CN111024906A - Method for rapidly evaluating content of furfural substances in solid dairy product based on storage temperature and humidity of solid dairy product - Google Patents
Method for rapidly evaluating content of furfural substances in solid dairy product based on storage temperature and humidity of solid dairy product Download PDFInfo
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Abstract
The invention relates to the field of food, in particular to a method for rapidly evaluating the content of furfural substances in a solid dairy product based on the storage temperature and humidity of the solid dairy product. The method comprises the following steps: (1) obtaining the storage temperature, the storage humidity and the storage time of the solid dairy product; (2) and (4) evaluating the content of furfural substances in the solid dairy product according to the storage temperature, the storage humidity and the storage time of the solid dairy product, wherein the furfural substances are selected from hydroxymethyl furfural and furfural. The method provided by the invention can accurately and efficiently evaluate the content of furfural compounds, such as hydroxymethylfurfural, furfural and the like, in the solid dairy product only by the storage temperature, the storage humidity and the storage time of the solid dairy product, and has the advantages of simplicity, rapidness, good accuracy and good industrialization prospect.
Description
Technical Field
The invention relates to the field of food, in particular to a method for rapidly evaluating the content of furfural substances in a solid dairy product based on the storage temperature and humidity of the solid dairy product.
Background
The solid dairy product such as milk powder is a dairy product which is rich in nutrient substances such as saccharides, amino acid, calcium and the like, is easy to store and convenient to carry, and has wide audience. Among them, infant formula powder occupies a large proportion in the milk powder market. Taking whole milk powder as an example, the general production process comprises the following steps: raw milk acceptance → pretreatment (filtration, purification, storage at 4 ℃) → preheating → standardization → sterilization (95 ℃, 24 seconds) → concentration → homogenization → spray drying (130-160 ℃, several seconds) → cooling → sifting → packaging → inspection → delivery. Amino acid, lactose, reducing sugar such as white granulated sugar in ingredients and the like in the cow milk can generate Maillard reaction in the heat treatment processes such as sterilization, spray drying and the like, and the Maillard reaction is generally divided into three stages, namely a front stage, a middle stage and a rear stage, wherein a representative substance of a front stage product is furfuryl acid, and furfural compounds represented by 5-hydroxymethylfurfural (5-HMF), furfural (F), furylmethyl ketone (FMC) and Methylfurfural (MF) are mainly used in the middle stage, wherein the front two stages are common and have the tendency of converting to substances in the rear stage such as glycosylation end products and the like. The furfural compound is a product of the Maillard reaction progress stage, and the content of the furfural compound is mainly determined by the content of amino acid and reducing sugar in milk and ingredients thereof and the heat treatment strength. With the enhancement of the heat treatment strength and the increase of the content of amino acid and reducing sugar, the Maillard reaction is intensified, and the content of furfural compounds also tends to increase integrally. 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 has a function of enhancing fragrance and toning color, but excessive intake of furfural is also reported to have a risk of damaging organs such as heart and inducing chronic diseases such as diabetes.
For the research of furfural compounds, at present, the research is mainly focused on the aspects of liquid chromatography of furfural compounds represented by HMF and F, development of a liquid chromatography-mass spectrometry rapid detection method, and the like, and the research objects are mostly focused on substrates rich in saccharides such as honey and xylo-oligosaccharide. Related researches also suggest that high-content furfural compounds in milk powder are easily generated by a high-temperature processing technology based on the characteristics that milk contains lactose and ingredients are brought into white granulated sugar, and can be further accumulated in the shelf life. The initial content of furfural compounds in part of milk powder is close to 700ug/100g, the total content is up to 1.0mg/100g, and the furfural compounds are higher than pasteurized milk and ultrahigh-temperature sterilized milk by about 1 order of magnitude. Considering that milk powder is the main food source for infants and young children and the daily maximum intake is between about 0.5L and 2L (wherein the ratio of milk powder to water is about 1:7), there is a risk of approaching the upper intake limit. In addition, the content of the furfural is likely to be further accumulated by the interference of external environmental factors such as temperature, humidity and the like in the shelf life, that is, the high generation amount and the high accumulation amount of the furfural compounds are likely to be particularly obvious in long-shelf-life dairy products represented by milk powder. Therefore, it is necessary to reduce and control the content of furfural compounds in the milk powder during the shelf life, so as to ensure the health and safety of infants and adults.
