CN111024907A - Method for rapidly evaluating content of furfural substances in liquid dairy product based on storage temperature and humidity of liquid dairy product - Google Patents
Method for rapidly evaluating content of furfural substances in liquid dairy product based on storage temperature and humidity of liquid dairy product Download PDFInfo
- Publication number
- CN111024907A CN111024907A CN201911369969.5A CN201911369969A CN111024907A CN 111024907 A CN111024907 A CN 111024907A CN 201911369969 A CN201911369969 A CN 201911369969A CN 111024907 A CN111024907 A CN 111024907A
- Authority
- CN
- China
- Prior art keywords
- storage
- liquid dairy
- dairy product
- furfural
- humidity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/02—Food
- G01N33/04—Dairy products
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/067—Preparation by reaction, e.g. derivatising the sample
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Immunology (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Molecular Biology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Medicinal Chemistry (AREA)
- Dairy Products (AREA)
Abstract
The invention relates to the field of food, in particular to a method for rapidly evaluating the content of furfural substances in liquid dairy products based on the storage temperature and humidity of the liquid dairy products. The method comprises the following steps: acquiring the storage temperature, the storage humidity and the storage time of the liquid dairy product; (2) and (4) evaluating the content of furfural substances in the liquid dairy product according to the storage temperature, the storage humidity and the storage time of the liquid 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 liquid dairy product only by the storage temperature, the storage humidity and the storage time of the liquid 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 liquid dairy products based on the storage temperature and humidity of the liquid dairy products.
Background
Liquid dairy has become an indispensable daily nutritional food as a recognized health drink.
The general production process of liquid dairy products such as UHI sterilized milk comprises: raw milk acceptance → purified milk → refrigeration → standardization → preheating → homogenization → ultrahigh temperature instant sterilization (135-150 ℃, 1-4 s) → cooling → aseptic filling (or keeping sterilization) → finished product storage. 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 based on the characteristics that milk contains lactose and ingredients are brought into white granulated sugar, the high-temperature processing technology is easy to cause the generation of high-content furfural compounds in UHI sterilized milk, and the furfural compounds can be further accumulated in the shelf life. Preliminary detection shows that the initial content of the furfural compounds in UHI sterilized milk is close to 50 mug/100 g, and the content of the furfural compounds is further accumulated easily by interference of external environmental factors such as temperature, humidity and the like in shelf life, namely the furfural compounds are very likely to be particularly obvious in long-shelf-life dairy products represented by UHI sterilized milk. Therefore, the content of the furfural compounds in UHI sterilized milk in shelf life needs to be reduced and controlled, so that the nutrition and health of national diet are ensured.
UHI sterilized milk in the liquid dairy product is used as a product with long shelf life at normal temperature, and does not need refrigeration transportation and storage, and the conventional conditions can avoid illumination. Although the normal temperature storage condition can cause the accumulation of Maillard reaction harmful substances including furfural compounds, no report has been made on the change of the furfural content in UHI sterilized milk under the conditions of high humidity, high temperature and extreme high temperature. Extreme external environmental factors such as high-humidity plum rain season, high temperature in summer for several months, extreme high temperature weather and the like may have important influence on the content of the furfural compounds in UHI sterilized milk.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, it is an object of the present invention to provide a method for rapidly estimating the furfural content in liquid dairy products based on the storage temperature and humidity of liquid dairy products, so as 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 liquid dairy products based on the storage temperature and humidity of the liquid dairy products, comprising:
(1) acquiring the storage temperature, the storage humidity and the storage time of the liquid dairy product;
(2) and (4) evaluating the content of furfural substances in the liquid dairy product according to the storage temperature, the storage humidity and the storage time of the liquid dairy product, wherein the furfural substances are selected from hydroxymethyl furfural and furfural.
In some embodiments of the present invention, in the step (1), the storage temperature of the liquid dairy product is 20 to 30 ℃, and the storage humidity is 85 to 95% rh.
In some embodiments of the present invention, in the step (1), the storage temperature of the liquid dairy product is 30-40 ℃, and the storage humidity is 65-85% rh.
