CN112326640A - Test paper for rapidly and directly reading and developing detection of lipid peroxide value, preparation method thereof, preparation method of standard colorimetric card and application thereof - Google Patents
Test paper for rapidly and directly reading and developing detection of lipid peroxide value, preparation method thereof, preparation method of standard colorimetric card and application thereof Download PDFInfo
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- CN112326640A CN112326640A CN201910718459.8A CN201910718459A CN112326640A CN 112326640 A CN112326640 A CN 112326640A CN 201910718459 A CN201910718459 A CN 201910718459A CN 112326640 A CN112326640 A CN 112326640A
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- G—PHYSICS
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G—PHYSICS
- 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
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N2021/0106—General arrangement of respective parts
- G01N2021/0112—Apparatus in one mechanical, optical or electronic block
Abstract
The invention discloses a preparation method and a specific application of test paper capable of quickly and directly reading, developing and quickly detecting the peroxide value of grease. The preparation method comprises the following steps: (1) preparing a precursor solution; (2) leading the precursor solution to pass through the dehydrated filter membrane by suction filtration so as to lead the filter membrane to adsorb the precursor solution in a saturated way; (3) preparing a ferrous ion solution; (4) the ferrous ion solution passes through a filter membrane by suction filtration, and a nano titanium dioxide coated ferrous ion compound membrane is generated by reaction; (5) and washing the composite membrane by using absolute ethyl alcohol to obtain a final finished membrane, packaging a finished product and detecting application. The chromogenic compound test paper constructed by the invention has very high chromogenic sensitivity to the peroxide value of the grease, the grease sample obtained by carrying out proper pretreatment on a food sample and the grease can realize direct-reading rapid detection of the peroxide value, and the chromogenic compound test paper has better correlation with a national standard method.
Description
Technical Field
The invention relates to a test paper for directly reading color development and rapidly detecting lipid peroxide value, a preparation method thereof, a preparation method of a standard colorimetric card and application thereof, belonging to the technical field of rapid detection of food quality and safety.
Background
In recent years, the color development direct-reading detection technology has great market demands in the fields of food processing, drug analysis, agricultural product safety, environmental monitoring, clinical medicine and the like. Compared with the instrument analysis technology, the color development direct-reading detection saves time, reduces analysis cost, and is beneficial to production and researchers to quickly determine the nature and quantity of specific compounds.
The edible oil is an important component of human diet and is one of three major nutrients for human beings. The grease is easily oxidized by itself due to the influence of factors such as air, light, temperature and the like during storage, so that various peroxides are generated. Although the peroxide generated by the oxidation of the grease can not cause harm to the human body in a short period, the peroxide is unstable and is easily decomposed into micromolecular volatile substances such as aldehydes, ketones, alcohols and the like, and meanwhile, the oxidation of fragrant substances, vitamins and the like is promoted, so that the complete rancidity of the grease is caused, and the rancidity grease is not beneficial to the health of the human body after being eaten for a long time, because the peroxide can damage the cell structure, and the gastric cancer, the liver cancer, the atherosclerosis, the myocardial infarction, the hair loss, the weight loss and the like are caused. The peroxide value is an index indicating the degree of oxidation of fats and oils, fatty acids, and the like, and is used to indicate whether or not a product is deteriorated by oxidation. Therefore, it is necessary to detect the peroxide value of the oil or fat.
The existing peroxide value detection method mainly comprises the following steps: chemical titration, ultraviolet detection, high performance liquid chromatography, ferric thiocyanate, xylenol orange, near infrared spectroscopy, electrochemical methods, and the like. The iodometry method has long reaction time and complicated steps, the reagent needs to be prepared more than one week in advance, the operation needs to be carried out by professional operators, and the iodometry method is easily interfered by human factors. High performance liquid chromatography, near infrared spectroscopy and the like require large-scale precise instruments which are generally expensive and high in detection cost, require special experimenters to operate and analyze data, and are difficult to meet the requirements of rapid, simple, accurate, on-site real-time and other measurement in the quality detection process.
