CN113848196B - Method for detecting content of trace iron in cereal food based on photoelectric coupling method - Google Patents

Method for detecting content of trace iron in cereal food based on photoelectric coupling method Download PDF

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CN113848196B
CN113848196B CN202111448628.4A CN202111448628A CN113848196B CN 113848196 B CN113848196 B CN 113848196B CN 202111448628 A CN202111448628 A CN 202111448628A CN 113848196 B CN113848196 B CN 113848196B
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sample
visible light
cereal food
film
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CN113848196A (en
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金钊
吕瑶瑶
钟光波
孟嫚
周孙林
黄景辉
邓清
杨哪
徐振林
孙远明
赵书馨
陈新文
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Licheng Testing and Certification Group Co., Ltd.
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Guangdong Licheng Detection Technology Co ltd
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    • G—PHYSICS
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    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/59—Transmissivity
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract

The invention discloses a method for detecting the content of trace iron in cereal food based on a photoelectric coupling method, which comprises the steps of crushing, pasting, pulping, homogenizing under high pressure, defoaming in vacuum, performing delayed flow film forming and the like on the cereal food to be detected to prepare a sample film, then applying excitation signal voltage with specific frequency between two ends of the sample film, detecting the absolute value of the light intensity difference of visible light before and after the visible light penetrates through the sample film, and then obtaining the iron content in the cereal food to be detected according to a pre-established relational expression of the iron content in the cereal food and the absolute value of the light intensity difference of the visible light before and after the visible light penetrates through the corresponding sample film. The detection method provided by the invention does not need to carry out complex pretreatment on the sample, does not need complex equipment, is simple to operate, has short detection period and good accuracy, and can well meet the requirements of simple and rapid detection.

Description

Method for detecting content of trace iron in cereal food based on photoelectric coupling method
Technical Field
The invention particularly relates to a method for detecting the content of trace iron in cereal food, and belongs to the technical field of photoelectric detection.
Background
Iron is a nutrient necessary for human bodies, iron deficiency is the first of 'hidden hunger' in the world, and iron deficiency diseases seriously harm the health of people. Wheat, corn and the like are used as staple food in the Chinese and western regions, but the iron content is low, and the dietary nutrition enrichment becomes the focus of attention of people. The GB 14880 and 2012 food nutrition enhancer use standard and the GB 2760 and 2014 food additive use standard are specifically specified for the nutrition enhancer. The iron as the enhancer mainly comprises more than ten kinds of lactoferrin, ferrous gluconate, ferric pyrophosphate, ferric citrate, ferrous lactate, NaFeEDTA and the like. The amount of the iron nutrition enhancer in the grains such as rice, wheat, coarse cereals and the like is 14-26 mg/kg, the iron is enhanced in the grains, the process is simple, the cost is low, and the prospect is good. However, the control of the content is very important when iron fortification of the grain is performed. Excessive iron is added into the grains, so that the color of the grains is changed, and the taste of the grains is also changed. In addition, excessive iron intake can not be metabolized by human body, and is deposited on organs such as liver, heart and endocrine, which affects human health. At present, methods for detecting the iron content in food mainly comprise chemical methods such as an atomic absorption method and a colorimetric method, for example, CN210401313U, but the pretreatment process is complex, the detection efficiency is low, and the detection period is long. In recent years, some researchers have proposed the detection of iron content by using photoelectric detection technology, such as CN101655476B and CN107782719A, but the operation is also complicated, and the cost of the related equipment is high, so that it is difficult to realize simple and rapid detection.
Disclosure of Invention
The invention mainly aims to provide a method for detecting the content of trace iron in cereal food based on a photoelectric coupling method, so as to overcome the defects in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
a method for detecting the content of trace iron in cereal food based on a photoelectric coupling method comprises the following steps:
s1, crushing the cereal food to be detected, mixing the crushed cereal food with deionized water, fully stirring the mixture until the mixture is completely gelatinized, pulping the mixture, and homogenizing the mixture under high pressure to obtain a to-be-detected pre-prepared sample;
s2, performing vacuum defoaming treatment on the to-be-detected prefabricated sample;
s3, performing flow extension on the to-be-detected prefabricated sample at room temperature to form a film, and standing to obtain a to-be-detected sample film;
s4, solidifying the film of the sample to be detected in a constant temperature and humidity environment;
s5, applying an excitation signal voltage with the frequency of 40kHz between the two ends of the sample film to be detected, irradiating one side surface of the sample film to be detected with visible light, and detecting the absolute value delta of the light intensity difference of the visible light before and after the visible light penetrates through the sample film to be detectedx c ；
S6, according to Deltax c And a predetermined iron content in the cerealYAbsolute value delta of light intensity difference between visible light before and after transmitting through corresponding sample filmxIs a relational expression ofY=0.005ΔxAnd the value of + C and C is 5.136-5.786, and the iron content in the cereal food to be detected is calculated.