In some embodiments of the present invention, in the step (1), the storage temperature of the liquid dairy product is 50 to 70 ℃, and the storage humidity is 40 to 60% rh.
In some embodiments of the present invention, the storage time of the liquid dairy product is 0 to 10 days.
In some embodiments of the present invention, in step (2), the method for evaluating hydroxymethylfurfural in liquid dairy food according to storage temperature, storage humidity and storage time of the liquid dairy food specifically comprises: and evaluating the content of the hydroxymethylfurfural in the liquid dairy product according to the storage temperature, the storage humidity and the storage time of the liquid 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 liquid dairy product.
In some embodiments of the invention, the method of obtaining the content of hydroxymethylfurfural in a standard comprises:
(a1) reacting the liquid 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 step (2), the method for evaluating furfural in liquid dairy product according to storage temperature, storage humidity and storage time of liquid dairy product specifically comprises: and evaluating the content of the furfural in the liquid dairy product according to the storage temperature, the storage humidity and the storage time of the liquid 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 liquid dairy product.
In some embodiments of the invention, the method of obtaining the content of furfural in a standard comprises:
(b1) reacting the liquid 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 liquid dairy product is selected from milk.
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.
Liquid dairy products, such as milk, are a long shelf life product at ambient temperature, and need not be refrigerated for transportation and storage, and conventional conditions avoid exposure to light. 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 great deal of exploration experiments that the content of furfural compounds in liquid dairy storage is related to the temperature and the humidity in the storage environment, particularly the content of hydroxymethylfurfural (CAS NO.67-47-0) and furfural (CAS NO.98-01-1) is closely related to the temperature and the humidity in the storage environment of the liquid dairy, so that the content of furfural compounds in the liquid dairy can be rapidly evaluated through the storage temperature and the humidity of the liquid dairy, and the invention is completed on the basis.
The invention provides a method for rapidly evaluating the content of furfural substances in liquid dairy products based on the storage temperature and humidity of the liquid dairy products, which comprises the following steps:
(1) acquiring the storage temperature, the storage humidity and the storage time of the liquid dairy product;
(2) and (4) evaluating the content of furfural substances in the liquid dairy product according to the storage temperature, the storage humidity and the storage time of the liquid dairy product, wherein the furfural substances are selected from hydroxymethyl furfural and furfural.
In the method for rapidly evaluating the furfural content in the liquid dairy product based on the storage temperature and humidity of the liquid dairy product, the liquid dairy product is usually prepared by raw milk which is directly extruded from the udder of a healthy dairy animal, has no change in composition, is not added with exogenous substances, is not processed, and can generally meet the relevant standards of TDTIA 001-2019, TDTIA 002-. The kind of liquid milk usually corresponds to the kind of raw milk. Preferably, the liquid dairy product according to the invention is a shelf-life liquid dairy product. In a specific embodiment of the present invention, the raw milk may be raw milk or the like, and the liquid milk may be milk or the like. The milk may be UHI sterilized milk (ultra-high temperature sterilized milk), etc., and UHI sterilized milk is obtained by instant sterilization with ultra-high temperature instant sterilization (135 deg.C to 150 deg.C, 4 to 15 seconds).
In the method for rapidly evaluating the content of furfural substances in liquid dairy products based on the storage temperature and humidity of the liquid dairy products, the temperature and humidity of the liquid dairy products in different storage environments are obtained in the step (1). Typically the storage temperature and humidity of liquid milk may be obtained using thermometers and hygrometers. The storage environment in the invention can be selected to be carried out under high humidity, high temperature and extremely high temperature. In one embodiment of the invention, in a high-humidity environment, the storage temperature of the liquid 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 liquid 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 liquid 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 liquid 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 liquid 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 liquid dairy product along with the storage time is measured.