The solid dairy product is a product with long shelf life at normal temperature, does not need refrigeration transportation and storage, and can be prepared under the conventional condition without illumination. Although it has been reported that maillard reaction harmful substances including furfural compounds are accumulated even under ordinary storage conditions at room temperature, no change in the furfural content of milk powder under high-humidity, high-temperature, and extremely high-temperature conditions has been reported. Changes of external environmental factors such as high temperature in summer, extreme high temperature weather, high humidity plum rain season and the like can have important influence on the content of the furfural compounds in the milk powder.
Disclosure of Invention
In view of the above disadvantages of the prior art, the present invention provides a method for rapidly estimating the content of furfural in a solid dairy product based on the storage temperature and humidity of the solid dairy product, which is used to solve the problems in the prior art.
In order to achieve the above objects and other related objects, the present invention provides a method for rapidly estimating the content of furfural in a solid dairy product based on the storage temperature and humidity of the solid dairy product, comprising:
(1) obtaining the storage temperature, the storage humidity and the storage time of the solid dairy product;
(2) and (4) evaluating the content of furfural substances in the solid dairy product according to the storage temperature, the storage humidity and the storage time of the solid dairy product, wherein the furfural substances are selected from hydroxymethyl furfural and furfural.
In some embodiments of the invention, in the step (1), the storage temperature of the solid dairy product is 20-30 ℃, and the storage humidity is 85-95% rh.
In some embodiments of the invention, in the step (1), the storage temperature of the solid dairy product is 30-40 ℃, and the storage humidity is 65-85% rh.
In some embodiments of the invention, in the step (1), the storage temperature of the solid dairy product is 50-70 ℃, and the storage humidity is 40-60% rh.
In some embodiments of the invention, the solid dairy product is stored for 0-10 days.
In some embodiments of the present invention, in the step (2), the method for evaluating hydroxymethylfurfural in the solid dairy product according to the storage temperature, the storage humidity and the storage time of the solid dairy product specifically comprises: and evaluating the content of the hydroxymethylfurfural in the solid dairy product according to the storage temperature, the storage humidity and the storage time of the solid dairy product by referring to the relationship between the content of the hydroxymethylfurfural in the standard product and the storage temperature, the storage humidity and the storage time of the solid dairy product.
In some embodiments of the invention, the method of obtaining the content of hydroxymethylfurfural in a standard comprises:
(a1) reacting the solid dairy product with oxalic acid;
(a2) reacting the product obtained in the step (a1) with trichloroacetic acid, and carrying out solid-liquid separation;
(a3) obtaining the content of the hydroxymethylfurfural in the liquid phase obtained in the step (a 2).
In some embodiments of the present invention, in the step (2), the method for evaluating furfural in the solid dairy product according to the storage temperature, the storage humidity and the storage time of the solid dairy product specifically comprises: and evaluating the content of the furfural in the solid dairy product according to the storage temperature, the storage humidity and the storage time of the solid dairy product by referring to the relationship between the content of the furfural in the standard product and the storage temperature, the storage humidity and the storage time of the solid dairy product.
In some embodiments of the invention, the method of obtaining the content of furfural in a standard comprises:
(b1) reacting the solid dairy product with oxalic acid;
(b2) reacting the product obtained in the step (b1) with trichloroacetic acid, and carrying out solid-liquid separation;
(b3) and (b) acquiring the content of the furfural in the liquid phase obtained in the step (b 2).
In some embodiments of the invention, the solid dairy product is selected from milk powder.
Drawings
Fig. 1 is a graph showing the overall trend of the content of hydroxymethylfurfural and furfural in example 1 of the present invention.
FIG. 2 is a graph showing the peak area in comparative example 1 of the present invention.
FIG. 3 is a graph showing the peak area in example 1 of the present invention.