Compared with the prior art, the detection method provided by the invention does not need to carry out complex pretreatment on the sample, does not need complex equipment, is simple to operate, has short detection period and good accuracy, and can well meet the requirements of simple and rapid detection.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a schematic diagram of a method for measuring the trace iron content in cereal based food by using a photoelectric coupling method according to an exemplary embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
The principle of the method for detecting the content of trace iron in cereal food based on the photoelectric coupling method mainly comprises the following steps: the dielectric relaxation effect of Fe on the alternating electric field under the specific frequency (40 kHz) strengthens the oscillation response of iron ions in a complex electrolyte system on the alternating electric field, and then causes specific absorption on visible light. The method comprises the steps of sample pre-preparation, vacuum defoaming, flow-extending film preparation, constant-temperature and constant-humidity film solidification, photoelectric detection, analysis and the like.
In some embodiments of the present invention, a method for detecting trace iron content in cereal food based on a photoelectric coupling method specifically includes:
s1, crushing the cereal food to be detected, mixing the crushed cereal food with deionized water, fully stirring the mixture until the mixture is completely gelatinized, pulping the mixture, and homogenizing the mixture under high pressure to obtain a to-be-detected pre-prepared sample;
s2, performing vacuum defoaming treatment on the to-be-detected prefabricated sample;
s3, performing flow extension on the to-be-detected prefabricated sample at room temperature to form a film, and standing to obtain a to-be-detected sample film;
s4, solidifying the film of the sample to be detected in a constant temperature and humidity environment;
s5, applying an excitation signal voltage with a specific frequency between two ends of the sample film to be detected, irradiating one side surface of the sample film to be detected with visible light, and detecting the absolute value delta of the light intensity difference of the visible light before and after the visible light penetrates through the sample film to be detectedx c ；
S6, according to Deltax c And a predetermined iron content in the cerealYAbsolute value delta of light intensity difference between visible light before and after transmitting through corresponding sample filmxIs a relational expression ofY=0.005ΔxAnd the value of + C and C is 5.136-5.786, and the iron content in the cereal food to be detected is calculated.
Further, the method further comprises the following steps: taking a series of cereal food samples with different iron contentsProcessing in steps S1-S5 to determine the iron content of the cerealYAbsolute value delta of light intensity difference between visible light before and after transmitting through corresponding sample filmxThe detection range corresponding to the relational expression is 0-30 mg/kg.
In order to ensure the detection accuracy, the grain food standard samples and the grain food to be detected are mixed with deionized water according to the same mass ratio, and sample films with the same thickness are prepared. The voltage of the excitation signal and the illumination intensity of the visible light applied to the sample films should be consistent.
In some embodiments, step S1 includes: and mixing the crushed cereal food to be detected with deionized water according to the mass ratio of 1: 2-1: 4, and fully stirring until complete gelatinization.
In some embodiments, step S1 includes: grinding cereal food to be detected, drying, pulverizing, mixing with deionized water, and stirring at 90-100 deg.C to completely gelatinize.
In some embodiments, step S2 includes: and (3) carrying out vacuum defoaming treatment on the to-be-detected prefabricated sample for 40-50 min under the vacuum condition of 0.2-0.5 MPa.
In some embodiments, step S3 includes: pouring the to-be-detected prefabricated sample into a transparent flat plate with a groove, performing casting film forming at room temperature, and standing for 40-50 min to obtain a to-be-detected sample thin film with the thickness of 0.2-1.2 mm.
In some embodiments, step S4 includes: and solidifying the sample film to be detected for 40-45 min in a constant-temperature and constant-humidity environment with the temperature of 50-55 ℃ and the relative humidity of 60-70% RH.
In some embodiments, step S5 includes: and applying an excitation signal voltage between two ends of the sample film to be detected at room temperature, wherein the magnitude of the excitation signal voltage is 100-.
In some embodiments, step S5 includes: and a light source and a light intensity detection device for emitting the visible light are respectively arranged on two sides of the sample film to be detected, wherein the distance between the light emitting surface of the light source and the surface of the sample film to be detected and the distance between the light receiving surface of the light intensity detection device and the surface of the sample film to be detected are both within 10 mm.
In a more specific embodiment of the present invention, a method for detecting the content of trace iron in cereal food based on a photoelectric coupling method may comprise the following steps:
s1, grinding the cereal food, drying at 40-120 deg.C (preferably 110 deg.C for 1.5 h), pulverizing, adding 2-4 times of deionized water, stirring at 90-100 deg.C (preferably 95 deg.C water bath) to completely gelatinize, pulping, and homogenizing under high pressure to obtain the desired product.
S2, defoaming the pre-prepared sample under the vacuum condition at 0.2-0.5 MPa for 40-50 min.
S3, pouring the prefabricated sample into a transparent flat plate (such as a quartz glass flat plate and other insulating flat plates) with a groove, wherein the length and width of the groove are 100mm multiplied by 100mm or less, the groove depth is 2mm or more, casting film formation is carried out at room temperature (such as 25 ℃) and the film thickness is 0.2-1.2 mm, and standing for 40-50 min to obtain a sample film.
S4, placing the transparent flat plate carrying the sample film in a constant temperature and humidity environment, adjusting the relative humidity to be 60-70% RH, fixing the film for 40-45 min, and setting the temperature to be 50-55 ℃.
S5, referring to FIG. 1, at room temperature (e.g. 25 ℃), two metal electrodes (e.g. copper electrodes with length, width, thickness and size of 100mm × 2mm × 2 mm) are placed at two ends of a sample film, and an excitation signal voltage (100 + 200mV, frequency 40 kHz) is connected, a light source is arranged at a position 10mm above the sample film to emit visible light with light intensity of 2000 + 4000Lx, a light intensity detection device is arranged at a position 10mm below the sample film to detect the light intensity of the transmitted visible light, and the absolute value delta of the light intensity difference of the visible light before and after the visible light transmits the sample film is calculated and obtainedx. Wherein the light source may be an LED lamp, a tungsten lamp, an iodine lamp, etc. without being limited thereto. The light intensity detecting device may be an illumination intensity measuring instrument or the like, and is not limited thereto.
S6, collecting numberAccording to the modeling, the iron content in the sample is obtainedYAnd the absolute value delta of the difference between the light intensities of the visible light before and after the visible light transmits through the corresponding sample filmxIs a relational expression ofY=0.005Δx+ C, wherein C is a constant, the value of the constant is changed within the range of 5.136-5.786 according to different types of cereal foods, and the detection range is 0-30 mg/kg.
The technical solution of the present invention will be explained in more detail with reference to several embodiments as follows.
Embodiment 1 a method for detecting the content of trace iron in a corn cake based on a photoelectric coupling method comprises the following steps:
s1, grinding the corn cake, drying for 1.5h at 110 ℃, crushing, adding the ground corn cake into deionized water to enable the mass ratio of the corn cake to the water to be 1:2, fully stirring in a water bath at 95 ℃ until the corn cake is completely gelatinized, pulping, and homogenizing under high pressure to obtain a pre-prepared sample.
And S2, defoaming the pre-prepared sample under the vacuum condition and 0.2MPa for 50 min.
S3, pouring the prefabricated sample into a quartz glass flat plate with a groove, wherein the length, width and depth of the groove are 100mm multiplied by 2mm, carrying out casting film formation at room temperature, and keeping the film thickness at 0.8mm for 40min to obtain a sample film.
S4, placing the quartz glass plate carrying the sample film in a constant temperature and humidity environment, adjusting the relative humidity to 60% RH, fixing the film for 40min, and setting the temperature to 55 ℃.
S5, connecting two copper electrodes with length, width and thickness of 100mm multiplied by 2mm at two ends of the sample film at room temperature, connecting the electrodes with excitation signal voltage of 160mV and frequency of 40kHz, emitting visible light with light intensity of 3200Lx at a position 10mm right above the film, detecting the light intensity of the transmitted visible light at a position 10mm below the film, and calculating to obtain the absolute value delta of the light intensity difference of the visible light before and after the visible light penetrates through the sample filmx。
S6, taking a series of corn cakes with known and different iron contents as standard samples, detecting the standard samples according to the operation of the steps S1-S5, and modeling by collecting obtained data to obtain the iron content in the standard samplesYAnd the absolute value delta of the difference between the light intensities of the visible light before and after the visible light transmits through the corresponding sample filmxIs onTying typeY=0.005Δx+5.136, the detection range is 0-30 mg/kg. Then, detecting the corn cake with unknown iron content to be detected according to the operation of the steps S1-S5 to obtain the absolute value delta of the corresponding light intensity difference valuex c According to ax c And calculating to obtain the iron content in the corn cake to be detected according to the relational expression.
The method of the embodiment and the method of GB 5009.268-2016 are respectively adopted to test 8 corn cakes sold by different merchants, and the results are shown in the following table 1, which fully illustrates the accuracy of the method of the embodiment.
TABLE 1 iron content test results for 8 commercially available corn cakes
Figure DEST_PATH_IMAGE001
Embodiment 2 a method for detecting the content of trace iron in whole-wheat bread based on a photoelectric coupling method, comprising the following steps:
s1, grinding the whole wheat bread, drying for 1.5h at 110 ℃, crushing, adding the crushed whole wheat bread into deionized water to enable the mass ratio of the whole wheat bread to the water to be 1:3, fully stirring in a water bath at 95 ℃ until the whole wheat bread is completely gelatinized, pulping, and homogenizing under high pressure to obtain a pre-prepared sample;
s2, defoaming the pre-prepared sample under the vacuum condition at 0.5MPa for 40 min;
s3, pouring the prefabricated sample into a quartz glass flat plate with a groove, wherein the length, width and depth of the groove are 100mm multiplied by 2mm, performing casting film forming at room temperature, and keeping the film thickness at 1.2mm for 50 min;
s4, placing the quartz glass flat plate carrying the sample film into a constant temperature and humidity environment, adjusting the relative humidity to 64% RH, fixing the film for 45min, and setting the temperature to 55 ℃;
s5, connecting two copper electrodes with length, width and thickness of 100mm multiplied by 2mm at two ends of the sample film at room temperature, connecting excitation signal with voltage of 200mV and frequency of 40kHz, emitting visible light with light intensity of 4000Lx at a position 10mm right above the film, detecting the light intensity of the transmitted visible light at a position 10mm below the film, and calculating to obtain the visible light intensity at the position 10mm below the filmAbsolute value delta of difference in light intensity before and after permeation through sample filmx。
S6, taking a series of whole wheat breads with known and different iron contents as standard samples, detecting the standard samples according to the operations of the steps S1-S5, and modeling by collecting obtained data to obtain the iron contents in the standard samplesYAnd the absolute value delta of the difference between the light intensities of the visible light before and after the visible light transmits through the corresponding sample filmxIs a relational expression ofY=0.005Δx+5.267, the detection range is 0-30 mg/kg. Then, detecting the whole wheat bread to be detected with unknown iron content according to the operation of the steps S1-S5 to obtain the absolute value delta of the corresponding light intensity difference valuex c According to ax c And calculating the iron content in the whole wheat bread to be measured according to the relational expression.
The method of the embodiment and the method of GB 5009.268-2016 were used to test 5 kinds of wholewheat breads sold by different merchants, and the results are shown in the following table 2, which fully illustrates the accuracy of the method of the embodiment.
TABLE 2 iron content test results of 5 kinds of wholewheat bread sold on the market
Figure 459088DEST_PATH_IMAGE002
Embodiment 3 a method for detecting the content of trace iron in a coarse cereal biscuit based on a photoelectric coupling method, comprises the following steps:
s1, grinding the coarse cereal biscuits, drying for 1.5h at 110 ℃, crushing, adding the crushed coarse cereal biscuits into deionized water to enable the mass ratio of the coarse cereal biscuits to the water to be 1:4, fully stirring in a water bath at 95 ℃ until the coarse cereal biscuits are completely gelatinized, pulping, and homogenizing under high pressure to obtain a pre-prepared sample;
s2, defoaming the pre-prepared sample under the vacuum condition for 50min under the pressure of 0.3 MPa;
s3, pouring the prefabricated sample into a quartz glass flat plate with a groove, wherein the length, width and depth of the groove are 100mm multiplied by 2mm, performing casting film forming at room temperature, and keeping the film thickness at 0.2mm for 45 min;
s4, placing the quartz glass flat plate carrying the sample film into a constant temperature and humidity environment, adjusting the relative humidity to 70% RH, fixing the film for 40min, and setting the temperature to 50 ℃;
s5, connecting two copper electrodes with length, width and thickness of 100mm multiplied by 2mm at two ends of the sample film at room temperature, connecting excitation signal with voltage of 100mV and frequency of 40kHz, emitting visible light with light intensity of 2000Lx at a position 10mm right above the film, detecting the light intensity of the transmitted visible light at a position 10mm below the film, and calculating to obtain the absolute value delta of the light intensity difference of the visible light before and after the visible light penetrates through the sample filmx。
S6, taking a series of different coarse cereal biscuits with known iron content as standard samples, detecting the standard samples according to the operation of the steps S1-S5, and modeling by collecting obtained data to obtain the iron content in the standard samplesYAnd the absolute value delta of the difference between the light intensities of the visible light before and after the visible light transmits through the corresponding sample filmxIs a relational expression ofY=0.005Δx+5.786, the detection range is 0-30 mg/kg. Then, detecting the coarse cereal biscuits to be detected with unknown iron content according to the operation of the steps S1-S5 to obtain the absolute value delta of the corresponding light intensity difference valuex c According to ax c And calculating to obtain the iron content in the coarse cereal biscuits to be detected according to the relational expression.
The method of the embodiment and the method of GB 5009.268-2016 are respectively adopted to test 10 kinds of cereal biscuits sold by different merchants, and the results are shown in the following table 3, which fully illustrates the accuracy of the method of the embodiment.
Table 3 iron content test results of 10 commercially available cereal biscuits
Figure DEST_PATH_IMAGE003
It should be understood that the above describes only some embodiments of the present invention and that various other changes and modifications may be affected therein by one of ordinary skill in the related art without departing from the scope or spirit of the invention.

Claims (7)

1. A method for detecting the content of trace iron in cereal food based on a photoelectric coupling method is characterized by comprising the following steps:
s1, crushing the cereal food to be detected, mixing the crushed cereal food with deionized water, fully stirring the mixture until the mixture is completely gelatinized, pulping the mixture, and homogenizing the mixture under high pressure to obtain a to-be-detected pre-prepared sample;
s2, performing vacuum defoaming treatment on the to-be-detected prefabricated sample;
s3, performing casting film forming on the pre-sample to be detected after vacuum defoaming treatment at room temperature, and standing to obtain a sample film to be detected;
s4, solidifying the sample film to be detected for 40-45 min in a constant temperature and humidity environment with the temperature of 50-55 ℃ and the relative humidity of 60-70% RH;
s5, applying an excitation signal voltage with the amplitude of 100-x c ；
S6, according to Deltax c And a predetermined iron content in the cerealYAbsolute value delta of light intensity difference between visible light before and after transmitting through corresponding sample filmxIs a relational expression ofY=0.005ΔxAnd the value of + C and C is 5.136-5.786, and the iron content in the cereal food to be detected is calculated.
2. The method of claim 1, comprising: processing a series of cereal standards with different iron contents by steps S1-S5 to determine the cerealIron content in foodYAbsolute value delta of light intensity difference between visible light before and after transmitting through corresponding sample filmxThe detection range corresponding to the relational expression is 0-30 mg/kg.
3. The method according to claim 1, wherein step S1 includes: and mixing the crushed cereal food to be detected with deionized water according to the mass ratio of 1: 2-1: 4, and fully stirring until complete gelatinization.
4. The method according to claim 3, wherein step S1 includes: grinding cereal food to be detected, drying, pulverizing, mixing with deionized water, and stirring at 90-100 deg.C to completely gelatinize.
5. The method according to claim 1, wherein step S2 includes: and (3) carrying out vacuum defoaming treatment on the to-be-detected prefabricated sample for 40-50 min under the vacuum condition of 0.2-0.5 MPa.
6. The method according to claim 1, wherein step S3 includes: and pouring the to-be-detected prefabricated sample into a transparent flat plate with a groove, performing casting film forming at room temperature, and standing for 40-50 min to obtain the to-be-detected sample film.
7. The method of claim 1, wherein: the thickness of the sample film to be detected is 0.2-1.2 mm.
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