CN112986437A - Purification detection method for furfural compounds in coffee dairy products - Google Patents
Purification detection method for furfural compounds in coffee dairy products Download PDFInfo
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Abstract
The invention discloses a method for purifying and detecting furfural compounds in coffee dairy products, which comprises the following steps: adding oxalic acid solution into a coffee dairy product sample, heating in a water bath, and cooling to room temperature; adding trichloroacetic acid solution A, shaking and mixing, centrifuging, taking supernatant, adding filter residue into trichloroacetic acid solution B, shaking and mixing, and centrifuging; mixing the supernatants, adding trichloroacetic acid solution B to desired volume; adding active carbon into the supernatant with constant volume, heating in water bath after shaking, and cooling to room temperature; and (4) enabling the sample solution to pass through a nylon filter membrane, and carrying out sample injection analysis by using a high performance liquid chromatograph. The method integrates the advantages of liquid chromatogram and activated carbon, and the activated carbon is added into a pre-treatment constant volume system and then heated in a water bath, so that the conditions of baseline drift, more impurity peaks and the like of the original chromatogram of the coffee dairy product are greatly improved; and simultaneously, the effective detection of the furfural compounds is ensured.
Description
Technical Field
The invention relates to the technical field of compound detection, in particular to a purification detection method of furfural compounds in coffee dairy products.
Background
After the reducing sugar and protein in the food are subjected to a heat treatment process, a non-enzymatic browning reaction, namely a Maillard reaction, often occurs, and different potential hazardous substances are generated at the early stage, the middle stage and the later stage of the reaction. Furfural compounds represented by 5-hydroxymethylfurfural (5-HMF), furfural (F), furylmethyl ketone (FMC) and Methylfurfural (MF) are products of the progress stage of maillard reaction, and have different content distributions in various foods such as honey, coffee, dairy products, and the like. The european food safety commission recommends that the daily intake limit of Hydroxymethylfurfural (HMF) per person is 1.6mg, and that a small amount of furfural compounds have a function of flavoring and toning foods, but excessive intake of furfural compounds is also reported to have a risk of damaging organs such as the heart and inducing chronic diseases such as diabetes.
The coffee dairy product is rich in nutrition, on one hand, milk is known as 'white blood', the milk is rich in abundant nutrient elements such as lactoprotein, lactose, high-quality fat and the like, and the addition of coffee further supplements nutrient substances such as vitamin B, free fatty acid, caffeine, tannic acid and the like; on the other hand, the coffee dairy product is taken as a dairy product with unique flavor and mellow taste, meets the taste requirements of consumers along with the change of the living habits and the improvement of the consumption level of the public, and is more and more popular at home and abroad; however, related researches also suggest that the coffee milk product contains coffee and milk components more complicated, and as the coffee and the milk generate furfural compounds mainly comprising 4 types of 5-HMF, F, FMC and F in the respective processing processes, and the furfural compounds in the coffee are relatively high, the furfural compounds in the coffee milk product need to be detected so as to ensure the nutrition, health and safety of national diet.
The related research of furfural compounds mainly focuses on aspects such as development of liquid chromatography and liquid chromatography-mass spectrometry combined rapid detection methods of furfural compounds represented by HMF and F at present, the detection methods mainly focus on 3 types, namely a liquid chromatography-tandem ultraviolet detector method, a liquid chromatography-tandem fluorescence detection method and a liquid chromatography-tandem mass spectrometry detection method, wherein the liquid chromatography-tandem ultraviolet detector method is widely applied due to simple operation and low cost, and the invention selects the liquid chromatography-tandem ultraviolet detector method (based on the furfural compound HPLC rapid detection method developed by our company, the patent application number is 201811562740.9); on the basis, aiming at the problem that the ingredients of the coffee dairy product are more complex, the detection of the furfural compounds has a plurality of interference factors, the chromatogram has more peaks and part of wave bands have base line drift. Therefore, a purification detection method for furfural compounds in coffee dairy products needs to be developed to solve the problems that chromatographic peaks deviate from a baseline and miscellaneous peaks are old and cannot be effectively detected due to complex components of the coffee dairy products.