Disclosure of Invention
Compared with the existing method, the method has the advantages of simple and convenient experimental steps, no limitation on detection places, no toxicity or harm, and no influence on the health and environment of detection personnel. The dosage of the experimental sample is less, and the detection speed is higher.
The invention also aims to provide the application of the test paper for rapidly and directly reading, developing and rapidly detecting the lipid peroxide value
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of test paper for rapidly and directly reading and developing to detect the peroxide value of grease comprises the following steps:
step (1), preparing a precursor solution;
step (2), leading the precursor solution to pass through a filter membrane subjected to dehydration treatment by utilizing suction filtration, and leading the filter membrane to adsorb the precursor solution in a saturated way;
step (3), preparing a ferrous ion solution with a certain concentration;
step (4), the prepared ferrous ion solution passes through the filter membrane treated in the step (2) by suction filtration, and a ferrous ion compound membrane wrapped by the precursor solution is generated by reaction;
and (5) washing the composite membrane by using absolute ethyl alcohol to obtain a final finished membrane, and packaging the finished product to obtain the test paper for detection.
Preferably, the steps (2) to (4) are repeated, and a plurality of layers of precursor solution wrapped ferrous ion composite films are obtained through layer-by-layer assembly.
Preferably, the precursor solution in the step (1) is tetrabutyl titanate solution, and the concentration is 0.1 mol/L.
Preferably, the concentration of the ferrous ion solution in the step (3) is 0.01-0.05 mol/L.
Preferably, before the precursor solution passes through the filter membrane in the step (2), the filter membrane is rinsed with ethanol for 3 times and is drained for 3-5 min.
The material of the filter membrane is natural cellulose.
Preferably, the filter is a neutral filter paper or a Whatman filter paper.
A method for preparing a standard colorimetric card by using the test paper prepared by the preparation method comprises the following steps:
(1) placing the test paper on an electric sample applicator, and setting the temperature to be 70-80 ℃;
(2) slowly printing 10-50 mu L of potassium thiocyanate solution with the mass volume percentage concentration of 10-30% on the test paper by using a sample injector to ensure that the potassium thiocyanate solution is uniformly distributed;
(3) after the potassium thiocyanate solution is dried, the test paper is taken down and is prevented from contacting other objects, and grease is prevented from leaking to other objects;
(4) respectively dripping the grease diluted by different peroxide values on test paper in equal quantity to ensure that the grease is uniformly distributed;
(5) and waiting for the color development of the test paper, manufacturing standard color blocks according to the color development result of the standard solution, arranging the standard color blocks according to the peroxide value of the grease, and pasting to prepare a standard color comparison card.
The invention also protects the application of the test paper in the oil oxidation detection.
Preferably, the application comprises the steps of:
dripping potassium thiocyanate solution on a test paper sheet, and dripping a sample to be tested diluted by an organic solvent on the test paper sheet after drying so as to uniformly distribute the sample; when the color development is stable, the range of the peroxide value of the sample to be detected can be obtained by comparing the color development with a standard color comparison card.
The detection principle of the peroxide value of the test paper for rapidly and directly reading the peroxide value of the grease is as follows: ferrous ions are constructed on the surface of the filter paper through a sol-gel method, the peroxidation of the grease is utilized, the ferrous ions are converted into ferric ions and potassium thiocyanate to generate an orange red complex, the color depth is in positive correlation with the peroxide value of the grease, therefore, the color of the grease peroxide value test paper is deepened along with the increase of the peroxide value in the sample, the color can be distinguished by naked eyes in different concentration ranges, and then the peroxide value in the sample is calculated through comparison with a standard colorimetric card.
