CN110146496B - Method for rapidly determining peroxide value of edible oil - Google Patents

Method for rapidly determining peroxide value of edible oil Download PDF

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CN110146496B
CN110146496B CN201910451200.1A CN201910451200A CN110146496B CN 110146496 B CN110146496 B CN 110146496B CN 201910451200 A CN201910451200 A CN 201910451200A CN 110146496 B CN110146496 B CN 110146496B
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peroxide value
halogen exchange
edible oil
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陈曦
朱祎濛
李飞明
王翊如
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Abstract

The invention discloses a method for rapidly determining peroxide value of edible oil, which takes oleylamine iodide as a reducing agent of a target peroxide and CsPbBr3The fluorescence color of the perovskite nanocrystalline after halogen exchange is used as a visual indication mode of the peroxidation degree of the edible oil; molecular fluorescence detection is used as a detection method. The method is economical and applicable, simple to operate, high in sensitivity, good in reproducibility, high in selectivity, rapid in detection, easy to popularize, capable of supporting field detection and suitable for rapid determination of peroxide value of edible oil.

Description

Method for rapidly determining peroxide value of edible oil
Technical Field
The invention relates to a method for rapidly determining peroxide value of edible oil.
Background
The peroxide value represents an index of the degree of oxidation of fats and oils, fatty acids, and the like, that is, a numerical value of the total amount of peroxides in fats and oils. The peroxide in the oil is a product which has oxidation effect with oxygen in the air during the storage period of the oil, has high activity, can rapidly change and be decomposed into aldehyde, ketone, oxide and the like, and can cause rancidity and deterioration of the oil under the influence of light, heat, water, microorganisms and impurities in the oil during the storage process. Since the degree of rancidity of oil and fat can be known by measuring the peroxide value of oil and fat, the peroxide value of edible oil is one of the indexes for inspecting the oil quality. The long-term consumption of food with excessive peroxide value is very unfavorable for human health, because the peroxide can destroy the cell membrane structure, and can cause gastric cancer, liver cancer, arteriosclerosis, myocardial infarction, alopecia, weight loss and the like. The food with high peroxide value can promote cardiovascular diseases and tumor. The peroxide value is generally expressed as the mass fraction of peroxide to iodine. The peroxide value of the edible oil is definitely specified in GB/T2716-2018 national standard vegetable oil for food safety in China and is not more than 0.25g/100 g. The traditional method for measuring the peroxide value of the edible oil adopts a titration method and a potential method in the national standard GB/T5009.227-2016, but the two methods are complicated to operate, have large influence on human factors, have large harm to the environment and operators, have low sensitivity and cannot realize real-time and visual detection.
The fluorescence visualization sensor has the characteristics of high sensitivity, high detection speed and the like, and has wide application prospects in various fields of food and medicine analysis, clinical diagnosis, environmental monitoring and the like. Compared with a method for performing qualitative and quantitative detection on fluorescence intensity, the visual sensing detection based on wavelength shift has the advantages of high visual sensitivity, obvious color gradient change, less interference from external conditions, no need of additionally introducing a reference luminescent material, convenience for field detection and capability of meeting the requirement of timely detection.
All-inorganic perovskite quantum dot CsPbX3The (X ═ Cl, Br and I) has the characteristics of high fluorescence quantum yield (50-90%), narrow half-peak width and the like. The research finds that CsPbX3The fluorescence emission peak of the quantum dot can continuously red shift along with the increase of the radius of the X ions, and if the proportion of Cl, Br and I ions in X is adjusted, the full coverage of blue light to red light can be presented. After further study, CsPbX was shown3The quantum dots not only have the advantages of Cd series conventional quantum dots, but also have halogen exchange characteristics (also called halogen exchange), namely CsPbX3The halogen ions in the solution can be exchanged with other halogen ions in the solution, and the CsPbCl can be preparedmBr3-mOr CsPbBrmI3-m(m is more than or equal to 0 and less than or equal to 3), the fluorescence emission peak of the product is correspondingly blue-shifted or red-shifted, the wavelength shift value of the fluorescence emission peak has certain correlation with the value m, and the presented color is correspondingly changed, thereby establishing a foundation for the visual sensing detection of the halogen.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides a method for rapidly determining the peroxide value of edible oil, and solves the problems in the background art.
