CN114460048A - Method for determining mass content of polar substances in edible oil by perovskite quantum dot fluorescence quenching method - Google Patents
Method for determining mass content of polar substances in edible oil by perovskite quantum dot fluorescence quenching method Download PDFInfo
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- 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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- G01N21/64—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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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- 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
- 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"
- G01N2021/6432—Quenching
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Abstract
The application discloses a method for determining the mass content of polar substances in edible oil by using a perovskite quantum dot fluorescence quenching method, which comprises the following steps: s1, obtaining an edible oil standard series group which comprises a plurality of standard edible oil samples, wherein the different standard edible oil samples have different mass contents of polar substances; s2, obtaining a solution containing perovskite quantum dots; s3, mixing the solution containing the perovskite quantum dots with a standard edible oil sample, measuring the fluorescence intensity of each mixed solution under a preset condition, and establishing a linear function relation between the mass content of the polar substances in the standard edible oil sample and the fluorescence intensity; and S4, mixing the edible oil sample to be detected with the solution containing the perovskite quantum dots, measuring the fluorescence intensity of the mixed solution under the preset condition, and measuring the content of the polar substances in the edible oil to be detected by utilizing the linear function relationship. The method is low in cost, easy to operate and high in accuracy, and provides a new basis for the application of the perovskite quantum dots in the field of food safety.
Description
Technical Field
The invention relates to the application field of perovskite quantum dots, in particular to a method for determining the mass content of polar substances in edible oil by using a perovskite quantum dot fluorescence quenching method.
Background
The edible oil can be continuously and repeatedly used at high temperature to generate a series of reactions such as oxidation, polymerization, cracking, hydrolysis and the like. In these processes, various compounds containing carbonyl group, carboxyl group, ketone group, aldehyde group, etc. are generated, and since these compounds have a polarity higher than that of triglycerides, they are collectively called polar compounds, and particularly in edible oil, polar compounds are continuously generated during frying. These compounds not only have adverse effects on the quality of the oil itself, but also cause direct damage to human health, for example, growth retardation, liver enlargement, reproductive and hepatic dysfunction, lymphocyte aberration, etc. Therefore, it is important to effectively evaluate the quality of the edible oil. The indexes for evaluating the quality of the edible oil mainly comprise sense, light transmittance, acid value, peroxide value, carbonyl value, iodine value, free fatty acid, polymer, total polar compound content and the like. The method for measuring the content of the polar compounds has the characteristics of high accuracy, high reliability and the like, and is the most stable index, so the method becomes an evaluation index recommended to be used in all countries in the world, and the content of the polar compounds in the frying oil is required to be not higher than 27% (by mass) according to national standards of China.
Column chromatography, especially preparative fast column chromatography is a method for measuring polar components of edible oil in national food safety standard of China, but the method is time-consuming and labor-consuming, needs to consume a large amount of organic solvent, and cannot realize fast and real-time monitoring of the mass content of total polar substances.
In recent years, many methods for detecting the mass content of total polar substances in edible oil have appeared, including infrared spectroscopy, nuclear magnetic resonance, dielectric constant method and the like.
The infrared spectroscopy method relates to the step of enabling an oil sample to be 4000-10000 cm-1Scanning is performed. Because the grease can form substances such as aldehyde, ketone, acid and the like in the using process, the intensity and the position of the characteristic peak of each group are different in the infrared absorption spectrogram obtained by oil samples with different polar substance contents, and therefore, the content of the polar substance is judged according to the intensity and the position of the characteristic peak of the infrared absorption spectrogram. However, infrared spectrometers are expensive and require calibration modeling at an early stage of use.
The detection principle of the nuclear magnetic resonance method is that the relaxation time of the grease changes along with the change of the content of polar substances. The higher the polar material content is, the shorter the relaxation time is, and by establishing a mathematical relationship between the polar material content and the relaxation time, the polar material content can be determined from the relaxation time. However, the apparatus used in this method is expensive and requires a professional to operate, and thus it is difficult to obtain a wide range of applications in a short time.
The dielectric constant method is to measure the polar material based on the principle that the oil-like conductivity is increased with the increase of the content of the polar material, and the dielectric constant is proportional to the capacitance. The content of polar substances can thus be determined by measuring the capacitance. The portable edible oil quality detector based on the principle is commercialized, but the instrument is still expensive in manufacturing cost, needs to be calibrated before use, and is easily influenced by electromagnetic fields, temperature and the like to cause inaccuracy of measurement results.