According to the method for rapidly evaluating the content of furfural substances in liquid dairy products based on the storage temperature and humidity of the liquid dairy products, the content of hydroxymethylfurfural in the liquid dairy products can be evaluated according to the storage temperature, the storage humidity and the storage time of the liquid dairy products. The method for evaluating the hydroxymethylfurfural in the liquid dairy product according to the storage temperature, the storage humidity and the storage time of the liquid dairy product specifically comprises the following steps: and evaluating the content of the hydroxymethylfurfural in the liquid dairy product according to the storage temperature, the storage humidity and the storage time of the liquid 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 liquid dairy product. As mentioned above, there is a close relationship between the content of hydroxymethylfurfural in liquid dairy product and the storage temperature, storage humidity and storage time of liquid dairy product, and generally speaking, the higher the content of hydroxymethylfurfural, the higher the storage temperature, the higher the storage humidity and the longer the storage time of liquid dairy product. The content of the hydroxymethylfurfural in the liquid dairy product can be evaluated according to the storage temperature, the higher the storage humidity and the storage time of the liquid dairy product. The inventors have found that for normal temperature, long shelf life, hermetically packaged liquid dairy products (e.g., UHI sterilized milk products), temperature is more likely to cause accumulation of hydroxymethylfurfural in the product over time than humidity, indicating that temperature conditions are of a more significant proportion in the evaluation of hydroxymethylfurfural content, that humidity has less effect on the hermetically packaged product but is still present, and that humidity is of a lower proportion in the evaluation of hydroxymethylfurfural content.
According to the method for rapidly evaluating the furfural content in the liquid dairy product based on the storage temperature and the storage humidity of the liquid dairy product, provided by the invention, the furfural content in the liquid dairy product can be evaluated according to the storage temperature, the storage humidity and the storage time of the liquid dairy product. The method for evaluating furfural in liquid dairy product according to storage temperature, storage humidity and storage time of the liquid dairy product specifically comprises the following steps: and evaluating the content of the furfural in the liquid dairy product according to the storage temperature, the storage humidity and the storage time of the liquid 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 liquid dairy product. As mentioned above, the content of furfural in liquid dairy product has a close relationship with the storage temperature, storage humidity and storage time of liquid 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 liquid dairy product. The furfural content in the liquid dairy product can be evaluated according to the storage temperature, the higher the storage humidity and the storage time of the liquid dairy product. The present inventors have discovered that for normal temperature, long shelf life, hermetically packaged liquid dairy products (e.g., UHI sterilized milk product), temperature is more likely to cause accumulation of furfural in the product over time than humidity, indicating that temperature conditions are a more important weight in the evaluation of furfural content, and that humidity has less effect on the hermetically packaged product but is still present, indicating that humidity is a lower weight in the evaluation of furfural content.
In the method for rapidly estimating the furfural content in liquid dairy based on the storage temperature and humidity of liquid dairy, the method for obtaining the furfural content in the standard should be known to those skilled in the art, for example, the method for obtaining the hydroxymethylfurfural content in the standard may specifically include:
(a1) reacting the liquid 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 liquid 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).
Removing protein by oxalic acid free combined furfural and trichloroacetic acid solution, and further analyzing the obtained sample to obtain the content of furfural compounds (such as hydroxymethyl furfural, furfural and the like) in the liquid dairy product to be detected in a conversion manner. In a specific embodiment of the present invention, the method for obtaining the content of hydroxymethylfurfural, furfural, etc. in the liquid dairy product may be the method disclosed in chinese patent application CN 201811562740.9.
According to the method, 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 liquid 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 liquid 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 liquid dairy product 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 liquid dairy product such as milk is stored under the conditions of normal temperature, normal humidity and below, thereby ensuring the quality safety of the liquid dairy product; 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 liquid dairy products based on the storage temperature and humidity of liquid dairy products, provided by the invention, can accurately and efficiently evaluate the content of furfural compounds (such as hydroxymethylfurfural, furfural and the like) in liquid dairy products only by the storage temperature, the storage humidity and the storage time of the liquid dairy products, 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
UHI the storage temperature of the sterilized milk is 25 deg.C and the humidity is 90% rh. Stored for 0, 5 and 10 days, respectively.