The invention has the following beneficial effects:
(1) the material of the filter membrane used in the invention is natural cellulose, and the filter membrane has rich sources, low price and easy obtainment; (2) due to the multilayer wrapping and bonding crosslinking effects of the nano titanium dioxide, ferrous ions are effectively fixed and uniformly distributed in the filter membrane fixed phase, and the filter membrane has very high color development sensitivity; (3) according to the invention, potassium thiocyanate is used as a color developing agent, ferrous ions are converted into ferric ions by utilizing the oxidability of grease, the ferric ions and the potassium thiocyanate undergo a complex reaction, and the generated orange-red complex is very stable, so that the stability is more excellent; (4) the nano titanium dioxide used for compounding ferrous ions is stable in property and colorless, and the color development of the filter paper sheet is not influenced; (5) because of the extremely high specific surface area of the nano material, the sensitivity of color development is improved, and the time for color development is greatly reduced; (6) compared with the prior art, the method has the advantages of simple experimental steps, simple equipment, no limitation on detection places, small amount of required samples, no toxicity and harm, no influence on the health and environment of detection personnel, realization of direct-reading rapid detection of the peroxide value of the grease, and better correlation with the national standard method.
Drawings
FIG. 1 is a schematic diagram of the reaction principle of ferric ions and thiocyanate.
FIG. 2 is a scanning electron microscope image of the microstructure of nano titanium dioxide/ferrous ion adsorbed on the surface of cellulose.
FIG. 3 is an elemental analysis spectrum of a ferrous ion-nano titanium dioxide composite filter paper.
Fig. 4 is a standard colorimetric card prepared according to the present invention.
FIG. 5 is a standard curve of peroxide values versus number and gray scale values.
Detailed Description
The invention is further illustrated by the following examples and figures.
Example 1
A preparation method of test paper for rapidly and directly reading and developing to detect the peroxide value of grease comprises the following steps:
(1) a 100mM solution of tetrabutyl titanate in toluene/ethanol (v: v ═ 1: 1) was prepared and stirred at room temperature for one hour.
(2) Preparing a ferrous chloride solution of 0.035mol/L, wherein the specific preparation method comprises the steps of weighing 0.7g of ferrous chloride tetrahydrate, dissolving in water, adding 2ml of hydrochloric acid solution of 10mol/L, and fixing the volume to 100ml by using water.
(3) The quantitative filter paper is placed in a suction filtration device, rinsed 3 times with ethanol, the water is removed, and the filter paper is dried by air flow for 5 min. And transferring about 10mL of tetrabutyl titanate solution, adding the tetrabutyl titanate solution into a suction filtration device, and standing for 3 minutes to enable the tetrabutyl titanate solution to be fully soaked in the cellulose paper.
(4) The suction filtration device was turned on so that the tetrabutyl titanate solution was slowly filtered through the cellulose paper, followed by addition of ethanol for 3 rinses and standing for 2 minutes.
(5) And (3) removing the residual ethanol by using a suction filtration device, adding the ferrous chloride solution prepared in the step (2), and standing for 2 minutes to enable the ferrous chloride solution to be fully soaked in the cellulose paper.
(6) The suction filtration device was turned on so that the ferrous chloride solution was slowly filtered through the cellulose paper, followed by addition of absolute ethanol for 3 rinses and standing for 2 minutes.
(7) After one period is finished, repeating the process for 2 times again to obtain the multilayer nano titanium dioxide ferrous ion composite membrane.
The scanning electron micrograph of the microstructure of the nano titanium dioxide/ferrous ion adsorbed on the surface of the cellulose is shown in fig. 2, and it can be seen that the nano titanium dioxide/ferrous ion composite is constructed on the filter paper more tightly and uniformly.
An element analysis spectrum of the ferrous ion-nano titanium dioxide composite filter paper is shown in fig. 3, the strength of each element under different voltages is shown, and the existence of Fe and Ti can be obviously observed.
Example 2
The preparation method of the standard colorimetric card comprises the following steps
Cutting the test paper sheet prepared in the example 1 into a plurality of small paper sheets of 0.5 x 1 cm;
placing the small paper sheets on an electric sample applicator, and setting the temperature to be 80 ℃;
thirdly, slowly printing 10 mu L of potassium thiocyanate solution on the paper by using a sample injector to ensure that the potassium thiocyanate solution is uniformly distributed;
after waiting for drying (about 1min), taking down and avoiding contacting with other objects, and preventing grease from leaking to other objects;
fifthly, after diluting different peroxide values (0, 0.0076%, 0.08%, 0.15%, 0.27%, the grease is dissolved in 5 times of volume
In chloroform solution) is respectively dripped on the filter paper sheets in the amount of 10 mu L to be uniformly distributed;
sixthly, preparing a standard color block according to the color development result of the standard solution after color development, and enabling the standard color block to be according to the oil peroxide value
The height is arranged and pasted to prepare a standard colorimetric card (figure 4).
Example 3
The method for detecting the oxidation degree of the edible oil by using the grease peroxide value detection test paper comprises the following steps:
pretreating waste oil (No. 1 and No. 2) of rice bran oil/olive oil with different degrees according to national standard (GB 5009.227-2016), taking 1mL of chloroform into a 50mL centrifuge tube, sucking 200 μ L of oil sample by using a pipette, dissolving the oil sample in the chloroform, and oscillating for 1min for later use. And (3) placing the cut filter paper sheet on a heating plate of an electric sample applicator, setting the temperature to be 80 ℃, and slowly dripping 10 mu L of 30% potassium thiocyanate solution on the paper sheet to ensure that the paper sheet is uniformly distributed. Waiting for drying for about 1min, the diluted rice bran oil and olive oil were dropped onto the filter paper sheet in an amount of 10 μ L, respectively, to be uniformly distributed, and when the color development was stabilized, the approximate ranges of peroxide values of rice bran oil and olive oil were 0.08% and 0.15%, respectively, for No. 1 oil and more than 0.27%, respectively, by comparing with the standard color chart prepared in example 2. Therefore, the oxidation degree of the grease can be rapidly detected in real time through the detection test paper. The principle is as shown in figure 1.
In addition, the grease to be detected is quantitatively detected according to a titration method in the national standard (GB 5009.227-2016), and the peroxide values of the grease are respectively 0.1432% and 0.2827%. Therefore, the method has better correlation and consistency with the national standard method.
Example 4
The method for detecting the peroxide value of the edible oil by using the grease peroxide value detection test paper comprises the following steps:
and (4) drawing a grease peroxide value standard curve. The prepared filter paper is cut into a plurality of 0.5 x 1cm paper sheets, and the paper sheets are placed on a heating plate of an electric spotter at the temperature of 80 ℃. Then respectively dripping 10 mu L of 30% potassium thiocyanate solution to ensure that the potassium thiocyanate solution is uniformly distributed, and respectively dripping 10 mu L of solution prepared by mixing 1: 5 (peroxide values of 0, 0.0076%, 0.08%, 0.15%, 0.27% respectively) in chloroform, and measuring the gray value of the filter paper with an instrument after color development is stabilized, and establishing a standard curve of the gray value and the peroxide value of the oil (FIG. 5).
Taking rice bran oil and olive oil as samples to be detected, taking 1mL of chloroform in a 50mL centrifuge tube, sucking 200 mu L of oil sample by using a pipette gun, dissolving in chloroform, and oscillating for 1min for later use. And (3) placing the cut filter paper sheet on a heating plate of an electric sample applicator, setting the temperature to be 80 ℃, and slowly dripping 10 mu L of 30% potassium thiocyanate solution on the paper sheet to ensure that the paper sheet is uniformly distributed. Waiting for drying for about 1min, respectively dripping diluted rice bran oil and olive oil onto filter paper sheets in an amount of 10 μ L to uniformly distribute, respectively measuring gray values of the filter paper after color development is stable, obtaining the peroxide value of the oil to be measured from a standard curve (figure 5) of the peroxide value, and judging the oxidation degree.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims (10)
1. A preparation method of test paper for rapidly and directly reading and developing to detect the peroxide value of grease is characterized by comprising the following steps:
step (1), preparing a precursor solution;
step (2), leading the precursor solution to pass through a filter membrane subjected to dehydration treatment by utilizing suction filtration, and leading the filter membrane to adsorb the precursor solution in a saturated way;
step (3), preparing a ferrous ion solution with a certain concentration;
step (4), the prepared ferrous ion solution passes through the filter membrane treated in the step (2) by suction filtration, and a ferrous ion compound membrane wrapped by the precursor solution is generated by reaction;
and (5) washing the composite membrane by using absolute ethyl alcohol to obtain a final finished membrane, and packaging the finished product to obtain the test paper for detection.
2. The method for preparing the test paper for rapidly and directly reading and developing the peroxide value of the grease according to claim 1, which is characterized in that: and (5) repeating the steps (2) to (4), and obtaining the ferrous ion composite film wrapped by the multilayer precursor solution through multiple layer-by-layer assembly.
3. The method for preparing the test paper for rapidly and directly reading and developing the peroxide value of the grease according to claim 1, which is characterized in that: the precursor solution in the step (1) is tetrabutyl titanate solution, and the concentration is 0.1 mol/L.
4. The method for preparing the test paper for rapidly and directly reading and developing the peroxide value of the grease according to claim 1, which is characterized in that: the concentration of the ferrous ion solution in the step (3) is 0.01-0.05 mol/L.
5. The method for preparing the test paper for rapidly and directly reading and developing the peroxide value of the grease according to claim 1, which is characterized in that: and (3) before the precursor solution passes through the filter membrane in the step (2), rinsing the filter membrane for 3 times by using ethanol and pumping for 3-5 min.
6. A test paper produced by the production method according to any one of claims 1 to 5, characterized in that: the filter membrane is made of natural cellulose.
7. The test strip of claim 6, wherein: the filter membrane is neutral filter paper or Whatman filter paper.
8. A method for preparing a standard colorimetric card by using the test paper prepared by the preparation method according to any one of claims 1 to 5, which is characterized by comprising the following steps:
(1) placing the test paper on an electric sample applicator, and setting the temperature to be 70-80 ℃;
(2) slowly printing 10-50 mu L of potassium thiocyanate solution with the mass volume percentage concentration of 10-30% on the test paper by using a sample injector to ensure that the potassium thiocyanate solution is uniformly distributed;
(3) after the potassium thiocyanate solution is dried, the test paper is taken down and is prevented from contacting other objects, and grease is prevented from leaking to other objects;
(4) respectively dripping the grease diluted by different peroxide values on test paper in equal quantity to ensure that the grease is uniformly distributed;
(5) and waiting for the color development of the test paper, manufacturing standard color blocks according to the color development result of the standard solution, arranging the standard color blocks according to the peroxide value of the grease, and pasting to prepare a standard color comparison card.
9. Use of a test strip according to claim 6 in the detection of oxidation of oils and fats.
10. The use of claim 9, comprising the steps of:
dripping potassium thiocyanate solution on a test paper sheet, and dripping a sample to be tested diluted by an organic solvent on the test paper sheet after drying so as to uniformly distribute the sample; when the color development is stable, the range of the peroxide value of the sample to be detected can be obtained by comparing the color development with a standard color comparison card.
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| CN113533314A (en) * | 2021-06-24 | 2021-10-22 | 卡莱丽化妆品有限公司 | Rapid detection method for acid value and peroxide value of snake fat |
| CN114280040A (en) * | 2021-11-18 | 2022-04-05 | 中国农业科学院油料作物研究所 | Test strip for detecting peroxide value of edible oil, preparation method and application thereof |
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| CN113533314A (en) * | 2021-06-24 | 2021-10-22 | 卡莱丽化妆品有限公司 | Rapid detection method for acid value and peroxide value of snake fat |
| CN114280040A (en) * | 2021-11-18 | 2022-04-05 | 中国农业科学院油料作物研究所 | Test strip for detecting peroxide value of edible oil, preparation method and application thereof |
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