The technical scheme adopted by the invention for solving the technical problems is as follows: the method for rapidly determining the peroxide value of the edible oil comprises the following steps:
1) oxidation-reduction reaction: performing redox reaction on oleylamine iodine and peroxide in an oil sample to be detected;
2) halogen exchange reaction: mixing the unoxidized iodide ions obtained in the step 1) with the quantum dots CsPbBr3Performing halogen exchange reaction to obtain a halogen exchange reaction solution CsPbBrmI3-mWherein m is less than or equal to 3;
3) and (3) qualitative detection: comparing the halogen exchange reaction solution in the step 2) with a peroxide value colorimetric card, and determining whether the peroxide value exceeds the standard;
4) and (3) quantitative detection: constructing a fluorescence visualization sensing mode by utilizing the correlation between the m value and the wavelength shift value of the fluorescence emission peak, and determining the peroxide value of the halogen exchange reaction solution in the step 2) by using a molecular fluorescence spectrometry.
Oleylamine iodide is an organic compound which has oxidizability and can be dissolved in toluene solution, can generate oxidation-reduction reaction with peroxide in edible oil, and can also generate oxidation-reduction reaction with all-inorganic perovskite CsPbBr3The halogen exchange reaction occurs in toluene solution, the preparation is convenient, and the halogen exchange reaction is reacted with peroxide and CsPbBr3The reaction is rapid, and a good detection effect can be achieved; CsPbBr3The quantum dots are inorganic perovskite nanocrystals with halogen exchange property and capable of being dissolved in toluene solution, are nanocubes in appearance, are uniform in size, good in dispersion and relatively stable in air, and have the characteristics of high fluorescence quantum yield, narrow half-peak width and the like. Can rapidly generate halogen exchange reaction with oleylamine iodide in toluene solution, and adjust CsPbBr by I ionsmI3-mThe proportion of middle Br and I ions generates corresponding CsPbBrmI3-m(m is less than or equal to 3). Iodo CsPbBrmI3-mThe spectrum of the fluorescent probe generates red shift along with the reduction of m, and the fluorescent probe shows the fluorescent change from yellow green, yellow, orange yellow to orange red under ultraviolet light, thereby realizing the visual detection of the halogen ions.
In a preferred embodiment of the present invention, the redox reaction time is not less than 10 minutes, and the halogen exchange reaction time is not less than 5 minutes.
In a preferred embodiment of the present invention, the step 1) includes the following steps:
heating iodine simple substance and oleylamine at a molar ratio of 1mmol to 3-5 mmol under stirring for reaction, firstly heating to 110-130 ℃, then continuing heating to 190-210 ℃, stopping heating, and cooling; adding an organic solution for dilution to obtain an oleylamine iodine solution, and sealing and storing in a dark place; and (4) pumping the oil sample to be detected to react with the oleylamine iodide solution, and uniformly shaking to ensure that the reaction is complete.
In a preferred embodiment of the present invention, the step 2) CsPbBr3The quantum dot is a quantum dot for fluorescence detection, and the shape of the quantum dot is a nanocrystalline cube.
In a preferred embodiment of the present invention, the step 2) includes the following steps:
①, preparing cesium oleate, namely adding a cesium precursor into an octadecene solution dissolved with oleic acid, stirring and heating to 110-160 ℃ to completely dissolve the precursor, wherein the volume ratio of octadecene to oleic acid is 16: 1;
② preparing lead bromide precursor, adding lead bromide into octadecene solution dissolved with oleic acid and oleylamine, heating to 110-160 ℃ under stirring, wherein the volume ratio of octadecene to oleic acid to oleylamine is 10:1: 1;
③ Synthesis of CsPbBr by thermal injection3Extracting the cesium precursor solution in the step ①, quickly injecting the cesium precursor solution into the lead bromide precursor solution in the step ②, quickly placing the cesium precursor solution and the lead bromide precursor in an ice-water bath with the mol ratio of 1mmol to 3-4 mmol, shaking the cesium precursor solution and the lead bromide precursor without stopping, centrifugally extracting the product, discarding the supernatant, adding the organic solution again, centrifuging the organic solution again, and taking the supernatant to obtain CsPbBr3A saturated solution of (a);
④ mixing CsPbBr3Diluting the saturated solution, and adding the diluted saturated solution into the solution reacted in the step 1) to perform halogen exchange reaction.
