ultrasonic treatment is carried out for 15min, the mixture is placed in an electrothermal blowing dry box, the temperature is set to be 100-180 ℃, and after the reaction is carried out for 4-12 h, the mixture is cooled to the room temperature. In practical experiments, the temperature is set to be one of 100 ℃, 120 ℃, 140 ℃, 160 ℃ and 180 ℃, and the reaction time is set to be one of 4h, 6h, 8h, 10h and 12h, so that the trend can be observed and a chart can be prepared conveniently.
a 2: and c, placing the solution obtained in the step a1 into a high-speed centrifuge for centrifugation for 10-15min, setting the centrifugation speed of the centrifuge to 10000-18000r/min, collecting supernatant, 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 filtrate to obtain the carbon quantum dots.
The application of carbon quantum dots for detecting the content of cephalosporin in a medicament, which takes lightyellow sophora root carbon quantum dots as a fluorescent probe to establish a method for detecting cefotaxime sodium, specifically comprises the following steps:
b1, preparing a carbon quantum dot solution with the concentration of 0.5mg/mL, 1.0mg/mL, 5.0mg/mL or 10.0 mg/mL in a volumetric flask as a mother solution, and then diluting step by step. The volumetric flask is 25mL, 50mL, 100mL or 250 mL.
b2, accurately transferring a carbon quantum dot solution and a BR buffer solution in a volume ratio of 1:2, transferring a proper amount of cefotaxime sodium to be detected, placing the cefotaxime sodium in a volumetric flask, adding water to dilute the cefotaxime sodium to a scale, and shaking up the cefotaxime sodium.
b3, setting the excitation wavelength of the fluorescence spectrophotometer to be 340nm, the emission wavelength to be 450nm and the slit width to be 5 nm. And (c) measuring the fluorescence intensity of the carbon quantum dots containing the cefotaxime sodium prepared in the step b2 and the fluorescence intensity of the reagent blank on a fluorescence spectrophotometer.
Example 1:
the invention provides a preparation method of a carbon quantum dot for detecting the content of cephalosporin in a medicament, which comprises the following steps during actual preparation:
a 1: 2.000g of sophora flavescens powder is accurately weighed, added into a polytetrafluoroethylene reaction kettle, and then added with 20mL of water. After 15min of ultrasonic treatment, the mixture is placed in an electrothermal blowing dry box, the temperature is set to be 180 ℃, and after 10h of reaction, the mixture is cooled to the room temperature.
a 2: and c, placing the dark brown solution obtained in the step a1 into a high-speed centrifuge for centrifugation for 15min, setting the centrifugation speed of the centrifuge to 10000r/min, collecting supernatant, passing through a micro-membrane with the pore diameter of 0.45 mu m to remove unreacted organic parts and large particles, and carrying out rotary evaporation on filtrate to obtain the carbon quantum dots.
Example 2:
the invention provides a preparation method of a carbon quantum dot for detecting the content of cephalosporin in a medicament, which comprises the following steps during actual preparation:
a 1: 1.000g of sophora flavescens powder is accurately weighed, added into a polytetrafluoroethylene reaction kettle, and then 10mL of sulfuric acid solution is added. After 15min of ultrasound, the mixture is placed in an electrothermal blowing dry box, the temperature is set to be 140 ℃, and after 4h of reaction, the mixture is cooled to the room temperature.
a 2: and c, placing the dark brown solution obtained in the step a1 into a high-speed centrifuge for centrifugation for 12min, setting the centrifugation speed of the centrifuge to be 18000r/min, collecting supernate, passing the supernate through a micro-membrane with the pore diameter of 0.45 mu m to remove unreacted organic parts and large particles, and carrying out rotary evaporation on filtrate to obtain the carbon quantum dots.
Example 3:
the invention provides a preparation method of a carbon quantum dot for detecting the content of cephalosporin in a medicament, which comprises the following steps during actual preparation:
a 1: 3.000g of sophora flavescens powder is accurately weighed, added into a polytetrafluoroethylene reaction kettle, and then added with 25mL of hydrochloric acid solution. After 15min of ultrasonic treatment, the mixture is placed in an electrothermal blowing dry box, the temperature is set to be 100 ℃, and after 12h of reaction, the mixture is cooled to the room temperature.
a 2: and c, placing the dark brown solution obtained in the step a1 into a high-speed centrifuge for centrifugation for 10min, setting the centrifugation speed of the centrifuge to 14000r/min, collecting supernatant, passing through a microfilm with the aperture of 0.45 mu m to remove unreacted organic parts and large particles, and performing rotary evaporation on filtrate to obtain the carbon quantum dots.