Disclosure of Invention
The invention aims to provide a method for purifying and detecting furfural compounds in coffee dairy products, which is characterized in that activated carbon with a proper proportion is added, the purification time and temperature of proper chromatographic peaks are explored, and the problems that the chromatographic peaks deviate from a base line and the chromatographic peaks are impure and old due to the complex components of the coffee dairy products are solved on the premise of ensuring the effective detection of the furfural compounds.
The invention is realized by the following technical scheme in order to achieve the purpose:
a purification detection method for furfural compounds in coffee dairy products comprises the following steps:
(1) adding oxalic acid solution into a coffee dairy product sample, heating in a water bath, and cooling to room temperature;
(2) adding trichloroacetic acid solution A, shaking and mixing, centrifuging at the rotating speed of 4-5g, taking supernatant, adding filter residue into trichloroacetic acid solution B, shaking and mixing, and centrifuging at the rotating speed of 4-5 g; mixing the supernatants, adding trichloroacetic acid solution B to desired volume;
(3) adding activated carbon into the supernatant obtained in the step (2) with constant volume, heating in a water bath after shaking, and cooling to room temperature;
(4) and (3) filtering the sample solution obtained in the step (3) through a nylon filter membrane, performing sample injection analysis by using a high performance liquid chromatograph, selecting a reversed phase C18 chromatographic column with the filler particle size of 2.7-3.5 mu m, wherein the mobile phase is water and acetonitrile, the flow rate is 0.5-0.7mL/min, the column temperature is 28-32 ℃, and detecting the content of the furfural compounds after chromatographic analysis.
Further, in the step (1), the volume of the oxalic acid solution added to each g of the sample solution is 0.3-0.5mL, and the concentration of the oxalic acid solution is 0.12-0.16 mol/L.
Further, in the step (1), the water bath heating temperature is 90-120 ℃, and the time is 20-30 min.
Further, in the step (2), the concentration of the trichloroacetic acid solution A is 35-45g/mL, and the concentration of the trichloroacetic acid solution B is 3.5-4.5 g/mL.
Further, in the step (2), the rotation speed of the two times of centrifugation is 4.355 g; and/or the time for two centrifugations is 12-18 min.
Further, in the step (3), the adding amount of the activated carbon is 1% -3%, and the activated carbon accounts for the mass/volume percentage of the constant volume supernatant obtained in the step (2).
Further, in the step (3), the oscillation time is 7-13 min.
Further, the water bath heating temperature is 75-80 ℃, and the heating time is 25-35 min.
Further, in the step (4), the aperture of the nylon filter membrane is 0.45 μm.
Further, in the step (3), the length of the chromatographic column is 12-18cm, the inner diameter is 2.8-3.2mm, and the film thickness is 2.5-3.5 μm.
Further, in the step (4), the sample injection amount is 4.5-5.5 mu L, and the temperature of a sample injection disc is 3.8-4.2 ℃; the ultraviolet detection wavelength is 270-290 nm.
Compared with the prior art, the invention provides an optimization method for detecting furfural compounds in coffee dairy products, integrates the advantages of liquid chromatogram and activated carbon, selectively adds the activated carbon into a pre-treatment constant volume system, and then heats in a water bath; the conditions of baseline drift, more miscellaneous peaks and the like of the original chromatogram of the coffee dairy product are greatly improved; and simultaneously, the effective detection of the furfural compounds is ensured. The method is simple to operate, has low cost, realizes efficient and rapid impurity removal, and optimizes the detection method of the coffee dairy product.
Drawings
FIG. 1 is a comparison of the chromatogram of a coffee milk product before and after treatment in example 1;
FIG. 2 is a comparison of the chromatogram of a coffee milk product before and after treatment in example 2;
FIG. 3 is a comparison of the chromatogram of a coffee milk product before and after treatment in example 3;
figure 4 is a comparison of the color spectrum of a coffee dairy product before and after treatment in example 4.