In a preferred embodiment of the present invention, in the step 3), the halogen exchange reaction solution is placed under an ultraviolet lamp to observe fluorescence thereof, and compared with a peroxide value colorimetric card for determination.
In a preferred embodiment of the present invention, in the step 4), a linear equation y is set to 0.0048x by using the m value and the wavelength shift value of the fluorescence emission peak, where y is the peroxide value of the edible oil, and x is the wavelength shift value of the fluorescence emission peak, and the halogen exchange reaction solution is subjected to molecular fluorescence spectrum analysis to measure the emission wavelength and then is substituted into the linear equation to obtain the peroxide value.
In a preferred embodiment of the present invention, the step 3) employs CsPbBr with peroxide colorimetric card3Or the oleylamine iodine headspace bottle contains the halogen exchange reaction solution.
In a preferred embodiment of the present invention, the ratio of the oil sample to be tested to the oleylamine iodide is 0.2-0.25 mL:2.5 mmol.
Compared with the background technology, the technical scheme has the following advantages:
the invention combines the common indirect iodometry with the fluorescence visualization detection technology, takes oleylamine iodine as the reducing agent of the peroxide of the target substance, and takes CsPbBr3The fluorescence color of the perovskite nanocrystalline after halogen exchange is used as a visual indication mode of the peroxidation degree of the edible oil; molecular fluorescence detection is used as a detection method. The method is economical and applicable, simple to operate, high in sensitivity, good in reproducibility, high in selectivity, rapid in detection, easy to popularize, capable of supporting field detection and suitable for rapid determination of peroxide value of edible oil.
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FIG. 1(a) CsPbBr3A PL spectrum of the quantum dot; (b) CsPbBr3UV-Vis spectrogram of the quantum dot; (c) CsPbBr3XRD patterns of quantum dots; (d) CsPbBr3A TEM image of the quantum dots;
FIG. 2(a) PL profile of different redox reaction times; (b) PL spectra for different halogen exchange reaction times;
FIG. 3(a) reproducibility of oleylamine iodotoluene solution synthesized in the same batch; (b) reproducibility of oleylamine iodotoluene solutions synthesized in different batches;
FIG. 4 is a wavelength spectrum of a common interfering substance in edible oil;
FIG. 5 is a PL spectrum and its linear range for oil samples of different peroxide values;
FIG. 6 is a schematic view of a colorimetric chart showing a gradual change from red to yellow and finally to green from left to right, corresponding to different peroxide values in the range of 0-0.6g/100 g;
FIG. 7 is a schematic diagram of a headspace bottle device with a peroxide value color card.
FIG. 8 is a comparison of the results of measuring the peroxide value of the edible oil by the fluorescence visualization method and the national standard method.
Detailed Description
Example 1
The method for rapidly determining the peroxide value of the edible oil comprises the following steps:
1) oxidation-reduction reaction: performing redox reaction on oleylamine iodine and peroxide in an oil sample to be detected;
2) halogen exchange reaction: mixing the unoxidized iodide ions obtained in the step 1) with the quantum dots CsPbBr3Performing halogen exchange reaction to obtain a halogen exchange reaction solution CsPbBrmI3-mWherein m is less than or equal to 3;
3) and (3) qualitative detection: comparing the halogen exchange reaction solution in the step 2) with a peroxide value colorimetric card, and determining whether the peroxide value exceeds the standard;
4) and (3) quantitative detection: and (3) constructing a linear equation y of 0.0048x by using the m value and the wavelength shift value of the fluorescence emission peak (wherein y is the peroxide value of the edible oil, and x is the wavelength shift value of the fluorescence emission peak), carrying out molecular fluorescence spectrum analysis on the halogen exchange reaction liquid, measuring the emission wavelength of the halogen exchange reaction liquid, and substituting the emission wavelength into the linear equation to obtain the peroxide value.