The method for detecting cefotaxime sodium by applying the carbon quantum dots prepared in the embodiment 1 as the fluorescent probe specifically comprises the following steps:
b1, preparing a carbon quantum dot solution with the concentration of 1.0mg/mL in a 100mL volumetric flask as a mother solution, and then diluting the mother solution step by step.
b2, accurately transferring 1mL of carbon quantum dot solution and 2mL of BR buffer solution, transferring 10mL of cefotaxime sodium to be detected, placing the cefotaxime sodium in a volumetric flask, adding water to dilute the cefotaxime sodium to a scale, and shaking up.
b3, setting the excitation wavelength of the fluorescence spectrophotometer to be 340nm, the emission wavelength to be 450nm and the slit width to be 5 nm. And (c) measuring the fluorescence intensity of the carbon quantum dot containing cefotaxime sodium prepared in the step b2 and the fluorescence intensity of the reagent blank on a fluorescence spectrophotometer.
According to the conditions optimized by experiments, the fluorescence quenching intensity delta F of the carbon quantum dots and the concentration c of corresponding cefotaxime sodium are in a linear relation, and the linear equation is that delta F is 1.374c + 41.617; the carbon quantum dot fluorescence quenching intensity and the concentration of cefotaxime sodium in the range of 20-400 mu g/mL show a good linear relation, and the correlation coefficient R is 0.993. Therefore, the detection of cefotaxime sodium based on the carbon quantum dot fluorescent probe is realized.
Claims (8)
1. A preparation method of a carbon quantum dot for detecting the content of cephalosporin in a medicament is characterized by comprising the following steps:
a 1: accurately weighing a certain amount of radix sophorae flavescentis powder, adding the radix sophorae flavescentis powder into a polytetrafluoroethylene reaction kettle, adding a certain amount of solvent, carrying out ultrasonic treatment for 15min, placing the mixture into an electric heating forced air drying oven, reacting for 4-12 h, and cooling to room temperature;
a 2: and c, placing the solution obtained in the step a1 into a high-speed centrifuge for centrifugation, passing the collected supernatant through a microfilm, and performing rotary evaporation on the filtrate to obtain the carbon quantum dots.
2. The method for preparing the carbon quantum dot for detecting the cephalosporin content in the drug according to claim 1, characterized in that: the mass of the radix sophorae flavescentis in the step a1 is 1.000g-3.000 g; 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 cephalosporin content in the drug according to claim 1, characterized in that: the temperature in the electrothermal blowing dry box in the step a1 is set to be 100-180 ℃.
4. The method for preparing the carbon quantum dot for detecting the cephalosporin content in the drug according to claim 1, characterized in that: the centrifugal speed of the centrifugal machine in the step a2 is 10000-.
5. The method for preparing the carbon quantum dot for detecting the cephalosporin content in the drug according to claim 1, characterized in that: the pore diameter of the micro-membrane in the step a2 is 0.45 μm.
6. The application of the carbon quantum dot as claimed in any one of claims 1 to 5, wherein the carbon quantum dot prepared from radix sophorae flavescentis is used for detecting the content of cephalosporin in a medicament, and the method specifically comprises the following steps:
b1, preparing a carbon quantum dot solution with a certain concentration in a volumetric flask as a mother solution, and diluting step by step;
b2, accurately transferring a carbon quantum dot solution and a BR buffer solution in a volume ratio of 1:2, transferring a proper amount of cefotaxime sodium to be detected, placing the cefotaxime sodium in a volumetric flask, and adding water to dilute the cefotaxime sodium to a scale;
b3, measuring the fluorescence intensity of the carbon quantum dots containing cefotaxime sodium prepared in the step b2 and the fluorescence intensity of the reagent blank on a fluorescence spectrophotometer.
7. The use of the carbon quantum dot for detecting the cephalosporin content in the drug according to claim 6, wherein: the concentration of the mother liquor is one of 0.5mg/mL, 1.0mg/mL, 5.0mg/mL and 10.0 mg/mL.
8. The method of synthesis according to claim 7, characterized in that: the excitation wavelength of the fluorescence spectrophotometer is 340nm, the emission wavelength is 450nm, and the slit width is 5 nm.
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| 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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| US20200392404A1 (en) * | 2019-06-12 | 2020-12-17 | Zhejiang University Of Science & Technology | Method of making biomass fluorescent carbon quantum dots from soybean dregs by hydrothermal synthesis and uses thereof |
| 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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