CN112649274A - Extraction method of furfural compounds - Google Patents
Extraction method of furfural compounds Download PDFInfo
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- CN112649274A CN112649274A CN202011359898.3A CN202011359898A CN112649274A CN 112649274 A CN112649274 A CN 112649274A CN 202011359898 A CN202011359898 A CN 202011359898A CN 112649274 A CN112649274 A CN 112649274A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4077—Concentrating samples by other techniques involving separation of suspended solids
- G01N2001/4094—Concentrating samples by other techniques involving separation of suspended solids using ultrasound
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Abstract
The invention relates to the field of dairy products, in particular to a method for extracting furfural compounds. The invention provides a method for extracting furfural compounds, which comprises the following steps: 1) mixing the dairy product to be extracted with water, carrying out ultrasonic treatment on the mixture, and fully oscillating; 2) adding oxalic acid aqueous solution into the mixture, heating the mixed solution, and cooling; 3) adding trichloroacetic acid aqueous solution into the mixed solution, fully vibrating, centrifuging and carrying out solid-liquid separation; 4) mixing the solid phase substance with trichloroacetic acid aqueous solution, fully vibrating, centrifuging, and carrying out solid-liquid separation; 5) the liquid phases are combined to provide an extract. The extraction method of the furfural compounds provided by the invention can fully extract the furfural compounds in the dairy products.
Description
Technical Field
The invention relates to the field of dairy products, in particular to a method for extracting furfural compounds.
Background
Cheese, condensed milk and special diet food are all common food which is prepared by taking milk as a main raw material, adding some common auxiliary materials and combining different processes. During the hot processing of milk added with different auxiliary materials, with the increase of the heat treatment temperature, physical and chemical reactions such as whey protein denaturation and aggregation, lactose isomerization and degradation, Maillard reaction and the like can occur in sequence, and the reduction of active ingredients (such as alkaline phosphatase, lactoferrin and the like) or the generation of reaction products (such as lactulose, furaldehyde, furfural and the like) can be caused.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention aims to provide a method for extracting furfural compounds, which solves the problems of the prior art.
In order to achieve the above objects and other related objects, the present invention provides a method for extracting furfural compounds, comprising:
1) mixing the dairy product to be extracted with water, carrying out ultrasonic treatment on the mixture, and fully oscillating;
2) adding oxalic acid aqueous solution into the mixture provided in the step 1), heating the mixed solution, and cooling;
3) adding trichloroacetic acid aqueous solution into the mixed solution provided by the step 2), fully oscillating, centrifuging and carrying out solid-liquid separation;
4) mixing the solid phase substance provided by the step 3) with trichloroacetic acid aqueous solution, fully vibrating, centrifuging and carrying out solid-liquid separation;
5) combining the liquid phase provided in step 3) and step 4) to provide an extract.
In some embodiments of the invention, in step 1), the dairy product is selected from one or more of cheese, condensed milk and milk-based special meal food.
In some embodiments of the invention, in step 1), the furfural compound is one or more of hydroxymethyl furfural and furfural.
In some embodiments of the invention, in the step 1), 0.01 to 2.00g of the dairy product to be extracted is added to every 12ml of water, and preferably, 0.04 to 0.06g of the dairy product to be extracted is added to every 12ml of water.
In some embodiments of the invention, in the step 1), the time of the ultrasonic treatment is 25-35 min, and the frequency of the ultrasonic treatment is 95-105 kHZ.
In some embodiments of the invention, in the step 2), the concentration of the oxalic acid aqueous solution is 0.13-0.17 mol/L, and the volume ratio of the mixture to the oxalic acid aqueous solution is 1-4: 1.
in some embodiments of the present invention, in the step 2), the heating temperature of the heating treatment is 95 to 105 ℃, and the heating time is 20 to 30 minutes.
In some embodiments of the present invention, in the step 3), the concentration of the trichloroacetic acid aqueous solution is 35 to 45 w/v%, and the volume ratio of the mixed solution to the trichloroacetic acid aqueous solution is 10: 1 to 4.
In some embodiments of the invention, in the step 3), the centrifugation is performed under the conditions of 4.255G-4.455G for 10-20 minutes.
In some embodiments of the present invention, in the step 4), the concentration of the trichloroacetic acid aqueous solution is 3 to 5 w/v%, and the volume ratio of the mixed solution to the trichloroacetic acid aqueous solution is 10: 1 to 4.