The preparation of the oleylamine iodotoluene solution in the step 1) comprises the following steps:
0.75g of elemental iodine (3mmol I) was weighed2) Placed in a 25mL round bottom flask, followed by 4mL oleylamine (0.012mol OLAM). Heating and reacting under nitrogen atmosphere and magneton stirring. When the reaction temperature reached 120 ℃, the solution became bright brown in color, indicating the formation of oleylamine iodide. And (4) continuously heating to the reaction temperature of 200 ℃, stopping heating, and cooling. After the reaction is finished and cooled, adding a toluene solution into 4mL of the reaction product to dilute the reaction product to 2400mL to obtain a 2.5mmol/L toluene solution of oleylamine iodide, and storing the mixture in a sealed and light-proof manner.
Preparation of CsPbBr in step 2)3The toluene solution comprises the following steps:
① preparation of Cesium oleate 0.814g of Cs are weighed2CO3Adding 40mL of octadecene solution and 2.5mL of oleic acid; vacuumizing to remove air, heating to 120 deg.C to make Cs2CO3And (4) completely dissolving to obtain a brown yellow solution, and continuously stirring at a controlled temperature under vacuum to prepare for subsequent experiments.
② preparation of lead bromide precursor 0.069g of PbBr was weighed2Adding 5mL of octadecene solution, 0.5mL of oleic acid and 0.5mL of oleylamine; vacuumizing to remove air, heating to 120 deg.C while stirring to make PbBr2Completely dissolving; then the temperature is raised to 150 ℃, and nitrogen is introduced.
③ Synthesis of CsPbBr by thermal injection3Quantum dot: heating the prepared cesium oleate to 150 ℃, introducing nitrogen, extracting 0.4mL of cesium oleate solution, quickly injecting the cesium oleate solution into the precursor solution, quickly placing the cesium oleate solution into an ice water bath after injection, shaking the cesium oleate solution without stopping to obtain a yellow-green colloidal product, taking out the yellow-green colloidal product, and naturally heating the product to room temperature. Centrifuging the quantum dot product at 10000r/min for 10 minutes, discarding the supernatant, and keeping the bottom precipitate; adding toluene solution into the precipitate, centrifuging for 10 min, collecting supernatant CsPbBr3Adding toluene into the saturated toluene solution to dilute the saturated toluene solution to half of the original concentration, and sealing and storing the saturated toluene solution at low temperature.
One, quantum dot CsPbBr3Measurement of (2)
To explore the synthesized CsPbBr3Macroscopic property and microscopic appearance of perovskite nanocrystal, and experiment on synthesized CsPbBr3Perovskite nanocrystals were characterized. The prepared quantum dots are in the shape of a nanocrystalline cube, are uniform in size, good in dispersion and relatively stable in air, and have the characteristics of high fluorescence quantum yield, narrow half-peak width and the like (CsPbBr prepared in the experimental process)3Quantum dots can function as shown in fig. 1).
Second, determination of optimum reaction time
To determine the optimum reaction time for this method, experiments were investigated with respect to the effect of the results on the unused redox reaction time and halogen exchange reaction time. The detected fluorescence emission wavelength of the oil sample having a certain peroxide value as shown in FIG. 2(a) was substantially stable after 10 minutes of the redox reaction, and the detected fluorescence emission wavelength of the oil sample having a certain peroxide value as shown in FIG. 2(b) was substantially stable after 5 minutes of the halogen exchange reaction. Therefore, the detection time was defined as 5 minutes of halogen exchange after 10 minutes of oxidation-reduction.
Third, test of reproducibility
In order to examine the reproducibility of the method, experiments were conducted to examine the reproducibility of the fluorescence signals detected by a plurality of sets of the same synthetic oleylamine iodide diluted solutions and the reproducibility of the fluorescence signals detected by different synthetic oleylamine iodide diluted solutions. Firstly, taking 6 parts of same oleylamine iodine diluent 1mL, 3 parts of blank, adding 0.22mL of oil sample with certain peroxide value into 3 parts of the oleylamine iodine diluent, reacting for 10 minutes, and respectively adding 1mL of CsPbBr3The toluene solution, the fluorescence emission wavelength reproducibility is shown in FIG. 3 (a). It can be seen that the detected fluorescence spectrogram patterns of the oil products with the same peroxide value are basically consistent, and the good reproducibility is shown.