Fig. 4 is a graph showing the overall trend of the content of hydroxymethylfurfural and furfural in example 2 according to the present invention.
FIG. 5 is a graph showing the peak area in comparative example 2 of the present invention.
FIG. 6 is a graph showing the peak area in example 2 of the present invention.
Fig. 7 is a graph showing the overall trend of the hydroxymethylfurfural and furfural contents in example 3 according to the present invention.
FIG. 8 is a graph showing the peak area in comparative example 3 of the present invention.
FIG. 9 is a graph showing the peak area in example 3 of the present invention.
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.
Solid dairy products, such as milk powder, as a product with long shelf life at normal temperature, do not need to be refrigerated for transportation and storage, and the conventional conditions can be realized by avoiding illumination. However, Maillard reaction occurs even under ordinary storage conditions at room temperature, resulting in the formation of reaction products (e.g., furfuryl acid, furfural, etc.). The inventor of the invention unexpectedly discovers through a large number of exploration experiments that the content of furfural compounds in the solid dairy product storage is related to the temperature and the humidity in the storage environment, particularly the content of hydroxymethylfurfural (CASNO.67-47-0) and furfural (CAS NO.98-01-1) is closely related to the temperature and the humidity in the solid dairy product storage environment, so that the content of furfural compounds in the solid dairy product can be rapidly evaluated through the storage temperature and the humidity of the solid dairy product, and the invention is completed on the basis.
The invention provides a method for rapidly evaluating the content of furfural substances in a solid dairy product based on the storage temperature and humidity of the solid dairy product, which comprises the following steps:
(1) obtaining the storage temperature, the storage humidity and the storage time of the solid dairy product;
(2) and (4) evaluating the content of furfural substances in the solid dairy product according to the storage temperature, the storage humidity and the storage time of the solid dairy product, wherein the furfural substances are selected from hydroxymethyl furfural and furfural.
In the method for rapidly evaluating the content of the furfural substances in the solid dairy product based on the storage temperature and humidity of the solid dairy product, the solid dairy product is usually a solid food prepared by adding exogenous substances into milk and then heating and spraying powder, the solid state can be powder or block and the like, and the solid dairy product can also be added with exogenous substances after heating and spraying the powder by the milk. Preferably, the solid dairy product of the invention is a shelf-life solid dairy product. In an embodiment of the present invention, the solid dairy product may be milk powder or the like.
In the method for rapidly evaluating the content of the furfural substances in the solid dairy product based on the storage temperature and humidity of the solid dairy product, the temperature and humidity of the solid dairy product in different storage environments are obtained in the step (1). The storage temperature and humidity of the solid dairy product can be obtained by a thermometer and a hygrometer. The storage environment in the invention can be selected to be carried out under high humidity, high temperature and extremely high temperature. In a specific embodiment of the invention, in a high-humidity environment, the storage temperature of the solid dairy product is 20-30 ℃, the storage humidity is 85-95% rh, the storage time is 0-10 days, and the change trend of the content of the furfural compounds in the solid dairy product along with the storage time is measured. In another embodiment of the invention, in a high-temperature environment, the storage temperature of the solid dairy product is 30-40 ℃, the storage humidity is 65-85% rh, the storage time is 0-10 days, and the change trend of the content of the furfural compounds in the solid dairy product along with the storage time is measured. In another embodiment of the invention, in an extreme high temperature environment, the storage temperature of the solid dairy product is 50-70 ℃, the storage humidity is 40-60% rh, the storage time is 0-10 days, and the change trend of the content of the furfural compounds in the solid dairy product along with the storage time is measured.