In some embodiments of the present invention, in the step 4), the centrifugation is performed under the conditions of 4.255G-4.455G for 10-20 minutes.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments, and other advantages and effects of the present invention will be apparent to those skilled in the art from the disclosure of the present specification.
The inventor of the invention provides a method for extracting furfural compounds in dairy products through a large amount of practical researches, and the method can fully extract the furfural compounds in the dairy products so as to be convenient for detecting the furfural compounds in the dairy products, thereby completing the invention.
The invention provides a method for extracting furfural compounds, which comprises the following steps:
1) mixing the dairy product to be extracted with water, carrying out ultrasonic treatment on the mixture, and fully oscillating;
2) adding oxalic acid aqueous solution into the mixture provided in the step 1), heating the mixed solution, and cooling;
3) adding trichloroacetic acid aqueous solution into the mixed solution provided by the step 2), fully oscillating, centrifuging and carrying out solid-liquid separation;
4) mixing the solid phase substance provided by the step 3) with trichloroacetic acid aqueous solution, fully vibrating, centrifuging and carrying out solid-liquid separation;
5) combining the liquid phase provided in step 3) and step 4) to provide an extract.
The extraction method of the furfural compound provided by the invention can comprise the following steps: mixing the dairy product to be extracted with water, carrying out ultrasonic treatment on the mixture, and fully shaking.
In the above extraction method, the furfural compound generally refers to one or more of hydroxymethyl furfural (HMF, CAS NO.67-47-0) and furfural (F, CAS NO. 98-01-1).
In the extraction method, the dairy product to be extracted is generally a food prepared by taking cow milk as a main raw material, further adding available auxiliary materials in other foods and combining different processes. For example, the dairy product to be extracted may be a combination of one or more of a processed cheese according to GB25192, a condensed milk according to GB13102, a milk-based specialty meal according to GB22570, etc. During the preparation process, certain amount of hydroxymethyl furfural and furfural are generated in the preparation process. For example, the content of hydroxymethylfurfural in the dairy product to be extracted can be generally less than or equal to 1 μ g/100g, 1 to 5 μ g/100g, 5 to 10 μ g/100g, 10 to 20 μ g/100g, 20 to 40 μ g/100g, 40 to 60 μ g/100g, 60 to 100 μ g/100g, 100 to 500 μ g/100g, 500 to 1000 μ g/100g, 1000 to 3000 μ g/100g, 3000 to 5000 μ g/100g, 5000 to 10000 μ g/100g, 10000 to 20000 μ g/100g, 20000 to 40000 μ g/100g, 40000 to 60000 μ g/100g, 60000 to 100000 μ g/100g, or higher, the content of furfural in the dairy product to be extracted can be generally less than or equal to 1 μ g/100g, 1 to 5 μ g/100g, 5 to 10 μ g/100g, 10 to 20 μ g/100g, or higher, 20-40 μ g/100g, 40-60 μ g/100g, 60-100 μ g/100g, 100-200 μ g/100g, 200-300 μ g/100g, 300-500 μ g/100g, 500-1000 μ g/100g, 1000-3000 μ g/100g, 3000-5000 μ g/100g, 5000-10000 μ g/100g, or more.
In the above extraction method, it is usually necessary to mix an appropriate amount of dairy product to be extracted with water to form a mixture with an appropriate concentration, so as to further improve the extraction efficiency of furfural compounds. In one embodiment of the invention, 0.01-2.00 g, 0.01-0.03 g, 0.03-0.05 g, 0.05-0.1 g, 0.1-0.2 g, 0.2-0.4 g, 0.4-0.6 g, 0.6-1.00 g, 1.00-1.50 g, or 1.50-2.00 g of dairy product to be extracted can be added into each 12ml of water, preferably, 0.04-0.06 g of dairy product to be extracted can be added into each 12ml of water.
Among the above extraction methods, the ultrasonic treatment generally refers to a treatment method in which a substance is uniformly dispersed in a solution system by cavitation of ultrasonic waves in a liquid. The sonication is generally required to be of sufficient power and duration to allow sufficient dispersion of the dairy product to be extracted in the water. In an embodiment of the present invention, the time of the ultrasonic treatment can be 25-35 min, 25-27 min, 27-29 min, 29-31 min, 31-33 min, or 33-35 min.