Therefore, the present invention provides a method for determining the mass content of polar substances in edible oil with low cost, easy operation and high accuracy.
Disclosure of Invention
To provide a method for measuring edible oil with low cost, easy operation and high accuracy. The inventors of the present application have found that polar substances in edible oils can affect the stability of perovskite quantum dots. Since the perovskite quantum dot belongs to an ionic crystal, the perovskite quantum dot cannot exist stably when being damaged by polar substances. By utilizing the unique property of sensitivity to polar substances, the perovskite quantum dots are used for quantitative analysis of the polar substances in the edible oil by the inventor.
The application provides a method for determining the mass content of polar substances in edible oil by using a perovskite quantum dot fluorescence quenching method, which comprises the following steps:
s1: obtaining an edible oil standard series group, wherein the edible oil standard series group comprises a plurality of standard edible oil samples, each standard edible oil sample comprises polar substances with known mass content, and the mass content of the polar substances in different standard edible oil samples is different;
s2: obtaining a solution containing perovskite quantum dots;
s3: respectively mixing the solution containing the perovskite quantum dots with the plurality of standard edible oil samples to obtain a plurality of mixed solutions, respectively measuring the fluorescence intensity of each mixed solution under a preset condition, and establishing a linear function relation between the mass content of the polar substances in the standard edible oil samples and the fluorescence intensity;
s4: and after uniformly mixing the edible oil sample to be detected with the solution containing the perovskite quantum dots, measuring the fluorescence intensity of the mixed solution under the preset condition, and measuring the mass content of the polar substances in the edible oil to be detected by utilizing the linear function relationship.
Specifically, the method for determining the mass content of the polar substances in the edible oil by using the perovskite quantum dot fluorescence quenching method comprises the following steps: step (1), a series of edible oil samples with known polar substance mass content are sucked and added into a centrifuge tube filled with quantum dot solution, and the mixture is fully mixed; and (2) sucking the mixed solution into a cuvette, and placing the cuvette into a fluorometer to measure the fluorescence intensity, wherein due to different contents of polar substances, different oil samples have different degrees of quenching of the fluorescence of the quantum dots, and the measured fluorescence intensities are also different. Recording the fluorescence intensity of all oil samples after reaction with the solution containing the perovskite quantum dots; step (3), taking the content of the polar substances in the oil sample as an independent variable x, taking the fluorescence intensity of the mixed solution as a dependent variable y, and establishing a linear equation between the mass content of the polar substances and the fluorescence intensity by regression analysis; and (4) according to the operation methods of the steps (1) and (2) and the linear equation obtained in the step (3), measuring the fluorescence intensity of the oil sample with unknown polar substance mass content after the reaction with the solution containing the perovskite quantum dots, substituting the obtained fluorescence intensity into the obtained linear equation to obtain the mass content of the polar substance in the oil sample, and verifying the obtained polar substance content by adopting a column chromatography.
Optionally, the preset condition includes: the range of fluorescence excitation wavelength lambda ex is 350-370 nm, and the emission wavelength of detection is 512-515 nm.
Alternatively, the fluorescence excitation wavelength λ ex is any value or a range value determined by any two values among 350nm, 365nm and 370 nm.
Optionally, in step S1, the volume of the edible oil is 0.1-1 mL, the concentration of the perovskite quantum dots is 10-30 mg/mL, the volume of the perovskite quantum dot solution is 0.1-3 mL, and the mixing reaction time is 1-10 minutes.
Optionally, the concentration of the perovskite quantum dots is any value of 10mg/mL, 14mg/mL, 25mg/mL30mg/mL, or any two determined range values.
Optionally, in the step S1, the edible oil is a blend oil selected from one or more of soybean oil, corn oil, sunflower oil, olive oil, peanut oil, rice bran oil and palm oil.
Optionally, the perovskite quantum dots are selected from CH3NH3PbX3、CH(NH2)2PbX3And CsPbX3Wherein, X is selected from one or more of Cl, Br and I.
Optionally, the solvent in the solution containing the perovskite quantum dots is selected from one of n-hexane, cyclohexane and toluene.
Optionally, the linear function relationship is y ═ ax + b, R2And more than or equal to 0.993, wherein x is the mass content of polar substances in the edible oil, y is the fluorescence intensity of a mixed solution of the edible oil and the solution containing the perovskite quantum dots, a is in the range of 3500-17000, and b is in the range of 3000-11000.
Alternatively, a is any of 3590, 4542 and 16370 and b is any of 3239, 5774 and 10583.
Optionally, the edible oil is olive oil, and the linear function relationship is-3590 x +3239, R20.993, wherein x is the mass content of polar substances in olive oil, y is the fluorescence intensity of a mixed solution of the olive oil and the solution containing the perovskite quantum dots, and R is2Is a linear correlation coefficient.
Optionally, the edible oil is soybean oil, and the linear function relationship is-16370 x +10583, R20.983, wherein x is the mass content of polar substances in the soybean oil, and y is the fluorescence intensity of the mixed solution of the soybean oil and the solution containing the perovskite quantum dots.
Optionally, the edible oil is sunflower seed oil, and the linear function relationship is-4542 x +5774, R2And (2) 0.980, wherein x is the mass content of polar substances in the sunflower seed oil, and y is the fluorescence intensity of the mixed solution of the sunflower seed oil and the solution containing the perovskite quantum dots.
Optionally, a series of edible oils containing different mass contents of polar substances has at least 5 different mass contents of polar substances, i.e. the number of samples selected for each linear function is 5 or more.
Optionally, the amount of polar material in the edible oil is any one or two of 18.5%, 20.5%, 21.5%, 23%, 25%, 26%, 26.5%, 27.5%, 28%, 29%, 30%, 30.5%, 33%.
The beneficial effects that this application can produce include:
1) the novel edible oil detection method provided by the application is simple and convenient to operate, low in cost, and capable of realizing real-time detection rapidly and efficiently, greatly shortens detection time, reduces the usage amount of organic reagents, and is based on the quantum dot fluorescence quenching principle, high in detection reaction sensitivity, good in reproducibility, high in detection result accuracy and high in precision.
2) The method provided by the application can realize the detection of the total polar substances of the edible oil at room temperature without heating, so that the influence of the temperature on the detection result is avoided.
3) The method provided by the application expands the application range of the perovskite quantum dot, and provides a new basis for the application of the perovskite quantum dot in the field of food safety.
Drawings
FIG. 1 shows a linear function of the content of polar substances in olive oil as a function of the fluorescence intensity according to example 1 of the present invention.
FIG. 2 is a graph showing the linear function of the content of polar substances in soybean oil and the fluorescence intensity according to example 2 of the present invention.
FIG. 3 shows the polar material content of sunflower oil as a function of fluorescence intensity in a linear manner according to example 3 of the present invention.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
The endpoints of the ranges and any values disclosed in the present application are not limited to the precise range or value, and such ranges or values should be understood to include proximity to such ranges or values. For numerical ranges, the endpoints of each of the ranges and the individual points between each may be combined with each other to give one or more new numerical ranges, and these numerical ranges should be considered as specifically disclosed herein.
Unless otherwise specified, the edible oil and the solvent and the like in the examples of the present application are commercially available, for example, by purchasing in a supermarket.
Perovskite quantum dots in the examples of the present application are all prepared by known methods, specifically please refer to Song, j.z.etc. from-temporal triple-ligand surface engineering synthetic carbohydrates link stability, registration dynamics, and charge injection aware qe-11.6% peroxide qleds.
In the examples of the present application, the fluorescence intensity was measured by a fluorescence spectrometer (FL4600, Hitachi corporation, japan), and the specific test conditions were: the range of fluorescence excitation wavelength lambda ex is 350-370 nm, the detected emission wavelength lambda em is 512-515 nm, and the scanning speed is as follows: 1200nm/min, excitation wavelength slit: 10mn, emission wavelength slit: 10 nm.
The column chromatography in the examples of the present application is a method commonly used in the prior art, for example, refer to the national standard GB-5009.202-2016.
Example 1
This example shows a method for determining the mass content of polar substances in olive oil using the perovskite quantum dot fluorescence quenching method.
Specifically, 1mL of olive oil samples with polar substance mass contents of 18.5%, 20.5%, 21.5%, 25%, 26.5% and 30% are respectively sucked, and 2mLCsPBBr is added3Fully mixing quantum dots (with the concentration of 10mg/mL) in a toluene solution in a centrifugal tube at room temperature; after 3 minutes of reaction, 1mL of the mixed solution was aspirated into a quartz cuvette, and the fluorescence intensity of the mixed solution was measured by a fluorescence spectrometer, with the excitation wavelength λ ex being 365nm and the emission wavelength λ em being 512nm, and each group was measured in parallel 3 times; establishing a linear equation between the fluorescence intensity and the polar substance mass content of the olive oil, wherein the fluorescence of the mixed solution is increased along with the increase of the polar substance mass contentThe intensity gradually decreases, and the linear equation obtained is that y is-3590 x +3239, R2X is the mass content of polar substances in olive oil (i.e. TPM in fig. 1), and y is the fluorescence intensity of the mixed solution of olive oil and the solution containing perovskite quantum dots, as shown in fig. 1.
According to the above method, the fluorescence intensity of an olive oil sample with unknown mass content of polar substances was measured to be 2257, and the content of polar substances was found to be 27.4% by substituting into the equation. The oil sample was verified by column chromatography and found to be 27.5%. Thus indicating the use of CsPbBr3The quantum dot fluorescence quenching method can be used for accurately and quantitatively measuring the mass content of the polar substances of the olive oil.
Example 2
This example shows a method for determining the mass content of polar substances in soybean oil using the perovskite quantum dot fluorescence quenching method.
Specifically, 0.5mL of soybean oil samples containing 25%, 26%, 27.5%, 28%, 29%, 30%, and 30.5% by mass of polar substances was aspirated, and 1mL of a dry solution of BSBr was added3Fully mixing quantum dots (with the concentration of 14mg/mL) in a toluene solution in a centrifuge tube at room temperature; after 1 minute of reaction, 1mL of the mixed solution was aspirated into a quartz cuvette, and the fluorescence intensity of the mixed solution was measured by a fluorescence spectrometer, with the excitation wavelength λ ex being 365nm and the emission wavelength λ em being 512nm, and each group was measured in parallel 3 times; establishing a linear equation between the fluorescence intensity and the mass content of the polar substances of the soybean oil, gradually weakening the fluorescence intensity of the mixed solution along with the increase of the mass content of the polar substances, and obtaining the linear equation of-16370 x + 10583R2X (i.e., TPM in fig. 2) is the mass content of polar substances in the soybean oil, and y is the fluorescence intensity of the mixed solution of the soybean oil and the solution containing perovskite quantum dots, as shown in fig. 2.
According to the method, the fluorescence intensity of the soybean oil sample with unknown mass content of the polar substance is measured, the fluorescence intensity is measured to be 5637, and the fluorescence intensity is substituted into the equation to obtain that the content of the polar substance is 30.2%. The oil sample was verified by column chromatography and found to be 30.5%. Thus indicating the use of CsPbBr3Quantum dot fluorescence quenchingThe extinguishing method can be used for accurately and quantitatively measuring the mass content of the polar substances of the soybean oil.
Example 3
This example shows a method for determining the mass content of polar substances in sunflower seed oil using the perovskite quantum dot fluorescence quenching method.
Sucking 0.9mL of soybean oil samples with polar substance mass contents of 23%, 26.5%, 27.5%, 29%, 30.5% and 33%, respectively, adding 1mLCsPBBr3Fully mixing quantum dots (with the concentration of 25mg/mL) in a toluene solution in a centrifuge tube at room temperature; after reacting for 2 minutes, 1mL of the mixed solution was taken out of a quartz cuvette, and the fluorescence intensity of the mixed solution was measured by a fluorescence spectrometer, with an excitation wavelength λ ex of 365nm and an emission wavelength λ em of 512nm, and each group was measured in parallel 3 times; establishing a linear equation between the fluorescence intensity and the mass content of the polar substances in the sunflower seed oil, gradually reducing the fluorescence intensity of the mixed solution along with the increase of the mass content of the polar substances, wherein the obtained linear equation is that the mass of the mixed solution is-4542 x +5774, and R is2X (i.e. TPM in fig. 3) is the mass content of polar substances in the sunflower seed oil, and y is the fluorescence intensity of the mixed solution of the sunflower seed oil and the solution containing perovskite quantum dots, as shown in fig. 3.
According to the method, the fluorescence intensity of the sunflower seed oil sample with unknown mass content of the polar substance is measured, the fluorescence intensity is 4504, and the content of the polar substance is 27.96% by substituting the measured fluorescence intensity into an equation. The oil sample was verified by column chromatography and found to be 28%. Thus indicating the use of CsPbBr3The quantum dot fluorescence quenching method can be used for accurately and quantitatively measuring the mass content of the polar substances in the sunflower seed oil.
Although the present application only exemplifies the above embodiments, the oil samples in the above embodiments may be replaced by other types of oils, such as any one of corn oil, sunflower oil, olive oil, peanut oil, rice bran oil, and palm oil, or a blend oil of several of soybean oil, corn oil, sunflower oil, olive oil, peanut oil, rice bran oil, and palm oil, and the corresponding linear functional relationship may also be obtained. Also although the above examples use only CsPbBr3The quantum dots quench the edible oil,however, CsPbBr can be used3Replacement of quantum dots with other perovskite quantum dots, e.g. CH3NH3PbX3、CH(NH2)2PbX3And CsPbX3X is selected from one or more of Cl, Br and I.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. A method for measuring the mass content of polar substances in edible oil by using a perovskite quantum dot fluorescence quenching method is characterized by comprising the following steps:
s1: obtaining an edible oil standard series group, wherein the edible oil standard series group comprises a plurality of standard edible oil samples, each standard edible oil sample comprises polar substances with known mass content, and the mass content of the polar substances in different standard edible oil samples is different;
s2: obtaining a solution containing perovskite quantum dots;
s3: respectively mixing the solution containing the perovskite quantum dots with the plurality of standard edible oil samples to obtain a plurality of mixed solutions, respectively measuring the fluorescence intensity of each mixed solution under a preset condition, and establishing a linear function relation between the mass content of the polar substances in the standard edible oil samples and the fluorescence intensity;
s4: and after uniformly mixing the edible oil sample to be detected with the solution containing the perovskite quantum dots, measuring the fluorescence intensity of the mixed solution under the preset condition, and measuring the mass content of the polar substances in the edible oil to be detected by utilizing the linear function relationship.
2. The method according to claim 1, wherein the preset condition comprises: the range of fluorescence excitation wavelength lambda ex is 350-370 nm, and the emission wavelength of detection is 512-515 nm.
3. The method according to claim 1, wherein in step S1, the edible oil is added in a volume of 0.1-1 mL, the concentration of the perovskite quantum dots is 10-30 mg/mL, the volume of the perovskite quantum dot solution is 0.1-3 mL, and the mixing reaction time is 1-10 minutes.
4. The method according to claim 1, wherein in the step S1, the edible oil is selected from one or more blend oils of soybean oil, corn oil, sunflower oil, olive oil, peanut oil, rice bran oil and palm oil.
5. The method according to claim 1, wherein the perovskite quantum dots are selected from CH3NH3PbX3、CH(NH2)2PbX3And CsPbX3Wherein, X is selected from one or more of Cl, Br and I.
6. The method according to claim 1, wherein the solvent in the solution containing the perovskite quantum dots is selected from one of n-hexane, cyclohexane and toluene.
7. The method of claim 4, wherein the linear function relationship is y-ax + b, R2And more than or equal to 0.993, wherein x is the mass content of polar substances in the edible oil, y is the fluorescence intensity of a mixed solution of the edible oil and the solution containing the perovskite quantum dots, a is in the range of 3500-17000, and b is in the range of 3000-11000.
8. The method of claim 7, wherein the edible oil is olive oil and the linear function relationship is-3590 x +3239, R2Not less than 0.980, wherein x is the mass content of polar substances in olive oil, and y is the mixture of olive oil andthe fluorescence intensity of the mixed solution of the solution containing perovskite quantum dots.
9. The method of claim 7, wherein the edible oil is soybean oil and the linear function relationship is y-16370 x +10583, R20.983, wherein x is the mass content of polar substances in the soybean oil, and y is the fluorescence intensity of the mixed solution of the soybean oil and the solution containing the perovskite quantum dots.
10. The method according to claim 7, wherein the edible oil is sunflower oil and the linear function relationship is y-4542 x +5774, R2And (2) 0.980, wherein x is the mass content of polar substances in the sunflower seed oil, and y is the fluorescence intensity of the mixed solution of the sunflower seed oil and the solution containing the perovskite quantum dots.
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