Detecting UHI the content of furfural compounds in sterilized milk at 25 deg.C and humidity of 90% rh by the following steps:
(1) weighing 2.25g UHI sterilized milk sample, adding water to 15g, mixing, adding 5mL0.15mol/L of oxalic acid prepared on the same day, heating in 100 deg.C water bath 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
UHI the storage temperature of the sterilized milk is 25 deg.C and the humidity is 65% rh. Stored for 0, 5 and 10 days, respectively.
UHI the content of furfural compounds in the sterilized milk is detected under the conditions that the storage temperature is 25 ℃ and the humidity is 65 percent, and the specific method comprises the following steps:
(1) weighing 2.25g UHI sterilized milk sample, adding water to 15g, mixing, adding 5mL0.15mol/L of oxalic acid prepared on the same day, heating in 100 deg.C water bath 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 furfural-like compounds in UHI sterilized milk 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, the changes of example 1 and comparative example 1 are not obvious under the high humidity condition of example 1(25 ℃, humidity of 90% rh); 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 a glycosylated end product; humidity has no great difference influence on the furfural content of UHI sterilized milk, which shows that good packaging tightness is an important way for controlling furfural compounds from being influenced by high humidity; the final value of example 1 is still higher than the initial value, which shows that the furfural compounds are 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 aim of stabilizing the accumulation of the furfural compounds.
Example 2
UHI the storage temperature of the sterilized milk is 37 deg.C and the humidity is 75% rh. Stored for 0, 5 and 10 days, respectively.
Detecting UHI the content of furfural compounds in the sterilized milk at the storage temperature of 37 ℃ and the humidity of 75% rh, which comprises the following steps:
(1) weighing 15g of UHI sterilized milk sample, adding 4.5ml of 0.16mol/L of oxalic acid prepared on the same day, heating in 90 ℃ water bath 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
UHI the storage temperature of the sterilized milk is 25 deg.C and the humidity is 65% rh. Stored for 0, 5 and 10 days, respectively.
Detecting UHI the content of furfural compounds in sterilized milk at 25 ℃ and 65% rh, which comprises the following steps:
(1) weighing 15g of UHI sterilized milk sample, adding 4.5ml of 0.16mol/L of oxalic acid prepared on the same day, heating in 90 ℃ water bath 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 furfural-like compounds in UHI sterilized milk 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
UHI the storage temperature of the sterilized milk is 60 deg.C and the humidity is 50% rh. Stored for 0, 5 and 10 days, respectively.
UHI the content of furfural compounds is detected when the storage temperature of the sterilized milk is 60 ℃ and the humidity is 50% rh, and the specific method is as follows:
(1) weighing 15g of UHI sterilized milk 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
UHI the storage temperature of the sterilized milk is 25 deg.C and the humidity is 65% rh. Stored for 0, 5 and 10 days, respectively.
Detecting UHI the content of furfural compounds in sterilized milk at 25 ℃ and 65% rh, which comprises the following steps:
(1) weighing 15g of UHI sterilized milk 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 furfural-like compounds in UHI sterilized milk 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), under the extreme high temperature condition, compared with 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 with humidity.
In summary, by combining three examples of high humidity, high temperature and extreme high temperature, for UHI sterilized milk products with normal temperature, long shelf life and closed package, compared with humidity, temperature is more likely to cause the accumulation of maillard reaction harmful substances represented by furfural compounds in the products, and the influence of humidity on the closed package products is smaller but still exists, which explains the potential control effect of suitable packing materials on the furfural compounds. The experimental results have practical significance for the actual production and storage of the liquid 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 liquid dairy products based on the storage temperature and humidity of the liquid dairy products comprises the following steps:
(1) acquiring the storage temperature, the storage humidity and the storage time of the liquid dairy product;
(2) and (4) evaluating the content of furfural substances in the liquid dairy product according to the storage temperature, the storage humidity and the storage time of the liquid dairy product, wherein the furfural substances are selected from hydroxymethyl furfural and furfural.
2. The method according to claim 1, wherein in step (1), the storage temperature of the liquid dairy product is 20-30 ℃ and the storage humidity is 85-95% rh.
3. The method according to claim 1, wherein in step (1), the storage temperature of the liquid dairy product is 30-40 ℃ and the storage humidity is 65-85% rh.