In the above extraction method, sufficient shaking generally refers to a treatment method in which the sample is sufficiently shaken so that the components in the sample are sufficiently mixed. After sonication, the mixture usually needs to be shaken well to further ensure a homogeneous distribution of the solution system.
The extraction method of the furfural compound provided by the invention can also comprise the following steps: adding oxalic acid aqueous solution into the mixture provided by the step 1), heating the mixed solution, and cooling.
In the above extraction method, the aqueous oxalic acid solution used generally needs to have a suitable concentration and a suitable ratio to the mixture, so as to ensure the liberation of the molecules of the bonded furfural-like compound. In an embodiment of the present invention, the concentration of the oxalic acid aqueous solution may be 0.13-0.17 mol/L, 0.13-0.14 mol/L, 0.14-0.15 mol/L, 0.15-0.16 mol/L, or 0.16-0.17 mol/L. In another embodiment of the invention, the volume ratio of the mixture to the oxalic acid aqueous solution is 1-4: 1. 1-1.5: 1. 1.5-2: 1. 2-3: 1. or 3-4: 1.
in the above extraction method, the mixture is usually heated after adding the oxalic acid aqueous solution, thereby ensuring the dissociation of the molecules of the bonded furfural compounds. In an embodiment of the present invention, the heating temperature of the heating treatment may be 95 to 105 ℃, 95 to 97 ℃, 97 to 99 ℃, 99 to 101 ℃, 101 to 103 ℃, or 103 to 105 ℃, and the heating time may be 20 to 30 minutes, 20 to 22 minutes, 22 to 24 minutes, 24 to 26 minutes, 26 to 28 minutes, or 28 to 30 minutes.
The extraction method of the furfural compound provided by the invention can also comprise the following steps: adding trichloroacetic acid aqueous solution into the mixed solution provided by the step 2), fully oscillating, centrifuging and carrying out solid-liquid separation.
In the above extraction method, the trichloroacetic acid aqueous solution used generally needs to have a proper concentration and a proper ratio with the mixed solution, so as to ensure effective removal of the protein. In one embodiment of the present invention, the concentration of the trichloroacetic acid aqueous solution may be 35-45 w/v%, 35-37 w/v%, 37-39 w/v%, 39-41 w/v%, 41-43 w/v%, or 43-45 w/v%. In another embodiment of the present invention, the volume ratio of the mixed solution to the trichloroacetic acid aqueous solution may be 10: 1-4, 10: 1-2, 10: 2-3, or 10: 3 to 4. Adding trichloroacetic acid aqueous solution into the mixed solution, and then, usually, fully shaking is needed, so that the substances in the solution system are fully contacted.
In the extraction method, the mixed solution is mixed with trichloroacetic acid aqueous solution and can be subjected to solid-liquid separation after being sufficiently shaken, so as to provide a solid phase substance and a liquid phase substance. In an embodiment of the present invention, the precipitate provided after centrifugation is a solid phase, the supernatant is a liquid phase, and the centrifugation condition may be 4.255G-4.455G, 4.255G-4.355G, or 4.355G-4.455G, 10-20 minutes, 10-15 minutes, or 15-20 minutes.
The extraction method of the furfural compound provided by the invention can also comprise the following steps: mixing the solid phase substance provided by the step 3) with trichloroacetic acid aqueous solution, fully shaking, centrifuging and carrying out solid-liquid separation.
In the above extraction method, the aqueous trichloroacetic acid solution used generally needs to have a suitable concentration and a suitable ratio to the solid phase, so as to ensure efficient removal of the proteins. In an embodiment of the present invention, the concentration of the trichloroacetic acid aqueous solution may be 3-5 w/v%, 3-3.5 w/v%, 3.5-4 w/v%, 4-4.5 w/v%, or 4.5-5 w/v%. In another embodiment of the present invention, the amount of the trichloroacetic acid aqueous solution used in step 4) may refer to the amount of the mixed solution in step 3), and the volume ratio of the mixed solution to the trichloroacetic acid aqueous solution may be 10: 1-4, 10: 1-2, 10: 2-3, or 10: 3 to 4. The solid phase and the trichloroacetic acid aqueous solution are mixed and then are usually required to be fully vibrated so as to ensure that the substances in the solution system are fully contacted.
In the extraction method, after the solid phase substance is mixed with the trichloroacetic acid aqueous solution and sufficiently shaken, solid-liquid separation can be carried out to provide the solid phase substance and the liquid phase substance. In an embodiment of the present invention, the precipitate provided after centrifugation is a solid phase, the supernatant is a liquid phase, and the centrifugation condition may be 4.255G-4.455G, 4.255G-4.355G, or 4.355G-4.455G, 10-20 minutes, 10-15 minutes, or 15-20 minutes.
In the above extraction method, step 4) may be repeated for a plurality of times, that is, the solid phase substance provided in step 4) may be mixed with the trichloroacetic acid aqueous solution again, sufficiently shaken, centrifuged, and subjected to solid-liquid separation to provide a liquid phase substance. Repeating the step 4) for many times can more fully extract the furfural compounds in the solid phase.
The extraction method of the furfural compound provided by the invention can also comprise the following steps: combining the liquid phase provided in step 3) and step 4) to provide an extract.
In the above extraction method, the combined extract is the extract of furfural compounds, and the extract can be further diluted by adding a proper amount of trichloroacetic acid aqueous solution for subsequent detection.
The extraction method of the furfural compounds provided by the invention can fully extract the furfural compounds in the dairy products, and related experiments can generally prove that the extraction method has good standard recovery rate, and samples obtained by extraction have high accuracy and good industrialization prospect.
The invention of the present application is further illustrated by the following examples, which are not intended to limit the scope of the present application.
Example 1
The method comprises the steps of respectively selecting three sample weighing amounts of 0.05g, 0.10g and 0.50g for different cheese samples, adding 12mL of water, 100Khz, carrying out ultrasonic treatment for 30min, then shaking for 20min (150 rpm of a vibrator, the same below), adding 5mL of 0.15mol/L oxalic acid prepared on the same day, heating in a water bath at 100 ℃ for 25 min, and cooling to room temperature. Adding 5mL of 40% (w/v) trichloroacetic acid solution, shaking for 10 minutes, and centrifuging for 15 minutes at 4.355G; pouring the supernatant into a 25mL volumetric flask, adding 5mL 4% (w/v) trichloroacetic acid solution into the residual solid, shaking for 10 minutes, and centrifuging for 15 minutes at 4.355G; the supernatant is combined, and 4% (w/v) trichloroacetic acid solution is added to the mixture to be constant volume to the scale. The content of HMF and F of cheese with different weighing amounts is detected by HPLC according to the existing method (a rapid detection method of furfural compounds in dairy products, application number: 201811562740.9), and the result is shown in Table 1:
TABLE 1
Selecting the four cheeses as experimental objects, carrying out a recovery rate experiment, selecting 0.05g of sample weighing, adding 12mL of water into the four cheeses, adding 1mL of standard substance mixed solution (wherein the concentration of HMF is 20 mu g/mL, the content of F is 1 mu g/mL, the concentration of FMC is 20 mu g/mL, and the content of MF is 20 mu g/mL), 100Khz, carrying out ultrasonic oscillation for 20min after 30min, adding 5mL of 0.15mol/L of oxalic acid prepared on the same day, heating in a water bath at 100 ℃ for 25 min, and cooling to room temperature. Adding 5mL of 40% (w/v) trichloroacetic acid solution, shaking for 10 minutes, and centrifuging for 15 minutes at 4.355G; pouring the supernatant into a 25mL volumetric flask, adding 5mL of 4% (w/v) trichloroacetic acid solution into the residual solid, shaking for 10 minutes, and centrifuging for 15 minutes at 4.355G; the supernatant is combined, and 4% (w/v) trichloroacetic acid solution is added to the mixture to be constant volume to the scale. According to the existing method (a rapid detection method of furfural compounds in dairy products, application number: 201811562740.9), the contents of HMF and F in cheese with different weighing amounts are detected by HPLC, and the recovery rate calculation formula is as follows:
the recovery rate of spiked sample (spiked sample measurement value-sample measurement value) ÷ spiked amount × 100%.
When the weight is 0.05g, the recovery rate of the standard addition is 95-105%, and the RSD range is 0.20-2.00%. The method is proved to have good recovery rate and high accuracy, and can be used as an experimental method for researching the furfural content in cheese.
TABLE 2
Example 2
Aiming at two different condensed milk samples, seven sample weighing amounts of 0.02g, 0.05g, 0.10g, 0.25g, 0.50g, 1.00g and 2.00g are respectively selected, the pretreatment method comprises the steps of adding 12mL of water, 100Khz, shaking for 20min after 30min of ultrasonic treatment, adding 5mL of 0.15mol/L of oxalic acid which is prepared on the same day, heating in a water bath at 100 ℃ for 25 min, and cooling to room temperature. Adding 5mL of 40% (w/v) trichloroacetic acid solution, shaking for 10 minutes, and centrifuging for 15 minutes at 4.355G; pouring the supernatant into a 25mL volumetric flask, adding 5mL of 4% (w/v) trichloroacetic acid solution into the residual solid, shaking for 10 minutes, and centrifuging for 15 minutes at 4.355G; the supernatant is combined, and 4% (w/v) trichloroacetic acid solution is added to the mixture to be constant volume to the scale. According to the existing method (a rapid detection method of furfural compounds in dairy products, application number: 201811562740.9), contents of HMF and F in condensed milk with different sample weighing amounts are detected by HPLC, and the results are shown in Table 3:
TABLE 3
Selecting the two condensed milks as experimental objects, carrying out a recovery rate experiment, selecting 0.05g of sample weighing amount, adding 12mL of water into the pre-treatment method, adding 1mL of standard substance mixed solution (wherein the concentration of HMF is 20 mu g/mL, the content of F is 1 mu g/mL, the concentration of FMC is 20 mu g/mL, and the content of MF is 20 mu g/mL), 100Khz, shaking for 20min after 30min of ultrasonic treatment, adding 5mL of 0.15mol/L of oxalic acid prepared on the same day, heating in a 100 ℃ water bath for 25 min, and cooling to room temperature. Adding 5mL of 40% (w/v) trichloroacetic acid solution, shaking for 10 minutes, and centrifuging for 15 minutes at 4.355G; pouring the supernatant into a 25mL volumetric flask, adding 5mL of 4% (w/v) trichloroacetic acid solution into the residual solid, shaking for 10 minutes, and centrifuging for 15 minutes at 4.355G; the supernatant is combined, and 4% (w/v) trichloroacetic acid solution is added to the mixture to be constant volume to the scale. The content of HMF and F in cheese with different sample weights is detected by HPLC according to the existing method (a rapid detection method of furfural compounds in dairy products, application number: 201811562740.9), and the standard recovery rate is calculated, and the result is shown in Table 4. When the weight is 0.05g, the recovery rate of the standard addition is 95-105%, and the RSD range is 0.50-4.00%. The method is proved to have good recovery rate and high accuracy, and can be used as an experimental method for researching the furfural content in condensed milk.
TABLE 4
Example 3
Aiming at two different milk-based special meal samples, six sample amounts of 0.02g, 0.05g, 0.10g, 0.25g, 0.50g and 2.25g are respectively selected and weighed, the pretreatment method comprises the steps of adding 12mL of water, 100Khz, shaking for 20min after ultrasonic treatment for 30min, adding 5mL0.15mol/L of oxalic acid which is prepared on the same day, heating in a water bath at 100 ℃ for 25 min, and cooling to room temperature. Adding 5mL of 40% (w/v) trichloroacetic acid solution, shaking for 10 minutes, and centrifuging for 15 minutes at 4.355G; pouring the supernatant into a 25mL volumetric flask, adding 5mL of 4% (w/v) trichloroacetic acid solution into the residual solid, shaking for 10 minutes, and centrifuging for 15 minutes at 4.355G; the supernatant is combined, and 4% (w/v) trichloroacetic acid solution is added to the mixture to be constant volume to the scale. According to the existing method (a rapid detection method of furfural compounds in dairy products, application number: 201811562740.9), the contents of HMF and F in condensed milk with different sample weighing amounts are detected by HPLC, and the results are shown in Table 5:
TABLE 5
Selecting the two milk-based special dietary foods as experimental objects, carrying out a recovery rate experiment, selecting 0.05g of sample weighing amount, adding 12mL of water into a pretreatment method, adding 1mL of standard substance mixed solution (wherein the concentration of HMF is 20 mu g/mL, the content of F is 1 mu g/mL, the concentration of FMC is 20 mu g/mL, and the content of MF is 20 mu g/mL)100Khz, shaking for 20min after ultrasonic treatment for 30min, adding 5mL of 0.15mol/L oxalic acid prepared on the same day, heating in a water bath at 100 ℃ for 25 min, and cooling to room temperature. Adding 5mL of 40% (w/v) trichloroacetic acid solution, shaking for 10 minutes, and centrifuging for 15 minutes at 4.355G; pouring the supernatant into a 25mL volumetric flask, adding 5mL of 4% (w/v) trichloroacetic acid solution into the residual solid, shaking for 10 minutes, and centrifuging for 15 minutes at 4.355G; the supernatant is combined, and 4% (w/v) trichloroacetic acid solution is added to the mixture to be constant volume to the scale. The content of HMF and F in cheese with different sample weights is detected by HPLC according to the existing method (a rapid detection method of furfural compounds in dairy products, application number: 201811562740.9), and the standard recovery rate is calculated, and the result is shown in Table 6. When the weight is 0.05g, the recovery rate of the standard addition is between 85 and 105 percent, and the RSD range is 0.50 to 6.00 percent. The method is proved to have good recovery rate and high accuracy, and can be used as an experimental method for researching the furfural content in milk-based special meal food.
TABLE 6
In conclusion, the present invention effectively overcomes various disadvantages of the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. A method for extracting furfural compounds comprises the following steps:
1) mixing the dairy product to be extracted with water, carrying out ultrasonic treatment on the mixture, and fully oscillating;
2) adding oxalic acid aqueous solution into the mixture provided in the step 1), heating the mixed solution, and cooling;
3) adding trichloroacetic acid aqueous solution into the mixed solution provided by the step 2), fully oscillating, centrifuging and carrying out solid-liquid separation;
4) mixing the solid phase substance provided by the step 3) with trichloroacetic acid aqueous solution, fully vibrating, centrifuging and carrying out solid-liquid separation;
5) combining the liquid phase provided in step 3) and step 4) to provide an extract.
2. The method for extracting furfural compounds as claimed in claim 1, wherein in the step 1), the dairy product is selected from one or more of cheese, condensed milk and milk-based special meal food;
and/or in the step 1), the furfural compound is one or more of hydroxymethyl furfural and furfural.
3. The method for extracting furfural compounds according to claim 1, wherein in the step 1), 0.01-2.00 g of dairy product to be extracted is added into each 12ml of water, and preferably, 0.04-0.06 g of dairy product to be extracted is added into each 12ml of water.
4. The extraction method of furfural compounds according to claim 1, wherein in the step 1), the time of ultrasonic treatment is 25-35 min, and the frequency of ultrasonic treatment is 95-105 kHZ.
5. The extraction method of furfural compounds according to claim 1, wherein in the step 2), the concentration of the oxalic acid aqueous solution is 0.13-0.17 mol/L, and the volume ratio of the mixture to the oxalic acid aqueous solution is 1-4: 1.
6. the method for extracting furfural compounds according to claim 1, wherein in the step 2), the heating temperature of the heating treatment is 95-105 ℃ and the heating time is 20-30 minutes.
7. The method for extracting furfural compounds according to claim 1, wherein in the step 3), the concentration of the trichloroacetic acid aqueous solution is 35-45 w/v%, and the volume ratio of the mixed solution to the trichloroacetic acid aqueous solution is 10: 1 to 4.
8. The method for extracting furfural compounds according to claim 1, wherein in the step 3), the centrifugation is performed under the conditions of 4.255G-4.455G for 10-20 minutes.
9. The method for extracting furfural compounds according to claim 1, wherein in the step 4), the concentration of the trichloroacetic acid aqueous solution is 3-5 w/v%, and the volume ratio of the mixed solution to the trichloroacetic acid aqueous solution is 10: 1 to 4.
10. The method for extracting furfural compounds according to claim 1, wherein in the step 4), the centrifugation is performed under the conditions of 4.255G-4.455G for 10-20 minutes.
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| US4514503A (en) * | 1982-09-01 | 1985-04-30 | Morton Norwich Products | Reagent and process for detecting furfural in petroleum products |
| CN109580820A (en) * | 2018-12-20 | 2019-04-05 | 光明乳业股份有限公司 | The rapid detection method of Furnan products in a kind of dairy products |
| CN111024906A (en) * | 2019-12-26 | 2020-04-17 | 光明乳业股份有限公司 | Method for rapidly evaluating content of furfural substances in solid dairy product based on storage temperature and humidity of solid dairy product |
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