Detailed Description
In order to more clearly illustrate the technical solution of the present invention, the technical solution of the present invention will be further described with reference to specific embodiments.
In a specific embodiment, a method for purifying and detecting furfural compounds in coffee dairy products is provided, which comprises the following steps:
(1) free furfural: adding oxalic acid solution into a coffee dairy product sample, heating in a water bath, and cooling to room temperature;
(2) protein removal: adding trichloroacetic acid solution A, shaking and mixing, centrifuging at the rotating speed of 4-5g, taking supernatant, adding filter residue into trichloroacetic acid solution B, shaking and mixing, and centrifuging at the rotating speed of 4-5 g; mixing the supernatants, adding trichloroacetic acid solution B to desired volume; the centrifugal rotation speed is preferably 4.355 g.
(3) Removing impurities: adding activated carbon into the supernatant obtained in the step (2) with constant volume, heating in a water bath after shaking, and cooling to room temperature;
(4) and (3) filtering the sample solution obtained in the step (3) through a nylon filter membrane, performing sample injection analysis by using a high performance liquid chromatograph, selecting a reversed phase C18 chromatographic column with the filler particle size of 2.7-3.5 mu m, wherein the mobile phase is water and acetonitrile, the flow rate is 0.5-0.7mL/min, the column temperature is 28-32 ℃, and detecting the content of the furfural compounds after chromatographic analysis. Preferably, a reversed phase C18 chromatographic column with a filler particle size of 3 μm is selected, the mobile phase is water and acetonitrile, the flow rate is 0.6mL/min, the column temperature is 30 deg.C
According to the invention, oxalic acid free combined furfural is used, then trichloroacetic acid solution is selected to remove protein, the obtained solution is added with active carbon for treatment, and the obtained treatment solution enters a liquid chromatograph for analysis. The scheme integrates the advantages of liquid chromatogram and activated carbon, the activated carbon is added into a pre-treatment constant volume system for water bath treatment, and an optimization method is provided for the detection of furfural compounds in coffee dairy products; the conditions of baseline drift, more miscellaneous peaks and the like of the original chromatogram of the coffee dairy product are greatly improved; and simultaneously, the effective detection of the furfural compounds is ensured.
In the specific embodiment of the invention, in the step (1), the volume of the oxalic acid solution added to each g of the sample solution is 0.3-0.5mL, and the concentration of the oxalic acid solution is 0.12-0.16 mol/L. And selecting the prepared oxalic acid solution, wherein the oxalic acid solution can reduce the pH value of a sample, destroy the chemical bond of the combined furfural under the heating condition and dissociate the furfural compound. Preferably, the volume of the oxalic acid solution added to each g of sample solution is 0.4mL, and the concentration of the oxalic acid solution is 0.15mol/L.
In the step (1) in the specific embodiment of the invention, the water bath heating temperature is 90-100 ℃ and the time is 20-30 min. Preferably, the temperature of the water bath heating is 100 ℃ and the time is 25 min.
In the specific embodiment of the invention, in the step (2), the concentration of the trichloroacetic acid solution A is 35 to 45g/mL, and the concentration of the trichloroacetic acid solution B is 3.5 to 4.5 g/mL. Under acidic conditions, trichloroacetic acid can form insoluble salts with proteins, thereby precipitating the proteins in the dairy product. Preferably, the concentration of the trichloroacetic acid solution A is 40g/mL, and the concentration of the trichloroacetic acid solution B is 4 g/mL.
In the specific embodiment of the invention, in the step (2), the rotation speed of both the centrifuges is 4.355 g; and/or, the time of both centrifugations is 12-18min, preferably 15 min.
In the specific embodiment of the invention, in the step (3), the addition amount of the activated carbon is 1% -3%, preferably 2%, and the percentage of the activated carbon is the mass/volume percentage of the constant volume supernatant obtained in the step (2). In example 1 and example 2, activated carbon a and activated carbon B having different adsorbability were used, respectively, and the adsorbability of activated carbon a was higher than that of activated carbon B.
In the specific embodiment of the present invention, in the step (3), the oscillation time is 7-13 min; the water bath heating temperature is 75-80 deg.C, and the heating time is 25-35 min.
In the specific embodiment of the present invention, in the step (4), the pore size of the nylon filter membrane is 0.45 μm.
In the specific embodiment of the present invention, in the step (3), the length of the column is 12 to 18cm, the inner diameter is 2.8 to 3.2mm, and the film thickness is 2.5 to 3.5. mu.m.
In the specific embodiment of the invention, in the step (4), the sample injection amount is 4.5-5.5 mu L, and the temperature of a sample injection disc is 3.8-4.2 ℃; the ultraviolet detection wavelength is 270-290 nm.
The technical effects of the invention can be realized within the scope of the above embodiments, and the specific effects are not greatly different. The present invention will be described in detail with reference to the accompanying drawings and examples. The invention will be better understood from the following examples.
Example 1
The purification detection method of the furfural compounds in the low-temperature coffee prepared milk comprises the following steps:
(1) weighing 15g of low-temperature coffee prepared milk sample, adding the prepared 5mL oxalic acid solution with the concentration of 0.15mol/L, heating in a water bath at 100 ℃ for 25 minutes, and cooling to room temperature;
(2) adding 3mL of trichloroacetic acid solution with the concentration of 40g/mL into the mixed solution obtained in the step (1), shaking for 10 minutes, centrifuging for 15 minutes at 4.355g, pouring the supernatant into a 25mL volumetric flask, adding 5mL of trichloroacetic acid solution with the concentration of 4g/mL into the filter residue, shaking for 10 minutes, and centrifuging for 15 minutes at 4.355 g; mixing the supernatants, adding trichloroacetic acid solution with concentration of 4g/mL to fix volume to the middle scale;
(3) adding 0.5g of activated carbon A into the supernatant with constant volume obtained in the step (2), shaking for 10 minutes, heating in a water bath at 78 ℃ for 30 minutes, and cooling to room temperature;
(4) and (3) enabling the sample solution obtained in the step (3) to pass through a 0.45-micrometer nylon filter membrane, performing sample injection analysis by using a high performance liquid chromatograph, and selecting a reversed-phase C18 chromatographic column with the filler particle size of 3 micrometers, wherein the chromatographic column comprises the following components: waters Atlantis T3(3.0 mm. times.15 cm, 3 μm); mobile phase: the mobile phase A is water, and the mobile phase B is acetonitrile; gradient elution: 0-10.0min, 5% B-95% B, 10.0-12.0min, 95% B-95% B, 12.0-12.1min, 95% B-5% B, 12.1-20.0min, 5% B-5% B; the flow rate is 0.6 mL/min; temperature of the column: 30 ℃; sample introduction amount: 5 mu L of the solution; temperature of a sample injection tray: 4 ℃; ultraviolet detection wavelength: 280 nm.
Example 1 the chromatogram of the assay results is shown in fig. 1, in which 1: 5-Hydroxymethylfurfural (HMF); 2: furfural (F); 3: 2-Furanylmethyl ketone (FMC); 4: 5-Methylfurfural (MF); 5: the original sample interferes with the stray peaks. The test compound pairs before and after treatment are shown in table 1:
TABLE 1
| HMF(ug/100g) | F(ug/100g) | MFC(ug/100g) | MF(ug/100g) | |
| Before treatment | 2280.32 | 306.50 | 81.65 | 127.93 |
| After treatment | 2049.48 | 167.21 | 15.05 | 10.78 |
Example 2
The purification detection method of the furfural compounds in the low-temperature coffee prepared milk comprises the following steps:
(1) weighing 15g of low-temperature coffee prepared milk sample, adding the prepared 5mL oxalic acid solution with the concentration of 0.15mol/L, heating in water bath at 110 ℃ for 25 minutes, and cooling to room temperature;
(2) adding 3mL of trichloroacetic acid solution with the concentration of 42g/mL into the mixed solution obtained in the step (1), shaking for 10 minutes, centrifuging for 15 minutes at 4.355g, pouring the supernatant into a 25mL volumetric flask, adding 5mL of trichloroacetic acid solution with the concentration of 4g/mL into the filter residue, shaking for 10 minutes, and centrifuging for 15 minutes at 4.355 g; mixing the supernatants, adding trichloroacetic acid solution with concentration of 4g/mL to fix volume to the middle scale;
(3) adding 0.5g of activated carbon B into the supernatant with constant volume obtained in the step (2), shaking for 10 minutes, heating in a water bath at 78 ℃ for 30 minutes, and cooling to room temperature;
(4) and (3) enabling the sample solution obtained in the step (3) to pass through a 0.45-micrometer nylon filter membrane, performing sample injection analysis by using a high performance liquid chromatograph, and selecting a reversed-phase C18 chromatographic column with the filler particle size of 3 micrometers, wherein the chromatographic column comprises the following components: waters Atlantis T3(3.0 mm. times.15 cm, 3 μm); mobile phase: the mobile phase A is water, and the mobile phase B is acetonitrile; gradient elution: 0-10.0min, 5% B-95% B, 10.0-12.0min, 95% B-95% B, 12.0-12.1min, 95% B-5% B, 12.1-20.0min, 5% B-5% B; the flow rate is 0.6 mL/min; temperature of the column: 30 ℃; sample introduction amount: 5 mu L of the solution; temperature of a sample injection tray: 4 ℃; ultraviolet detection wavelength: 280 nm.
Example 2 the chromatogram of the assay results is shown in FIG. 2, in which 1: 5-Hydroxymethylfurfural (HMF); 2: furfural (F); 3: 2-Furanylmethyl ketone (FMC); 4: 5-Methylfurfural (MF); 5: the original sample interferes with the stray peaks. The test compound pairs before and after treatment are shown in table 2:
TABLE 2
| HMF(ug/100g) | F(ug/100g) | MFC(ug/100g) | MF(ug/100g) | |
| Before treatment | 2280.32 | 306.50 | 81.65 | 127.93 |
| After treatment | 1885.38 | 149.57 | 8.91 | 11.85 |
Example 3
The purification detection method of the furfural compounds in the normal-temperature coffee milk comprises the following steps:
(1) weighing 15g of a normal-temperature coffee milk sample, adding 5mL of oxalic acid solution with the concentration of 0.15mol/L prepared in situ, heating in a water bath at 100 ℃ for 25 minutes, and cooling to room temperature;
(2) adding 3mL of trichloroacetic acid solution with the concentration of 40g/mL into the mixed solution obtained in the step (1), shaking for 10 minutes, centrifuging for 15 minutes at 4.355g, pouring the supernatant into a 25mL volumetric flask, adding 5mL of trichloroacetic acid solution with the concentration of 4g/mL into the filter residue, shaking for 10 minutes, and centrifuging for 15 minutes at 4.355 g; mixing the supernatants, adding trichloroacetic acid solution with concentration of 4g/mL to fix volume to the middle scale;
(3) adding 0.5g of activated carbon A into the supernatant with constant volume obtained in the step (2), shaking for 10 minutes, heating in a water bath at 78 ℃ for 30 minutes, and cooling to room temperature;
(4) and (3) enabling the sample solution obtained in the step (3) to pass through a 0.45-micrometer nylon filter membrane, performing sample injection analysis by using a high performance liquid chromatograph, and selecting a reversed-phase C18 chromatographic column with the filler particle size of 3 micrometers, wherein the chromatographic column comprises the following components: waters Atlantis T3(3.0 mm. times.15 cm, 3 μm); mobile phase: the mobile phase A is water, and the mobile phase B is acetonitrile; gradient elution: 0-10.0min, 5% B-95% B, 10.0-12.0min, 95% B-95% B, 12.0-12.1min, 95% B-5% B, 12.1-20.0min, 5% B-5% B; the flow rate is 0.6 mL/min; temperature of the column: 30 ℃; sample introduction amount: 5 mu L of the solution; temperature of a sample injection tray: 4 ℃; ultraviolet detection wavelength: 280 nm.
Example 3 the chromatogram of the assay result is shown in fig. 3, in which 1: 5-Hydroxymethylfurfural (HMF); 2: furfural (F); 3: 2-Furanylmethyl ketone (FMC); 4: 5-Methylfurfural (MF); 5: the original sample interferes with the stray peaks. The test compound pairs before and after treatment are shown in table 3:
TABLE 3
| HMF(ug/100g) | F(ug/100g) | MFC(ug/100g) | MF(ug/100g) | |
| Before treatment | 4383.13 | 334.71 | 0 | 287.94 |
Example 4
The purification detection method of the furfural compounds in the normal-temperature coffee dairy product comprises the following steps:
(1) weighing 15g of a normal-temperature coffee dairy product sample, adding 7.5mL of oxalic acid solution with the concentration of 0.12mol/L prepared in situ, heating in a water bath at 120 ℃ for 20 minutes, and cooling to room temperature;
(2) adding 3mL of trichloroacetic acid solution with the concentration of 45g/mL into the mixed solution obtained in the step (1), shaking for 12 minutes, centrifuging for 18 minutes at 5g, pouring the supernatant into a 25mL volumetric flask, adding 5mL of trichloroacetic acid solution with the concentration of 4.5g/mL into the filter residue, shaking for 12 minutes, and centrifuging for 15 minutes at 5 g; mixing the supernatants, adding trichloroacetic acid solution with concentration of 4.5g/mL to fix volume to the middle scale;
(3) adding 0.75g of activated carbon B into the constant volume supernatant obtained in the step (2), shaking for 7 minutes, heating in a water bath at 80 ℃ for 25 minutes, and cooling to room temperature;
(4) and (3) enabling the sample solution obtained in the step (3) to pass through a 0.45-micrometer nylon filter membrane, performing sample injection analysis by using a high performance liquid chromatograph, and selecting a reversed phase C18 chromatographic column with the filler particle size of 3.5 micrometers, wherein the chromatographic column comprises the following components: waters Atlantis T3(3.0 mm. times.15 cm, 3.5 μm); mobile phase: the mobile phase A is water, and the mobile phase B is acetonitrile; gradient elution: 0-10.0min, 5% B-95% B, 10.0-12.0min, 95% B-95% B, 12.0-12.1min, 95% B-5% B, 12.1-20.0min, 5% B-5% B; the flow rate is 0.7 mL/min; temperature of the column: at 32 ℃; sample introduction amount: 5.5 mu L; temperature of a sample injection tray: 4.2 ℃; ultraviolet detection wavelength: 290 nm.
Example 4 the chromatogram of the assay results is shown in fig. 4, in which 1: 5-Hydroxymethylfurfural (HMF); 2: furfural (F); 3: 2-Furanylmethyl ketone (FMC); 4: 5-Methylfurfural (MF); 5: the original sample interferes with the stray peaks. The test compound pairs before and after treatment are shown in table 4:
TABLE 4
| HMF(ug/100g) | F(ug/100g) | MFC(ug/100g) | MF(ug/100g) | |
| Before treatment | 4383.13 | 334.71 | 0 | 287.94 |
| After treatment | 3329.24 | 196.56 | 0 | 54.55 |
4 furfural compounds in the existing method (patent: rapid detection method of furfural compounds in dairy products) (application number: 201811562740.9)) can be effectively detected, but the existing method has more impurity peaks and higher content, and particularly a chromatographic impurity peak with a larger value appears before the retention time is 10 min.