According to the method for rapidly evaluating the content of furfural substances in the solid dairy product based on the storage temperature and humidity of the solid dairy product, provided by the invention, the content of hydroxymethylfurfural in the solid dairy product can be evaluated according to the storage temperature, the storage humidity and the storage time of the solid dairy product. The method for evaluating the hydroxymethylfurfural in the solid dairy product according to the storage temperature, the storage humidity and the storage time of the solid dairy product specifically comprises the following steps: and evaluating the content of the hydroxymethylfurfural in the solid dairy product according to the storage temperature, the storage humidity and the storage time of the solid dairy product by referring to the relationship between the content of the hydroxymethylfurfural in the standard product and the storage temperature, the storage humidity and the storage time of the solid dairy product. As mentioned above, the content of hydroxymethylfurfural in the solid dairy product has a close relationship with the storage temperature, the storage humidity and the storage time of the solid dairy product, and generally speaking, the higher the content of hydroxymethylfurfural is, the higher the storage temperature, the higher the storage humidity and the longer the storage time of the solid dairy product are. The content of the hydroxymethylfurfural in the solid dairy product can be evaluated according to the storage temperature, the higher the storage humidity and the storage time of the solid dairy product. The inventor of the invention finds that for normal-temperature, long-shelf-life and hermetically-packaged solid dairy products (such as milk powder), the temperature is more likely to cause accumulation of hydroxymethylfurfural in the products than the humidity over time, which indicates that the temperature condition has a more important proportion in the evaluation of hydroxymethylfurfural content, the humidity has less influence on the hermetically-packaged products and still exists, and indicates that the humidity has a lower proportion in the evaluation of hydroxymethylfurfural content.
According to the method for rapidly evaluating the content of the furfural substances in the solid dairy product based on the storage temperature and the humidity of the solid dairy product, provided by the invention, the content of the furfural substances in the solid dairy product can be evaluated according to the storage temperature, the storage humidity and the storage time of the solid dairy product. The method for evaluating the furfural in the solid dairy product according to the storage temperature, the storage humidity and the storage time of the solid dairy product specifically comprises the following steps: and evaluating the content of the furfural in the solid dairy product according to the storage temperature, the storage humidity and the storage time of the solid dairy product by referring to the relationship between the content of the furfural in the standard product and the storage temperature, the storage humidity and the storage time of the solid dairy product. As mentioned above, the content of furfural in the solid dairy product has a close relationship with the storage temperature, the storage humidity and the storage time of the solid dairy product, and generally speaking, the higher the content of furfural, the higher the storage temperature, the higher the storage humidity and the longer the storage time of the solid dairy product. The furfural content in the solid dairy product can be evaluated according to the storage temperature, the higher the storage humidity and the storage time of the solid dairy product. The inventor of the invention finds that for normal-temperature, long-shelf-life and hermetically-packaged solid dairy products (such as milk powder), the temperature is more likely to cause the accumulation of furfural in the products than the humidity over time, which indicates that the temperature condition has a more important proportion in the evaluation of the furfural content, the humidity has less influence on the hermetically-packaged products and still exists, and indicates that the humidity has a lower proportion in the evaluation of the furfural content.
In the method for rapidly evaluating the content of furfural in a solid dairy product based on the storage temperature and humidity of the solid dairy product, a method for obtaining the content of furfural in a standard product should be known to those skilled in the art, for example, the method for obtaining the content of hydroxymethylfurfural in the standard product may specifically include:
(a1) reacting the solid dairy product with oxalic acid;
(a2) reacting the product obtained in the step (a1) with trichloroacetic acid, and carrying out solid-liquid separation;
(a3) obtaining the content of the hydroxymethylfurfural in the liquid phase obtained in the step (a 2).
For another example, the method for obtaining the content of furfural in the standard product may specifically include:
(b1) reacting the solid dairy product with oxalic acid;
(b2) reacting the product obtained in the step (b1) with trichloroacetic acid, and carrying out solid-liquid separation;
(b3) and (b) acquiring the content of the furfural in the liquid phase obtained in the step (b 2).
Protein is removed by oxalic acid free combined furfural and trichloroacetic acid solution, and the obtained sample is further analyzed, so that the content of furfural compounds (such as hydroxymethyl furfural, furfural and the like) in the solid dairy product to be detected can be obtained through conversion. In a specific embodiment of the present invention, the method for obtaining the content of hydroxymethylfurfural, furfural, etc. in the solid dairy product may be the method disclosed in chinese patent application CN 201811562740.9.