4. The method according to claim 1, wherein in step (1), the storage temperature of the liquid dairy product is 50-70 ℃ and the storage humidity is 40-60% rh.
5. The method according to claim 1, wherein the liquid dairy product is stored for a period of time of 0 to 10 days.
6. The method according to claim 1, wherein in step (2), the method for evaluating hydroxymethylfurfural in liquid dairy product based on storage temperature, storage humidity and storage time of liquid dairy product specifically comprises: and evaluating the content of the hydroxymethylfurfural in the liquid dairy product according to the storage temperature, the storage humidity and the storage time of the liquid 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 liquid dairy product.
7. The method of claim 6, wherein obtaining the content of hydroxymethylfurfural in the standard comprises:
(a1) reacting the liquid 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 step (2), the method for estimating furfural in liquid dairy product based on storage temperature, storage humidity and storage time of liquid dairy product specifically comprises: and evaluating the content of the furfural in the liquid dairy product according to the storage temperature, the storage humidity and the storage time of the liquid 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 liquid dairy product.
9. The method of claim 8, wherein obtaining the furfural content of the standard comprises:
(b1) reacting the liquid 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 said liquid dairy product is selected from milk.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911369969.5A CN111024907A (en) | 2019-12-26 | 2019-12-26 | Method for rapidly evaluating content of furfural substances in liquid dairy product based on storage temperature and humidity of liquid dairy product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911369969.5A CN111024907A (en) | 2019-12-26 | 2019-12-26 | Method for rapidly evaluating content of furfural substances in liquid dairy product based on storage temperature and humidity of liquid dairy product |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111024907A true CN111024907A (en) | 2020-04-17 |
Family
ID=70213995
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911369969.5A Pending CN111024907A (en) | 2019-12-26 | 2019-12-26 | Method for rapidly evaluating content of furfural substances in liquid dairy product based on storage temperature and humidity of liquid dairy product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111024907A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111696630A (en) * | 2020-07-01 | 2020-09-22 | 光明乳业股份有限公司 | Method for predicting content of hydroxymethylfurfural and furfural in ultra-high temperature sterilized milk based on storage temperature and storage time |
| CN111721899A (en) * | 2020-07-01 | 2020-09-29 | 光明乳业股份有限公司 | Method for predicting content of hydroxymethylfurfural and furfural in milk powder based on storage temperature and storage time |
| CN111739590A (en) * | 2020-07-01 | 2020-10-02 | 光明乳业股份有限公司 | Method for predicting content of hydroxymethylfurfural and furfural in normal-temperature yogurt based on storage temperature and storage time |
| CN112986437A (en) * | 2020-12-30 | 2021-06-18 | 光明乳业股份有限公司 | Purification detection method for furfural compounds in coffee dairy products |
| CN113932558A (en) * | 2021-04-27 | 2022-01-14 | 海信（山东）冰箱有限公司 | Method for determining shelf life of food materials in refrigerator |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN205470869U (en) * | 2016-02-04 | 2016-08-17 | 宏业生化股份有限公司 | Furfural high stability storage device |
| CN105911198A (en) * | 2016-06-07 | 2016-08-31 | 云南中烟工业有限责任公司 | Pretreatment device for furfural substance detection and application thereof |
| 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 |
-
2019
- 2019-12-26 CN CN201911369969.5A patent/CN111024907A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN205470869U (en) * | 2016-02-04 | 2016-08-17 | 宏业生化股份有限公司 | Furfural high stability storage device |
| CN105911198A (en) * | 2016-06-07 | 2016-08-31 | 云南中烟工业有限责任公司 | Pretreatment device for furfural substance detection and application thereof |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 李宇栋: "羟甲基糠醛在乳制品热损伤评价中的应用", 《中国优秀硕士毕业论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111696630A (en) * | 2020-07-01 | 2020-09-22 | 光明乳业股份有限公司 | Method for predicting content of hydroxymethylfurfural and furfural in ultra-high temperature sterilized milk based on storage temperature and storage time |