In the detection chromatogram after the activated carbon treatment, the volume-fixed supernatant is treated by 2 percent of activated carbon at 78 ℃ for 30min, the number 5 miscellaneous peak represented by 10min is obviously reduced, the baseline drift condition is obviously improved, and the detection chromatogram is purified to a great extent; meanwhile, 4 types of furfural compounds are slightly reduced, and can be effectively detected.
In the examples 1-4, furfural compounds in normal-temperature coffee milk are effectively detected, the number 5 miscellaneous peak is obviously reduced, the baseline drift condition is obviously improved, and the detection chromatogram is purified to a great extent.
The embodiments of the present invention are merely illustrative and not restrictive, and those skilled in the art can modify the embodiments without inventive contribution as required after reading the present specification, but the present invention is protected by patent law within the scope of the appended claims.
Claims (10)
1. A purification detection method for furfural compounds in coffee dairy products is characterized by comprising the following steps:
(1) adding oxalic acid solution into a coffee dairy product sample, heating in a water bath, and cooling to room temperature;
(2) adding trichloroacetic acid solution A, shaking and mixing, centrifuging at the rotating speed of 4-5g, taking supernatant, adding filter residue into trichloroacetic acid solution B, shaking and mixing, and centrifuging at the rotating speed of 4-5 g; mixing the supernatants, adding trichloroacetic acid solution B to desired volume;
(3) adding activated carbon into the supernatant obtained in the step (2) with constant volume, heating in a water bath after shaking, and cooling to room temperature;
(4) and (3) filtering the sample solution obtained in the step (3) through a nylon filter membrane, performing sample injection analysis by using a high performance liquid chromatograph, selecting a reversed phase C18 chromatographic column with the filler particle size of 2.7-3.5 mu m, wherein the mobile phase is water and acetonitrile, the flow rate is 0.5-0.7mL/min, the column temperature is 28-32 ℃, and detecting the content of the furfural compounds after chromatographic analysis.
2. The method for purifying and detecting furfural compounds in coffee dairy products as claimed in claim 1, wherein in the step (1), the volume of the oxalic acid solution added to each g of sample solution is 0.3-0.5mL, and the concentration of the oxalic acid solution is 0.12-0.16 mol/L.
3. The method for purifying and detecting the furfural compounds in the coffee dairy product according to claim 1, characterized in that in the step (1), the water bath heating temperature is 90-120 ℃ and the time is 20-30 min.
4. The method for purifying and detecting furfural compounds in coffee dairy products as claimed in claim 1, wherein in the step (2), the concentration of trichloroacetic acid solution A is 35-45g/mL, and the concentration of trichloroacetic acid solution B is 3.5-4.5 g/mL.
5. The method for purifying and detecting the furfural compounds in the coffee dairy product as claimed in claim 1, wherein in the step (2), the rotation speed of both the centrifuges is 4.355 g; and/or the time for two centrifugations is 12-18 min.
6. The method for purifying and detecting the furfural compounds in the coffee dairy product according to claim 1, characterized in that in the step (3), the adding amount of the activated carbon is 1% -3%, and the activated carbon accounts for the mass/volume percentage of the constant volume supernatant obtained in the step (2).
7. The method for purifying and detecting furfural compounds in coffee dairy products as claimed in claim 1, wherein in the step (3), the shaking time is 7-13 min; and/or the water bath heating temperature is 75-80 ℃, and the heating time is 25-35 min.
8. The method for purifying and detecting furfural compounds in coffee dairy products as claimed in claim 1, wherein in the step (3), the length of the chromatographic column is 12-18cm, the inner diameter is 2.8-3.2mm, and the film thickness is 2.5-3.5 μm.
9. The method for purifying and detecting furfural compounds in coffee dairy products as claimed in claim 1, wherein in the step (4), the aperture of the nylon filter membrane is 0.45 μm.
10. The method for purifying and detecting the furfural compounds in the coffee dairy product as claimed in claim 1, wherein in the step (4), the sample injection amount is 4.5-5.5 μ L, and the temperature of a sample injection tray is 3.8-4.2 ℃; the ultraviolet detection wavelength is 270-290 nm.
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