According to the invention, the improvement of the quality evaluation index of the dairy product is supplemented by the change of the content of the furfural compounds in the solid dairy product under three extreme environmental conditions of high humidity, high temperature and extreme high temperature, and the high initial value measured by the furfural compounds in the solid dairy product also has guiding significance for the optimization of the processing technology; secondly, providing a guidance scheme for maintaining the level of the furfural compounds of the solid dairy products within the shelf life, namely avoiding the accumulation of the furfural compounds caused by high humidity, especially extreme high temperature and other environments, and suggesting that the solid dairy products such as milk powder are stored under the conditions of normal temperature, normal humidity and below, thereby ensuring the quality safety of the solid dairy products; in addition, the evaluation method of the invention does not need special packaging, thereby ensuring the safety and health of the product.
In summary, the method for rapidly evaluating the content of furfural substances in the solid dairy product based on the storage temperature and humidity of the solid dairy product, provided by the invention, can accurately and efficiently evaluate the content of furfural compounds (such as hydroxymethylfurfural, furfural and the like) in the solid dairy product only by the storage temperature, the storage humidity and the storage time of the solid dairy product, and has the advantages of simplicity, rapidness, good 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 storage temperature of the milk powder is 25 ℃, and the humidity is 90% rh. Stored for 0, 5 and 10 days, respectively.
The method for detecting the content of the furfural compounds in the milk powder at the storage temperature of 25 ℃ and the humidity of 90% rh comprises the following steps:
(1) weighing 2.25g of milk powder sample, adding water to 15g, mixing uniformly, adding 5mL0.15mol/L of oxalic acid prepared on the same day, heating in a water bath at 100 ℃ for 25min, and cooling to room temperature;
(2) then adding 3mL of trichloroacetic acid solution A with the concentration of 40g/mL, shaking for 10min, and centrifuging for 15min at 4.355 g; pouring the supernatant into a 25mL volumetric flask, adding 5mL4g/mL trichloroacetic acid solution B into the filter residue, shaking for 10min, and centrifuging for 15min at 4.355 g; mixing the supernatants, adding 4g/mL trichloroacetic acid solution B, and metering to a certain volume;
(3) taking a proper amount of liquid, passing through a nylon filter membrane with the diameter of 0.45 mu m, and analyzing by a chromatograph. Selecting a reversed phase C18 chromatographic column with the filler particle size of 3 mu m, wherein the chromatographic column comprises the following components in percentage by weight: 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.
Comparative example 1
The storage temperature of the milk powder is 25 ℃, and the humidity is 65% rh. Stored for 0, 5 and 10 days, respectively.
Detecting the content of furfural compounds in milk powder at a storage temperature of 25 ℃ and a humidity of 65%, which comprises the following steps:
(1) weighing 2.25g of milk powder sample, adding water to 15g, mixing uniformly, adding 5mL0.15mol/L of oxalic acid prepared on the same day, heating in a water bath at 100 ℃ for 25min, and cooling to room temperature;
(2) then adding 3mL of trichloroacetic acid solution A with the concentration of 40g/mL, shaking for 10min, and centrifuging for 15min at 4.355 g; pouring the supernatant into a 25mL volumetric flask, adding 5mL4g/mL trichloroacetic acid solution B into the filter residue, shaking for 10min, and centrifuging for 15min at 4.355 g; mixing the supernatants, adding 4g/mL trichloroacetic acid solution B, and metering to a certain volume;
(3) taking a proper amount of liquid, passing through a nylon filter membrane with the diameter of 0.45 mu m, and analyzing by a chromatograph. Selecting a reversed phase C18 chromatographic column with the filler particle size of 3 mu m, wherein the chromatographic column comprises the following components in percentage by weight: 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.
The peak areas of the furfural-like compounds in the milk powders of example 1 and comparative example 1 are shown in table 1:
TABLE 1
(Note: HMF is hydroxymethylfurfural; F is furfural)
FIG. 2 is a graph of peak areas from top to bottom for 0 day, 5 days, and 10 days of storage, respectively. FIG. 3 is a graph of peak areas from top to bottom for 0 day, 5 days, and 10 days of storage, respectively.
As can be seen from FIGS. 1 to 3, in example 1(25 ℃, humidity 90% rh) under high humidity conditions, the change trend of example 1 is substantially consistent with that of comparative example 1; both HMF and F levels decreased and increased slightly, with the final value being slightly above the initial value, although the overall change was not significant, which may be related to the product having an overwrapping and conversion of HMF to glycosylated end product; humidity has no great difference influence on the furfural content in the milk powder, which shows that good packaging tightness is an important way for controlling the furfural compounds from being influenced by high humidity factors; the final value of example 1 is still higher than the initial value, which shows that the furfural compound is accumulated in a small amount, while the comparative example 1 has almost no obvious change, which shows that the actual storage should avoid high humidity, and the normal humidity is selected as much as possible to store the product so as to achieve the purpose of stabilizing the content of the furfural compound.
Example 2
The storage temperature of the milk powder is 37 ℃, and the humidity is 75% rh. Stored for 0, 5 and 10 days, respectively.
The method for detecting the content of the furfural compounds in the milk powder at the storage temperature of 37 ℃ and the humidity of 75% rh comprises the following steps:
(1) weighing 15g of milk powder sample, adding 4.5ml of 0.16mol/L of oxalic acid prepared on the same day, heating in a water bath at 90 ℃ for 30min, and cooling to room temperature;
(2) then adding 3mL of trichloroacetic acid solution A with the concentration of 35g/mL, shaking for 10min, and centrifuging for 18min at 4 g; pouring the supernatant into a 25mL volumetric flask, adding 5mL of 3.5g/mL trichloroacetic acid solution B into the filter residue, shaking for 10min, and centrifuging for 18min at 4 g; the supernatant is combined, and 3.5g/mL trichloroacetic acid solution B is added to the volume to be calibrated.
(3) Taking a proper amount of liquid, passing through a nylon filter membrane with the diameter of 0.45 mu m, and analyzing by a chromatograph. Selecting a reversed phase C18 chromatographic column with the filler particle size of 2.7 mu m, wherein the chromatographic column comprises the following components in percentage by weight: WatersatlantIST3(2.8 mm. times.12 cm, 2.8 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 0.5 mL/min; temperature of the column: 28 ℃; sample introduction amount: 4.5 mu L; temperature of a sample injection tray: 3.8 ℃; ultraviolet detection wavelength: 270 nm.
Comparative example 2
The storage temperature of the milk powder is 25 ℃, and the humidity is 65% rh. Stored for 0, 5 and 10 days, respectively.
The method for detecting the content of the furfural compounds in the milk powder at the storage temperature of 25 ℃ and the humidity of 65% rh comprises the following steps:
(1) weighing 15g of milk powder sample, adding 4.5ml of 0.16mol/L of oxalic acid prepared on the same day, heating in a water bath at 90 ℃ for 30min, and cooling to room temperature;
(2) then adding 3mL of trichloroacetic acid solution A with the concentration of 35g/mL, shaking for 10min, and centrifuging for 18min at 4 g; pouring the supernatant into a 25mL volumetric flask, adding 5mL of 3.5g/mL trichloroacetic acid solution B into the filter residue, shaking for 10min, and centrifuging for 18min at 4 g; the supernatant is combined, and 3.5g/mL trichloroacetic acid solution B is added to the volume to be calibrated.
(3) Taking a proper amount of liquid, passing through a nylon filter membrane with the diameter of 0.45 mu m, and analyzing by a chromatograph. Selecting a reversed phase C18 chromatographic column with the filler particle size of 2.7 mu m, wherein the chromatographic column comprises the following components in percentage by weight: WatersatlantIST3(2.8 mm. times.12 cm, 2.8 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 0.5 mL/min; temperature of the column: 28 ℃; sample introduction amount: 4.5 mu L; temperature of a sample injection tray: 3.8 ℃; ultraviolet detection wavelength: 270 nm.
The peak areas of the furfural compounds in the milk powders of example 2 and comparative example 2 are shown in table 2:
TABLE 2
(Note: HMF is hydroxymethylfurfural; F is furfural)
FIG. 5 is a graph of peak areas from top to bottom for 0 day, 5 days, and 10 days of storage, respectively. FIG. 6 is a graph of peak areas from top to bottom for 0 day, 5 days, and 10 days of storage, respectively.
As can be seen from fig. 4 to 6, in example 2 (temperature 37 ℃, humidity 75% rh) under high temperature conditions, HMF increased significantly. The trend of slightly decreasing HMF in comparative example 2 is probably due to the conversion of HMF to glycosylation endproducts under the normal temperature and humidity conditions of comparative example 2, while the large accumulation of HMC due to temperature in example 2 compensates for the decreasing trend of HMC due to the prolonged storage time, which is shown by the combination of the trend of significantly increasing HMC; the peak area of F showed a tendency to rise slowly.
Example 3
The storage temperature of the milk powder is 60 ℃, and the humidity is 50% rh. Stored for 0, 5 and 10 days, respectively.
The method for detecting the content of the furfural compounds in the milk powder at the storage temperature of 60 ℃ and the humidity of 50% rh comprises the following steps:
(1) weighing 15g of milk powder sample, adding 7.5ml of 0.12mol/L of oxalic acid prepared on the same day, heating in 120 ℃ water bath for 20min, and cooling to room temperature;
(2) then adding 3mL of trichloroacetic acid solution A with the concentration of 45g/mL, shaking for 12min, and centrifuging for 18min at 5 g; pouring the supernatant into a 25mL volumetric flask, adding 5mL of 4.5g/mL trichloroacetic acid solution B into the filter residue, shaking for 12min, and centrifuging for 18min at 5 g; the supernatant is combined, and 4.5g/mL trichloroacetic acid solution B is added to the volume to be calibrated.
(3) Taking a proper amount of liquid, passing through a nylon filter membrane with the diameter of 0.45 mu m, and analyzing by a chromatograph. Selecting a reversed phase C18 chromatographic column with the filler particle size of 3.5 mu m, wherein the chromatographic column comprises the following components in percentage by weight: WatersatlantIST3(3.2 mm. times.18 cm, 3.2 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.
Comparative example 3
The storage temperature of the milk powder is 25 ℃, and the humidity is 65% rh. Stored for 0, 5 and 10 days, respectively.
The method for detecting the content of the furfural compounds in the milk powder at the storage temperature of 25 ℃ and the humidity of 65% rh comprises the following steps:
(1) weighing 15g of milk powder sample, adding 7.5ml of 0.12mol/L of oxalic acid prepared on the same day, heating in 120 ℃ water bath for 20min, and cooling to room temperature;
(2) then adding 3mL of trichloroacetic acid solution A with the concentration of 45g/mL, shaking for 12min, and centrifuging for 18min at 5 g; pouring the supernatant into a 25mL volumetric flask, adding 5mL of 4.5g/mL trichloroacetic acid solution B into the filter residue, shaking for 12min, and centrifuging for 18min at 5 g; the supernatant is combined, and 4.5g/mL trichloroacetic acid solution B is added to the volume to be calibrated.
(3) Taking a proper amount of liquid, passing through a nylon filter membrane with the diameter of 0.45 mu m, and analyzing by a chromatograph. Selecting a reversed phase C18 chromatographic column with the filler particle size of 3.5 mu m, wherein the chromatographic column comprises the following components in percentage by weight: WatersatlantIST3(3.2 mm. times.18 cm, 3.2 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.
The peak areas of the furfural-like compounds in the milk powders of example 3 and comparative example 3 are shown in table 3:
TABLE 3
(Note: HMF is hydroxymethylfurfural; F is furfural)
FIG. 8 is a graph of peak areas from top to bottom for 0 day, 5 days, and 10 days of storage, respectively. FIG. 9 is a graph of peak areas from top to bottom for 0 day, 5 days, and 10 days of storage, respectively.
As can be seen from fig. 7 to 9, in example 3(60 ℃, humidity 50% rh), compared to comparative example 3, the peak areas of HMF and F in example 3 are entirely increased, and the peak area of comparative example 3 is not significantly changed, but the peak area of HMF is significantly increased (more than 2 times of the initial content), which indicates that the extreme high temperature is likely to significantly affect the accumulation of furfural compounds, especially HMF, compared to the relative humidity.
In summary, by combining three examples of high humidity, high temperature and extreme high temperature, for a milk powder product with normal temperature, long shelf life and closed package, compared with humidity, the temperature is more likely to cause the accumulation of maillard reaction harmful substances represented by furfural compounds in the product, and the influence of the humidity on the closed package product is smaller but still exists, which shows the potential control effect of a suitable packaging material on the furfural compounds. The experimental results have practical significance for the actual production and storage of the solid dairy product in shelf life: firstly, the long-shelf-life product is necessarily subjected to sterilization or drying at a certain high temperature, and the like, so that the reduction of the sterilization or drying temperature is helpful for controlling the initial amount of the furfural compound from a production source on the premise of ensuring the stability of the product in the shelf life; secondly, in the packaging link, if an outer package with better tightness is selected, the accumulation of the furfural compounds is probably weakened to a certain extent; thirdly, the temperature and humidity in different seasons of different regions are different, and the product is recommended to be stored in the environment of normal temperature and normal humidity (25 ℃, 65 +/-20% rhrh), and the storage condition of the product should be changed in time to avoid the accumulation of furfural harmful substances when meeting high humidity and high temperature, particularly in the rainy season.
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 rapidly evaluating the content of furfural substances in a solid dairy product based on the storage temperature and humidity of the solid dairy product comprises the following steps:
(1) obtaining the storage temperature, the storage humidity and the storage time of the solid dairy product;
(2) and (4) evaluating the content of furfural substances in the solid dairy product according to the storage temperature, the storage humidity and the storage time of the solid dairy product, wherein the furfural substances are selected from hydroxymethyl furfural and furfural.
2. The method according to claim 1, wherein in the step (1), the storage temperature of the solid dairy product is 20-30 ℃, and the storage humidity is 85-95% rh.
3. The method according to claim 1, wherein in the step (1), the storage temperature of the solid dairy product is 30-40 ℃, and the storage humidity is 65-85% rh.
4. The method according to claim 1, wherein in the step (1), the storage temperature of the solid dairy product is 50-70 ℃, and the storage humidity is 40-60% rh.
5. The method of claim 1, wherein the solid dairy product is stored for a period of 0 to 10 days.
6. The method according to claim 1, wherein in the step (2), the method for evaluating the hydroxymethylfurfural in the solid dairy product according to the storage temperature, the storage humidity and the storage time of the solid dairy product specifically comprises the following steps: and evaluating the content of the hydroxymethylfurfural in the solid dairy product according to the storage temperature, the storage humidity and the storage time of the solid dairy product by referring to the relationship between the content of the hydroxymethylfurfural in the standard product and the storage temperature, the storage humidity and the storage time of the solid dairy product.
7. The method of claim 6, wherein obtaining the content of hydroxymethylfurfural in the standard comprises:
(a1) reacting the solid dairy product with oxalic acid;
(a2) reacting the product obtained in the step (a1) with trichloroacetic acid, and carrying out solid-liquid separation;
(a3) obtaining the content of the hydroxymethylfurfural in the liquid phase obtained in the step (a 2).
8. The method according to claim 1, wherein in the step (2), the method for evaluating furfural in the solid dairy product according to the storage temperature, the storage humidity and the storage time of the solid dairy product specifically comprises the following steps: and evaluating the content of the furfural in the solid dairy product according to the storage temperature, the storage humidity and the storage time of the solid dairy product by referring to the relationship between the content of the furfural in the standard product and the storage temperature, the storage humidity and the storage time of the solid dairy product.
9. The method of claim 8, wherein obtaining the furfural content of the standard comprises:
(b1) reacting the solid dairy product with oxalic acid;
(b2) reacting the product obtained in the step (b1) with trichloroacetic acid, and carrying out solid-liquid separation;
(b3) and (b) acquiring the content of the furfural in the liquid phase obtained in the step (b 2).
10. The method of claim 1, wherein the solid dairy product is selected from the group consisting of milk powder.
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