| CN111721899A (en) * | 2020-07-01 | 2020-09-29 | 光明乳业股份有限公司 | Method for predicting content of hydroxymethylfurfural and furfural in milk powder based on storage temperature and storage time |
| CN111739590A (en) * | 2020-07-01 | 2020-10-02 | 光明乳业股份有限公司 | Method for predicting content of hydroxymethylfurfural and furfural in normal-temperature yogurt based on storage temperature and storage time |
| CN111696630B (en) * | 2020-07-01 | 2022-09-30 | 光明乳业股份有限公司 | Method for predicting content of hydroxymethyl furfural and furfural in ultra-high temperature sterilized milk based on storage temperature and storage time |
| CN111739590B (en) * | 2020-07-01 | 2022-10-04 | 光明乳业股份有限公司 | Method for predicting content of hydroxymethylfurfural and furfural in normal-temperature yogurt based on storage temperature and storage time |
| CN112986437A (en) * | 2020-12-30 | 2021-06-18 | 光明乳业股份有限公司 | Purification detection method for furfural compounds in coffee dairy products |
| CN113932558A (en) * | 2021-04-27 | 2022-01-14 | 海信（山东）冰箱有限公司 | Method for determining shelf life of food materials in refrigerator |
| CN113932558B (en) * | 2021-04-27 | 2023-07-21 | 海信冰箱有限公司 | Method for determining shelf life of food materials in refrigerator |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111024907A (en) | Method for rapidly evaluating content of furfural substances in liquid dairy product based on storage temperature and humidity of liquid dairy product | |
| CN111024906A (en) | Method for rapidly evaluating content of furfural substances in solid dairy product based on storage temperature and humidity of solid dairy product | |
| Wang et al. | Effects of ultrasonic treatment on the maturation of Zhenjiang vinegar | |
| Moreno et al. | Effect of postharvest dehydration on the composition of pinot noir grapes (Vitis vinifera L.) and wine | |
| López et al. | Impact odorants of different young white wines from the Canary Islands | |
| Mendes et al. | Quality evaluation of Portuguese honey | |
| Ajlouni et al. | Hydroxymethylfurfuraldehyde and amylase contents in Australian honey | |
| Câmara et al. | 3-Hydroxy-4, 5-dimethyl-2 (5 H)-furanone levels in fortified Madeira wines: Relationship to sugar content | |
| Baglio | Chemistry and technology of honey production | |
| Sáenz-Navajas et al. | Pigment composition and color parameters of commercial Spanish red wine samples: Linkage to quality perception | |
| US20230071696A1 (en) | Process for preparing a pumpable broth composition | |
| Oral et al. | 5-hydroxymethyl furfural formation and reaction kinetics of different pekmez samples: effect of temperature and storage | |
| CN111044692A (en) | Method for rapidly evaluating furfural substance content in liquid milk based on liquid milk heating temperature | |
| CN111044694A (en) | Method for evaluating furfural substance content in liquid milk based on liquid milk heat treatment process | |
| Meier et al. | Impact of drought stress on concentration and composition of wine proteins in Riesling | |
| Morozova et al. | Effect of headspace volume, ascorbic acid and sulphur dioxide on oxidative status and sensory profile of Riesling wine | |
| CN111048159A (en) | Evaluation method of liquid milk heat treatment process | |
| CN116858974B (en) | Identification method and application of pasteurized milk sterilization temperature | |
| BATH et al. | A research note chemical changes in Helianthus annuus and Eucalyptus lanceolatus honey during storage | |
| CN111044695A (en) | Rapid assessment method for liquid milk heat treatment process | |
| Suhag et al. | Degradation kinetics of ascorbic acid in encapsulated spray-dried honey powder packaged in aluminium laminated polyethylene and high-density polyethylene | |
| Olieman et al. | Determination of d-and l-lactic acid in fermented dairy products with HPLC | |
| Baglio et al. | The industry of honey. An introduction | |
| Aljuhaimi et al. | Determination of physicochemical properties of multifloral honeys stored in different containers | |
| JP5290721B2 (en) | Flavor improving method for bonito extract or seasoning containing bonito extract |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |