CN111751365A - Preparation method of antioxidant flour benzoyl peroxide detection test paper - Google Patents
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Abstract
The invention provides a preparation method of antioxidant flour benzoyl peroxide test paper, which comprises the following steps: firstly, pretreating a test paper substrate; step two, preparing a color developing agent, namely weighing 3,3,5, 5-tetramethylbenzidine, adding a mixed solution of distilled water and ethanol and an aqueous solution of a surfactant, and performing ultrasonic dissolution to obtain a color developing solution; step three, loading a color developing agent; step four, preparing an antioxidant solution, namely weighing the load of the antioxidant solution in the step five; and step six, drying and cutting to obtain a finished product. The invention also correspondingly provides the test paper for detecting the antioxidant flour benzoyl peroxide. The preparation method of the antioxidant flour benzoyl peroxide test paper is simple to operate and short in time consumption, the prepared antioxidant flour benzoyl peroxide test paper is not easy to oxidize and lose efficacy, the quality guarantee period of the flour test paper is effectively prolonged, and the detection efficiency is greatly improved.
Description
Technical Field
The invention relates to the technical field of food detection, in particular to a preparation method of antioxidant flour benzoyl peroxide test paper.
Background
The Benzoyl Peroxide (BPO) is a strong oxidant, in the aspect of food, BOP (blow-off gas) is also an allowable food additive and is mainly used as a flour whitening agent, but the excessive BOP is used to damage the body, and then the addition of the benzoyl peroxide is completely prohibited from 5/1 days in 2011 according to the benzoyl peroxide announcement of withdrawing the flour whitening agent in the Ministry of health, so that the benzoyl peroxide is very important for measuring the content of the benzoyl peroxide in the flour.
At present, BPO detection methods mainly comprise methods such as gas chromatography, high performance liquid chromatography, spectrophotometry, redox titration and the like, but the methods are mainly limited to laboratory operation, need professional experimenters for carrying out the methods, are complex in operation and are not suitable for rapid field screening and detection of basic-level workers.
Although the kit colorimetric method and the test paper method are more convenient and faster than the above methods, a plurality of problems still exist, such as the name of the authorized bulletin number CN106872451B, the name of the starch-potassium iodide reagent, the preparation method of the starch-potassium iodide reagent, the test paper, the kit and the semi-quantitative detection method of benzoyl peroxide in flour, the starch-potassium iodide test paper is adopted, the preparation process is more complex, the detection limit of a flour sample is 20mg/kg, the detection limit is too high, and the sensitivity is lower; application No. 201810331485.0, entitled benzoyl peroxide test paper and its preparation method and detection method, adopts 3,3,5, 5-tetramethyl benzidine as color developing agent, and thiomicrobial ketone as promoter, and can make the product detection limit lower through the synergistic effect of two reagents, the detection limit can be 5 mg/kg; however, high- concentration 3,3,5, 5-tetramethylbenzidine is easy to be oxidized and lose efficacy when being used as a color developing solution, and the flour test paper and the preparation method thereof need to be improved in order to meet the circulation requirements of the test paper on the market and delay the shelf life of the test paper.
Disclosure of Invention
In view of the above, there is a need to provide a method for preparing a test paper for detecting benzoyl peroxide in antioxidant flour, so as to solve the above problems.
The invention provides a preparation method of antioxidant flour benzoyl peroxide test paper, which comprises the following steps:
the method comprises the following steps: pretreating a test paper substrate, selecting medium-speed qualitative filter paper as the test paper substrate, placing the test paper substrate in 20mL of ethanol, ultrasonically cleaning for three times, and drying for later use;
step two: preparing a color developing agent, namely weighing 3,3,5, 5-tetramethylbenzidine, adding a mixed solution of distilled water and ethanol, adding an aqueous solution of a surfactant after the 3,3,5, 5-tetramethylbenzidine is dissolved, and performing ultrasonic treatment to obtain a color developing solution;
step three: loading a color developing agent, namely soaking the pretreated test paper substrate in color developing solution, taking out the test paper substrate, draining the test paper substrate, and drying the test paper substrate in a vacuum drying box to obtain test paper with a color developing layer;
step four: preparing an antioxidant solution, namely weighing sodium tungstate and sodium molybdate, adding distilled water, and performing ultrasonic dissolution to obtain the antioxidant solution;
step five: loading an anti-oxidation solution, and dripping the anti-liquefaction solution on the surface of the test paper with the color development layer in a spin coating mode;
step six: drying and cutting to obtain a finished product, cutting the dried filter paper into filter paper strips, and pasting the filter paper strips on a substrate covered with double-sided adhesive tape to prepare a finished test paper product.
Further, the mass of the 3,3,5, 5-tetramethylbenzidine weighed in the second step is 0.05-0.5g, the ratio of distilled water to ethanol in the mixed solution is 1:9, and the volume of the mixed solution is 50 mL.
Further, in the second step, the surfactant is cetyl trimethyl ammonium bromide, cetyl trimethyl sodium benzene sulfonate or sodium dodecyl sulfonate.
Further, the mass of the sodium tungstate in the fourth step is 0.025-0.15g, the mass of the sodium molybdate is 0.025-0.15g, and the volume of the distilled water is 50 mL.
Further, the rotation speed during the spin coating in the sixth step is 200r/min, and annealing treatment is performed after the spin coating, wherein the annealing temperature is 50 ℃.
The application also provides an anti-oxidant flour benzoyl peroxide test paper, the test paper includes:
the substrate is obtained by processing rapid qualitative filter paper;
the color development layer is obtained by drying a mixed solution of ethanol and distilled water of 3,3,5, 5-tetramethylbenzidine;
an oxidation resistant protective layer comprising sodium tungstate and sodium molybdate.
Further, the test paper further comprises:
the portable handheld terminal comprises a bottom plate, wherein a handheld end is arranged on one side of the bottom plate;
the substrate is arranged above the bottom plate;
the base is arranged between the bottom plate and the pressing plate.
Furthermore, the pressing plate is connected with the bottom plate through an adhesive layer.
The invention provides a preparation method of antioxidant flour benzoyl peroxide test paper, which comprises the steps of pretreating a test paper substrate, preparing a color developing agent solution, adopting a mixed solution of distilled water and ethanol of 3,3,5, 5-tetramethylbenzidine, loading a color developing agent on the surface of the test paper substrate, preparing an antioxidant solution, adopting sodium tungstate and sodium molybdate as solutes, then adopting a spin coating mode to load the antioxidant solution, drying and cutting to obtain a test paper finished product. Compared with the prior art, the method is simple to operate, the obtained flour test paper is more stable in the air, the quality guarantee period is longer, the flour test paper is not easy to lose efficacy, the detection result is accurate, the detection efficiency is greatly improved, and the method is suitable for the needs of actual life.
Drawings
FIG. 1 is a flow chart of a method of making a flour test strip in one embodiment of the present invention.
FIG. 2 is an image and SEM image of the pretreated strip in one embodiment of the present invention.
Fig. 3 is a scanning electron microscope image of test paper loaded with developers of different concentrations in one embodiment of the present invention.
FIG. 4 is an EDS energy spectrum of an antioxidant-free dipstick in one embodiment of the invention.
FIG. 5 is an EDS energy spectrum of the antioxidant-loaded dipstick in one embodiment of the invention.
FIG. 6 is a block diagram of a flour-based test strip in one embodiment of the invention.
FIG. 7 is a substrate view of a flour-based test strip in one embodiment of the invention.
FIG. 8 is a graph of a comparative test of flour testing in one embodiment of the present invention.
Description of the main elements
Oxidation resistant protective layer 3
Hand-held terminal 5
The following detailed description will further illustrate the invention in conjunction with the above-described figures.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Example 1
In this embodiment, a preparation method of the antioxidant flour benzoyl peroxide test paper is provided, and reference may be specifically made to fig. 1.
In this embodiment, the method includes the steps of:
the method comprises the following steps: pretreating a test paper substrate, selecting medium-speed qualitative filter paper as the test paper substrate, placing the test paper substrate in 20mL of ethanol, ultrasonically cleaning for three times, and drying for later use;
step two: preparing a color developing agent, namely weighing 3,3,5, 5-tetramethylbenzidine, adding a mixed solution of distilled water and ethanol, adding an aqueous solution of a surfactant after the 3,3,5, 5-tetramethylbenzidine is dissolved, and performing ultrasonic treatment to obtain a color developing solution;
step three: loading a color developing agent, namely soaking the pretreated test paper substrate in color developing solution, taking out the test paper substrate, draining the test paper substrate, and drying the test paper substrate in a constant-temperature vacuum drying oven to obtain test paper with a color developing layer;
step four: preparing an antioxidant solution, namely weighing sodium tungstate and sodium molybdate, adding distilled water, and performing ultrasonic dissolution to obtain the antioxidant solution;
step five: loading an anti-oxidation solution, and dripping the anti-liquefaction solution on the surface of the test paper with the color development layer in a spin coating mode;
step six: drying and cutting to obtain a finished product, cutting the dried filter paper into filter paper strips, and pasting the filter paper strips on a substrate covered with double-sided adhesive tape to prepare a finished test paper product.
By adopting the preparation method of the embodiment, the prepared flour benzoyl peroxide test paper is more stable in air, has a longer quality guarantee period, is not easy to lose efficacy, has an accurate detection result, greatly improves the detection efficiency, and is suitable for the needs of actual life.
FIG. 2 is an image of a test strip after pretreatment according to an embodiment of the present invention. From FIG. 2(a), it can be seen that the test paper has a smooth surface and no other impurities are present. Furthermore, the surface of the test paper is observed by adopting an SEM scanning electron microscope, and the experimental result further shows that the surface of the test paper after pretreatment is smooth, clean and free of impurities.
Example 2
In order to further prepare a color-developing agent solution with an appropriate concentration, in this example, the weight of the color-developing agent 3,3,5, 5-tetramethylbenzidine was weighed to be 0.05 to 0.5g, and the color-developing agent 3,3,5, 5-tetramethylbenzidine was further dissolved in the mixed solution.
Wherein, the chemical structural formula of the 3,3,5, 5-tetramethyl benzidine is as follows:
in this example, the mixed solution is a mixed solution obtained by mixing ethanol and distilled water at a volume ratio of 9:1, and the volume of the mixed solution is 50 mL.
In this embodiment, the surfactant is one or two of cetyltrimethylammonium bromide, cetyltrimethylbenzene sulfonate or sodium dodecyl sulfonate.
The invention takes 3,3,5, 5-tetramethyl benzidine as color developing agent, utilizes self-condensation reaction to detect flour, and has the following reaction principle:
if Benzoyl Peroxide (BPO) is added into the flour, the benzoyl peroxide has strong oxidizing property, and reacts with a color developing agent to generate a blue substance azo compound which can be obviously observed in a test paper. Wherein, the color depth of the test paper is in direct proportion to the concentration of Benzoyl Peroxide (BPO) in the flour.
In this example, the chemical structure of the resulting blue azo compound is as follows:
further, as shown in fig. 3, an SEM scanning electron micrograph of the test paper loaded with the color developer is shown.
Wherein, fig. 3(a) is a scanning electron microscope image of the test paper soaked in the developer solution for 5 minutes, fig. 3(b) is a scanning electron microscope image of the test paper soaked for 10 minutes, and fig. 3c is a scanning electron microscope image of the test paper soaked for 20 minutes.
The results show that the surface of the test paper after soaking and drying is obviously changed, the fibers on the surface of the test paper are gradually weakened, the soaking time is related to the increase of the soaking time and the increase of the amount of the loaded color developing agent, and the soaking time is comprehensively selected to be 10 minutes.
In the embodiment of the invention, whether the additive Benzoyl Peroxide (BPO) exists in the flour can be easily judged based on the color depth of the test paper, the detection process is convenient, and the detection speed is high.
Example 3
In this example, the antioxidant solution was prepared such that the solute sodium tungstate was 0.025 to 0.15g in mass, the solute sodium molybdate was 0.025 to 0.15g in mass, and the volume of distilled water was 50 mL.
When spin coating was performed, the rotation speed of the spin coater was set at 200r/min, and annealing was performed after spin coating at a temperature of 50 ℃.
In this example, to further determine whether the antioxidant is successfully loaded on the surface of the developer, we performed an X-ray spectroscopy (EDS) test on the test paper before and after spin coating, respectively, so as to determine the surface element distribution of the test paper after loading the antioxidant, and the specific test results can be shown in fig. 4 and fig. 5.
Specifically, when the antioxidant is not loaded, the surface of the test paper is a color developing agent, most of the surface of the test paper is organic matter, and C, N and Na elements are selected respectively to determine the element distribution. As can be seen from FIGS. 4(a), (b), and (C), the C element and N element are uniformly distributed on the surface of the test paper, while the Na element is less in content and is hardly distributed.
Further, we performed EDS spectrum test on the test paper obtained by spin coating in this example. As can be seen from FIGS. 5(a), (b), and (C), the elements C and N are still uniformly distributed, while the surface Na element is clearly distributed. Test results show that the antioxidant can be successfully loaded on the surface of the test paper by adopting a spin coating mode.
In the embodiment, the antioxidant is uniformly loaded, so that the contact area between the color developing agent and air can be reduced, the color developing agent is prevented from being oxidized, the quality guarantee period of the flour benzoyl peroxide detection test paper is effectively prolonged, and the service life of the flour benzoyl peroxide detection test paper is effectively prolonged.
Meanwhile, sodium tungstate and sodium molybdate are colorless substances, and the covering of the sodium tungstate and the sodium molybdate on the surface of the color developing agent does not influence the color developing reaction of the color developing agent and interfere the detection effect of the color developing agent.
Example 4
In the present embodiment, there is provided an antioxidant flour benzoyl peroxide test paper, which is manufactured by the method of the above embodiments, and includes a substrate 1, a color development layer 2, and an antioxidant protection layer 3.
Further, the substrate 1 is obtained by medium-speed qualitative filter paper treatment.
The color development layer is obtained by drying a mixed solution of ethanol and distilled water of 3,3,5, 5-tetramethylbenzidine.
The oxidation-resistant protective layer comprises sodium tungstate and sodium molybdate.
The test paper further comprises a bottom plate 4, one side of the bottom plate 4 is a handheld end 5, and the substrate 1 is arranged above the bottom plate 4.
The bottom plate 4 is further provided with a pressing plate 6, and the substrate 1 is arranged between the bottom plate 4 and the pressing plate 6.
Further, the pressing plate 6 is connected with the bottom plate 4 through an adhesive layer 7.
The antioxidant flour benzoyl peroxide test paper provided in the embodiment can reduce the contact between the test paper and the viscose layer 7, prevent the corrosion of the chemical position on the surface of the viscose layer 7 to the test paper, and prolong the quality guarantee period of the test paper.
In order to further verify the protection effect of the antioxidant protection layer on the color development layer, three test paper sheets which are not loaded with the antioxidant and three test paper sheets loaded with the antioxidant are respectively selected for testing.
Firstly, three test paper without antioxidant and three test paper with antioxidant are placed under the same condition and sealed and protected from light for 30 days.
Specific results can be seen in figure 8. In fig. 8, the left 3 pieces are antioxidant flour benzoyl peroxide test paper prepared by the method of the present application, and the right 3 pieces are flour benzoyl peroxide test paper without antioxidant coating.
As can be seen from the figure, 3 pieces of the test paper for detecting the antioxidant-free wheat flour benzoyl peroxide on the right side have failed because the test paper itself undergoes a color reaction due to oxidation. The surfaces of the left 3 pieces of blank test paper are not obviously changed, and the comparison result shows that the benzoyl peroxide test paper has good oxidation resistance.
The first experimental example: test paper determination
A90% ethanol solution (the volume ratio of ethanol to water is 9:1) is used for preparing a mixed color developing solution containing 8.0g/L3,3',5,5' -tetramethylbenzidine and 6.0g/L sodium dodecyl sulfate. Soaking chromatography filter paper in the color development solution for 10 minutes, taking out the filter paper, draining, vacuum-drying at 40 ℃ for 20 minutes, and then dripping 2.0g/L sodium molybdate solution to cover the surface of the filter paper in a spin coating manner. After drying, cutting the filter paper into small strips of 8mm × 100mm by a cutting machine, adhering 5mm wide viscose glue to two sides of one end of a PVC base plate of 65mm × 400mm, placing a detection test paper in the middle, arranging 6mm × 200mm pressing sheets on the upper sides of the viscose glue, covering the pressing sheets on the upper surface of a viscose body, partially covering the pressing sheets on the upper sides of the detection test paper, fixing the detection paper on the base plate by means of the pressing sheets, and finally cutting the detection paper into finished detection test paper strips of 5mm × 65mm again.
Examples of Standard color cards
Ethanol is used as a solvent, 8 benzoyl peroxide standard solutions with different concentrations, such as 0mg/L, 2.5mg/L, 5mg/L, 10mg/L, 20mg/L, 50mg/L, 75mg/L and 100mg/L, are respectively prepared, a disposable pipette is used for sucking the solutions, 1-2 drops of the solutions are dripped into a BPO detection test paper color development area, and after 30 seconds, the test paper shows different gradient color changes. And a color comparison card is manufactured according to the relation between the color development condition and the concentration of the solution, so that the comparison is convenient for users in actual use.
The test paper is placed in a sealed light-proof bag and is stored in an oven at the temperature of 45 ℃ for 37 days, namely, the test paper is stored at the room temperature (20 ℃) for 1 year, the appearance of the test paper is observed every other week, and a stability test and an actual color development condition test are carried out. The color development test method comprises the following steps: preparing 2.5mg/L, 5mg/L, 10mg/L, 20mg/L and 50mg/L benzoyl peroxide standard solutions respectively, taking the standard solutions, respectively dripping the standard solutions into a test paper color development area, observing the color development effect after the color development is completed for 30 seconds, and comparing the color development effect with a matched standard color comparison card respectively to obtain the following data. As the BPO content increased, the color developed by the test paper gradually changed from yellow-green to dark-green.
Table-test paper stability
Therefore, according to the test result, after the BPO test paper is placed in the environment of 45 ℃ for 5 weeks, the color development time is slightly delayed, but the color development effect is good, and according to the shelf life acceleration experiment, the shelf life of the test paper prepared by the method at normal temperature can reach one year.
Second Experimental example sample test
The prepared test paper is used for carrying out a wheat flour sample test and is compared with the result of a colorimetric method. And when the color tone of the sample after color development is consistent with the standard color gradation, taking the color gradation indicating concentration as a measured value, and if the color is between the two color gradations, taking the middle concentration of the two color gradations indicating concentration as the measured value. The colorimetric method is to react BPO with potassium iodide to generate iodine by using the oxidability of BPO, then measure a specific numerical value on an instrument after the color is developed with starch, and finally carry out labeling verification. The test method of the test paper comprises the following steps: weighing 1g of sample in a 5mL sample tube, adding 1mL of absolute ethyl alcohol, carrying out vortex oscillation for 1 minute, standing for layering, and obtaining a supernatant which is a sample solution to be detected after 5 minutes.
Selecting wheat flour of different batches for carrying out sample and sample labeling tests, and simultaneously carrying out comparison tests with a colorimetric method, wherein the results are shown in the following table:
as can be seen from the test results in Table 2, the detection result of the BPO detection test paper conforms to the detection result of the colorimetric method, and the method does not need other instrument accessories, is simple to operate, has reliable results and has higher practical value.
The antioxidant flour benzoyl peroxide test paper provided by the embodiment is stable in the air, is not easy to oxidize, effectively prolongs the service life, and ensures the detection effect of the flour test paper.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned. Furthermore, it will be obvious that the term "comprising" does not exclude other elements or steps.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. The preparation method of the antioxidant flour benzoyl peroxide test paper is characterized by comprising the following steps of:
the method comprises the following steps: pretreating a test paper substrate, selecting rapid qualitative filter paper as the test paper substrate, placing the test paper substrate in 20mL of ethanol, ultrasonically cleaning for three times, and drying for later use;
step two: preparing a color developing agent, namely weighing 3,3,5, 5-tetramethylbenzidine, adding a mixed solution of distilled water and ethanol, adding an aqueous solution of a surfactant after the 3,3,5, 5-tetramethylbenzidine is dissolved, and performing ultrasonic treatment to obtain a color developing solution;
step three: loading a color developing agent, namely soaking the pretreated test paper substrate in color developing solution, taking out the test paper substrate, draining the test paper substrate, and drying the test paper substrate in a constant-temperature vacuum drying oven to obtain test paper with a color developing layer;
step four: preparing an antioxidant solution, namely weighing sodium tungstate and sodium molybdate, adding distilled water, and performing ultrasonic dissolution to obtain the antioxidant solution;
step five: loading an anti-oxidation solution, and dripping the anti-liquefaction solution on the surface of the test paper with the color development layer in a spin coating mode;
step six: drying and cutting to obtain a finished product, cutting the dried filter paper into filter paper strips, and pasting the filter paper strips on a substrate covered with double-sided adhesive tape to prepare a finished test paper product.
2. The method for preparing the anti-oxidation flour benzoyl peroxide test paper as claimed in claim 1, wherein the mass of the 3,3,5, 5-tetramethylbenzidine weighed in the second step is 0.05-0.5g, the ratio of distilled water to ethanol in the mixed solution is 1:9, and the volume of the mixed solution is 50 mL.
3. The method for preparing the antioxidant flour benzoyl peroxide test paper as claimed in claim 2, wherein in the second step, the surfactant is cetyl trimethyl ammonium bromide, cetyl trimethyl sodium benzene sulfonate or sodium dodecyl sulfonate.
4. The method for preparing the antioxidant flour benzoyl peroxide test paper as claimed in claim 1, wherein the mass of sodium tungstate is 0.025-0.15g, the mass of sodium molybdate is 0.025-0.15g, and the volume of distilled water is 50 mL.
5. The method for preparing the antioxidant flour benzoyl peroxide test paper as claimed in claim 1, wherein the rotation speed during the spin coating in the sixth step is 200r/min, and the annealing treatment is performed after the spin coating, wherein the annealing temperature is 50 ℃.
6. An antioxidant flour test strip produced by the method of any one of claims 1 to 5, wherein the test strip comprises:
the substrate is obtained by processing rapid qualitative filter paper;
the color development layer is obtained by drying a mixed solution of ethanol and distilled water of 3,3,5, 5-tetramethylbenzidine;
an oxidation resistant protective layer comprising sodium tungstate and sodium molybdate.
7. The antioxidant flour benzoyl peroxide test paper of claim 6, further comprising:
the portable handheld terminal comprises a bottom plate, wherein a handheld end is arranged on one side of the bottom plate;
the substrate is arranged above the bottom plate;
the base is arranged between the bottom plate and the pressing plate.
8. The test paper for detecting benzoyl peroxide in antioxidant flour according to claim 7, wherein the pressing plate is connected with the bottom plate through an adhesive layer.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113295683A (en) * | 2021-05-24 | 2021-08-24 | 烟台海关技术中心 | Benzoyl peroxide detection method |
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