CN108426863B - Method for determining content of cannabidiol based on silver nano resonance Rayleigh scattering spectrometry - Google Patents
Method for determining content of cannabidiol based on silver nano resonance Rayleigh scattering spectrometry Download PDFInfo
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Abstract
The invention discloses a method for determining content of industrially extracted cannabidiol based on silver nano resonance Rayleigh scattering spectrometry, which comprises the following steps: adding polyethylene glycol solution, silver nitrate solution, sodium hydroxide solution and ammonia water solution into a colorimetric tube in sequence, mixing uniformly, and adding sodium hydroxide solutionCarrying out constant volume mixing on the cannabidiol solution, and then reacting in a water bath; on a fluorescence spectrophotometer, the scattering peak intensity difference at 450nm is measured and calculatedΔI(ii) a Drawing a standard curve; and (4) after the scattering peak value of the sample is measured, calculating the content of the cannabidiol in the extract according to a standard curve and a sample solution preparation method.
Description
Technical Field
The invention belongs to the field of analytical chemistry, and particularly relates to a method for determining content of industrially extracted cannabidiol based on silver nano resonance Rayleigh scattering spectrometry.
Background
Cannabidiol is a non-addictive biological component extracted, separated and identified from industrial cannabis sativa, and modern biomedical research shows that the cannabidiol can prevent the addictive component tetrahydrocannabinol in the cannabis sativa from influencing the human nervous system, and has pharmacological activities of resisting spasm, rheumatic arthritis, anxiety, depression and insomnia.
The existing methods for measuring the content of cannabidiol include gas chromatography-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (L C-MS), gas chromatography (GC-FID), high performance liquid chromatography (HP L C) and the like.
The determination of the content of cannabidiol in the industrial high-purity extract needs a rapid, simple and prepared detection method, so that a method which is simple to operate, accurate, rapid and feasible must be found.
Disclosure of Invention
The invention aims to provide a method for determining the content of cannabidiol based on resonance Rayleigh scattering spectrometry, which is simple, high in accuracy and easy to operate, aiming at the defects of the prior art. The method has the advantages of high sensitivity, good selectivity, simplicity, convenience, rapidness, low cost and the like, and has good application prospect in determination of cannabidiol content in industrial high-purity extract.
The technical scheme for realizing the purpose of the invention is as follows:
the method for determining the content of industrially extracted cannabidiol based on the silver nano resonance Rayleigh scattering spectrometry comprises the following steps:
(1) a standard solution system for preparing the cannabidiol is prepared by sequentially adding a polyethylene glycol solution with the mass percentage of 1.0m L of 0.1-1.0%, a silver nitrate solution with the mass percentage of 1.0m L0.1.1-1.0 g/L, a sodium hydroxide solution with the mass percentage of 0.5m L0.1-1.0 g/L and an ammonia water solution with the mass percentage of 0.1-1.0% of 0.5m L into a colorimetric tube with the mass percentage of 10m L, uniformly mixing, adding a cannabidiol standard solution with the mass percentage of 1.0m L0.001.001-0.020 mg/m L, fixing the volume by using distilled water, uniformly mixing, and reacting in a water bath with the temperature of 50-90 ℃ for 40 min;
(2) preparing a blank control system without adding cannabidiol according to the method of the step (1);
(3) respectively placing the solutions of the standard solution system and the blank control system in a quartz cuvette, scanning synchronously on a fluorescence spectrophotometer with excitation light wavelength consistent with emission light wavelength to obtain resonance Rayleigh scattering method spectrum, and measuring the scattering peak intensity of the standard solution at 450nm to obtainISimultaneously measuring the intensity of the scattering peak of the blank control systemI 0CalculatingΔI=I- I 0 ；
(4) To be provided withΔIMaking a standard curve for the concentration relation of the cannabidiol standard solution;
(5) getmDissolving and fixing the cannabidiol sample extracted industrially in mg with analytical pure ethanolVm L volumetric flask, preparing the sample solution to be measured according to the method in the step (1), replacing the added cannabidiol standard solution with the sample solution, and measuring the resonant Rayleigh scattering peak intensity of the sample solution according to the method in the step (3)I Sample (A)；
(6) Calculating the concentration C of cannabidiol in the sample solution according to the working curve of the step (4)Sample (A)By the formula:
calculating the content of cannabis sativa in the extractThe content of diphenol.
The principle is as follows: under the condition of the invention, phenolic hydroxyl in the cannabidiol is converted into quinone under an alkaline condition so as to have reducibility, and the reducibility can reduce silver ions in the silver ammonia solution into silver nanoparticles, so that a characteristic resonance Rayleigh scattering spectrum appears at 310-650 nm, and the scattering peak is linearly increased along with the increase of the concentration of the cannabidiol. And (3) performing absorption scanning on the solution obtained by the reaction by using a fluorescence spectrophotometer to obtain a resonance Rayleigh scattering spectrum, and rapidly determining the content of cannabidiol in the industrial high-purity extract according to the linear relation between the peak value of the resonance Rayleigh scattering spectrum and the concentration of cannabidiol.
The invention has the advantages that: compared with the existing method, the measuring method has the advantages of simple instrument requirement, simple and convenient operation, easy reagent acquisition, good selectivity and low cost.
Drawings
FIG. 1 is a graph of the resonance Rayleigh scattering spectra of the cannabidiol standard solution system of example 1;
FIG. 2 is a standard curve diagram of the cannabidiol standard solution system of example 1;
FIG. 3 is a transmission electron microscope image of silver nanoparticles generated by the reaction of 0.012mg/m L cannabidiol standard solution in example 1.
Detailed Description
The invention is further illustrated by the following examples, which are not to be construed as limiting the invention thereto.
Example 1
The method for measuring the content of cannabidiol in the extract based on the silver nano resonance Rayleigh scattering spectrometry comprises the following steps:
(1) preparing a standard solution system of cannabidiol, namely taking 6 colorimetric tubes of 10m L, sequentially adding a polyethylene glycol solution with the mass percent of 1.0m L of 0.1 percent, a silver nitrate solution with the mass percent of 1.0m L0.1.1 g/L, a sodium hydroxide solution with the mass percent of 0.5m L0.1.1 g/L and an ammonia water solution with the mass percent of 0.5m L into each colorimetric tube, shaking up the colorimetric tubes respectively, adding cannabidiol standard solutions with different concentrations of 1.0m L into the 6 colorimetric tubes respectively, adding the cannabidiol standard solutions with the concentrations of 0.002, 0.004, 0.006, 0.008, 0.010 and 0.012mg/m L into each colorimetric tube, uniformly mixing the solutions with distilled water to fix the volume, and reacting the mixture in a water bath at 50 ℃ for 40min (the transmission image of silver nanoparticles generated by the reaction of the cannabidiol standard solution of 0.012mg/m L is shown in a picture 3);
(2) preparing a blank control system without adding cannabidiol according to the method of the step (1);
(3) respectively placing the solutions of the standard solution system and the blank control system in a quartz cuvette, scanning synchronously on a fluorescence spectrophotometer with excitation light wavelength consistent with emission light wavelength to obtain resonance Rayleigh scattering spectrum (shown in figure 1), and measuring the scattering peak intensity of the standard solution at 450nm to obtainISimultaneously measuring the intensity of the scattering peak of the blank control systemI 0CalculatingΔI=I-I 0 ；
(4) To be provided withΔIA standard curve is made for the cannabidiol standard solution concentration relationship:ΔI=130713C-70.907（R 2= 0.9970), the unit of the cannabidiol concentration C is mg/m L, the linear range is 0.002-0.012 mg/m L, and the standard curve chart is shown in fig. 2;
(5) dissolving 5.0mg of industrially extracted cannabidiol sample in an analytically pure ethanol and dissolving the sample in a 500m L volumetric flask to prepare a cannabidiol sample ethanol solution, taking a 10m L colorimetric tube, sequentially adding a polyethylene glycol solution with the mass percent of 1.0m L of 0.1%, a silver nitrate solution with the mass percent of 1.0m L0.1.1 g/L, a sodium hydroxide solution with the mass percent of 0.5m L0.1.1 g/L, an ammonia water solution with the mass percent of 0.1% of 0.5m L and a cannabidiol sample ethanol solution with the mass percent of 1.0m L, fixing the volume by using distilled water, uniformly mixing, reacting in a water bath at 50 ℃ for 40min to prepare a sample solution to be detected, and determining the Rayleigh resonance scattering peak intensity of the sample solution according to the method in the step (3)I Sample (A)=1122.5；
(6) Calculating the concentration of cannabidiol in the sample solution according to the standard curve of the step (4)C Sample (A)=0.00913mg/m L, by the formula:
the cannabidiol content in the extract can be calculated to be 913%, RSD (n = 6) of 6 replicates was 7.2%.
Example 2
The method for measuring the content of cannabidiol in the extract based on the silver nano resonance Rayleigh scattering spectrometry comprises the following steps:
(1) preparing a standard solution system of cannabidiol, namely taking 8 colorimetric tubes of 10m L, sequentially adding 1.0m L mass percent of 1.0% polyethylene glycol solution, 1.0m L1.0 g/L silver nitrate solution, 0.5m L1.0.0 g/L sodium hydroxide solution and 0.5m L mass percent of 1.0% ammonia water solution into each colorimetric tube, shaking uniformly, respectively adding 1.0m L concentration different cannabidiol standard solutions into the 8 colorimetric tubes, respectively adding 0.002, 0.004, 0.006, 0.008, 0.010, 0.012, 0.014 and 0.016mg/m L cannabidiol standard solutions into each colorimetric tube, uniformly mixing the cannabidiol standard solutions with distilled water, and reacting in a water bath at 90 ℃ for 40 min;
(2) preparing a blank control system without adding cannabidiol according to the method of the step (1);
(3) respectively placing the solutions of the standard solution system and the blank control system in a quartz cuvette, scanning synchronously on a fluorescence spectrophotometer with excitation light wavelength consistent with emission light wavelength to obtain resonance Rayleigh scattering spectrum, and measuring the scattering peak intensity of the standard solution at 450nm to obtainISimultaneously measuring the intensity of the scattering peak of the blank control systemI 0CalculatingΔI=I-I 0 ；
(4) To be provided withΔIA standard curve is made for the cannabidiol standard solution concentration relationship:ΔI=115231C-40.574（R 2= 0.9943), the unit of the cannabidiol concentration C is mg/m L, and the linear range is 0.002-0.016 mg/m L;
(5) dissolving 2.0mg of industrially extracted cannabidiol sample in a 200m L volumetric flask by using analytical ethanol to prepare a cannabidiol sample ethanol solution, taking a 10m L colorimetric tube, sequentially adding a 1.0m L mass percent polyethylene glycol solution, a 1.0m L1.0.0 g/L silver nitrate solution, a 0.5m L1.0.0 g/L sodium hydroxide solution, a 0.5m L mass percent ammonia water solution and a 1.0m L cannabidiol sample ethanol solution, and fixing by using distilled waterAfter being mixed evenly, the mixture reacts in water bath at 90 ℃ for 40min to prepare a sample solution to be measured, and the resonance Rayleigh scattering peak intensity of the sample solution is measured according to the method in the step (3)I Sample (A)=934.3；
(6) Calculating the concentration of cannabidiol in the sample solution according to the standard curve of the step (4)C Sample (A)=0.00846mg/m L, by the formula:
the cannabidiol content of the extract was calculated to be 84.6% and RSD (n = 6) was calculated to be 6.2% for 6 replicates.
(7) Using the sample solution prepared in step (5) as a sample, a recovery rate of 0.0115mg/m L was prepared and the solution was examined to calculate a recovery rate of 89.1% and an RSD (n = 6) of 7.5%.
Example 3
The method for measuring the content of cannabidiol in the extract based on the silver nano resonance Rayleigh scattering spectrometry comprises the following steps:
(1) preparing a cannabidiol analysis system, namely taking 10 colorimetric tubes of 10m L, sequentially adding a polyethylene glycol solution with the mass percent of 1.0m L to be 0.2%, a silver nitrate solution with the mass percent of 1.0m L0.5.5 g/L, a sodium hydroxide solution with the mass percent of 0.5m L0.7 to be 0.7 g/L and an ammonia water solution with the mass percent of 0.5m L to each colorimetric tube, shaking up the colorimetric tubes respectively, adding cannabidiol standard solutions with different concentrations of 1.0m L to each colorimetric tube, wherein the cannabidiol standard solutions added to each colorimetric tube have the concentrations of 0.002, 0.004, 0.006, 0.008, 0.012, 0.014, 0.016, 0.018 and 0.020mg/m L respectively, fixing the volume with distilled water, uniformly mixing, and reacting in a water bath at 70 ℃ for 40 min;
(2) preparing a blank control system without adding cannabidiol according to the method of the step (1);
(3) respectively placing the solutions of the standard solution system and the blank control system in a quartz cuvette, scanning synchronously on a fluorescence spectrophotometer with excitation light wavelength consistent with emission light wavelength to obtain resonance Rayleigh scattering spectrum, and measuring the scattering peak intensity of the standard solution at 450nm to obtainISimultaneous measurement of scattering for the placebo systemPeak intensityI 0CalculatingΔI=I-I 0 ；
(4) To be provided withΔIA standard curve is made for the cannabidiol standard solution concentration relationship:ΔI=157283C-105.554（R 2= 0.9914), the unit of the cannabidiol concentration C is mg/m L, and the linear range is 0.002-0.020 mg/m L;
(5) dissolving 5.0mg of industrially extracted cannabidiol sample in an analytically pure ethanol and dissolving the sample in a 500m L volumetric flask to prepare a cannabidiol sample ethanol solution, taking a 10m L colorimetric tube, sequentially adding a polyethylene glycol solution with the mass percent of 1.0m L of 0.2%, a silver nitrate solution with the mass percent of 1.0m L0.5.5 g/L, a sodium hydroxide solution with the mass percent of 0.5m L0.7.7 g/L, an ammonia water solution with the mass percent of 0.8% of 0.5m L and a cannabidiol sample ethanol solution with the mass percent of 1.0m L, fixing the volume by using distilled water, uniformly mixing, reacting in a water bath at 70 ℃ for 40min to prepare a sample solution to be detected, and determining the Rayleigh resonance scattering peak intensity of the sample solution according to the method in the step (3)I Sample (A)=1310.0；
(6) Calculating the concentration of cannabidiol in the sample solution according to the standard curve of the step (4)C Sample (A)=0.0090mg/m L, by the formula:
the cannabidiol content of the extract was calculated to be 90.0% and RSD (n = 6) was calculated to be 9.4% for 6 replicates.
(7) Using the sample solution to be tested prepared in the step (5) as a sample, preparing a recovery rate solution with the concentration of 0.01748mg/m L, and observing the solution, calculating the recovery rate to be 84.7% and the RSD (n = 6) to be 8.5%.
Claims (1)
1. The method for determining the content of industrially extracted cannabidiol based on the silver nano resonance Rayleigh scattering spectrometry comprises the following steps:
(1) a standard solution system for preparing the cannabidiol is prepared by sequentially adding a polyethylene glycol solution with the mass percentage of 1.0m L of 0.1-1.0%, a silver nitrate solution with the mass percentage of 1.0m L0.1.1-1.0 g/L, a sodium hydroxide solution with the mass percentage of 0.5m L0.1-1.0 g/L and an ammonia water solution with the mass percentage of 0.1-1.0% of 0.5m L into a colorimetric tube with the mass percentage of 10m L, uniformly mixing, adding a cannabidiol standard solution with the mass percentage of 1.0m L0.001.001-0.020 mg/m L, fixing the volume by using distilled water, uniformly mixing, and reacting in a water bath at the temperature of 50 ℃ for 40 min;
(2) preparing a blank control system without adding cannabidiol according to the method of the step (1);
(3) respectively placing the solutions of the standard solution system and the blank control system in a quartz cuvette, scanning synchronously on a fluorescence spectrophotometer with excitation light wavelength consistent with emission light wavelength to obtain resonance Rayleigh scattering method spectrum, and measuring the scattering peak intensity of the standard solution at 450nm to obtainISimultaneously measuring the intensity of the scattering peak of the blank control systemI 0 CalculatingΔI=I-I 0 ；
(4) To be provided withΔIMaking a standard curve for the concentration relation of the cannabidiol standard solution;
(5) getmDissolving a mg industrially extracted cannabidiol sample in an analytical pure ethanol, dissolving and dissolving in an V m L volumetric flask, preparing a sample solution to be detected according to the method in the step (1), replacing the added cannabidiol standard solution with the sample solution, and determining the resonance Rayleigh scattering peak intensity of the sample solution according to the method in the step (3)I Sample (A) ；
(6) Calculating the concentration of cannabidiol in the sample solution according to the working curve of the step (4)C Sample (A) By the formula: content (%) =C Sample (A) ×V÷m× 100 the content of cannabidiol in the extract can be calculated.
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