And secondly, the reproducibility of the fluorescence signals detected by the oleylamine iodine diluent synthesized in different batches is shown in the experimental result of fig. 3(b), and the experimental result shows that the oleylamine iodine diluent synthesized in different batches has better reproducibility of the fluorescence signals detected by the oleylamine iodine diluent with different peroxide values.
Interference test
To examine the selectivity of this method, an interference test was also performed before the actual sample analysis. In the experiment, oleic acid salt of some metals and the like are respectively selected for carrying out interference experiments. When interference experiments are carried out, a trace amount of interference substances are added into an oil sample with a certain peroxide value, the mixture is subjected to ultrasonic mixing, then the mixture reacts with 1mL of 2.5mmol/L oleylamine iodine diluent for 10 minutes, and 1mL of CsPbBr is added3Toluene solution, and fluorescence detection was performed after 5 minutes.
The spectrum obtained by the interference test is shown in FIG. 4. It can be seen from the figure that the addition of the interfering oleate causes a slight shift in wavelength due to the presence of oleate (peroxidizing substance) in the oleate, whereas the metal cations, other than copper ions, cause a greater shift in the fluorescence emission wavelength, without significant interference from other cations. Because the normal edible oil basically does not contain copper ions, the method has higher selectivity for measuring the peroxide value of the edible oil.
Fifth, determination of sensitivity and Linear Range
In order to examine the sensitivity and linear range of the method, standard oil samples with peroxide values ranging from 0 to 0.6g/100g were tested by the method. The preparation of the standard oil sample comprises the following steps: mixing the fried oil product with high over oxidation value with toluene solution according to volume ratio of 0:10, 1:9, 2:8, 3:7, 4:6, 5:5, 6:4 and 7:3, measuring oxidation values of 8 standard oil samples according to national standard GB5009.227-2016 (determination of peroxide value in food) for marking, accurately transferring 0.22mL standard oil sample to react with 1mL 2.5mmol/L iodoxylin solution for 10 minutes during measurement, adding 1mL CSPBBr3Toluene solution, and fluorescence detection was performed after 5 minutes.
The obtained fluorescence spectra and the linear relationship are shown in FIGS. 5(a) and 5 (b). It can be seen from FIG. 5a that as the peroxide value increases, the fluorescence emission wavelength gradually decreases, and the color gradually changes from red to yellow-green. FIG. 5b shows that the method has good linear response in the peroxide value range of 0-0.6g/100g when the peroxide value is measured by the method, and R is2Reaching 0.997, which shows that the method can be completely applied to the peroxide value measurement of the actual edible oil.
Sixthly, verifying reliability
In order to examine the reliability of this method, the results of the experiment were shown in FIG. 8, in which the peroxide values of 6 different edible oils were measured by the titration method of GB/T5009.227-2016 as a control. The result data shows that the method is basically consistent with the national standard determination method and has higher reliability. Compared with the defects of large dosage, complexity and long measuring time of the traditional national standard method, the method can realize the rapid detection and analysis of the sample, thereby judging whether the oil product is qualified on site and achieving the purpose of rapidly, simply and conveniently analyzing the peroxide value of the edible oil.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims and their equivalents.

Claims (9)

1. A method for rapidly determining the peroxide value of edible oil is characterized by comprising the following steps:
1) oxidation-reduction reaction: performing redox reaction on oleylamine iodine and peroxide in an oil sample to be detected;
2) halogen exchange reaction: mixing the unoxidized iodide ions obtained in the step 1) with the quantum dots CsPbBr3Performing halogen exchange reaction to obtain a halogen exchange reaction solution CsPbBrmI3-mWherein m is less than or equal to 3;
3) and (3) qualitative detection: comparing the halogen exchange reaction solution in the step 2) with a peroxide value colorimetric card, and determining whether the peroxide value exceeds the standard;
4) and (3) quantitative detection: constructing a fluorescence visualization sensing mode by utilizing the correlation between the m value and the wavelength shift value of the fluorescence emission peak, and determining the peroxide value of the halogen exchange reaction solution in the step 2) by using a molecular fluorescence spectrometry.
2. The method for rapidly determining the peroxide value of the edible oil according to claim 1, wherein the method comprises the following steps: the redox reaction time is not less than 10 minutes, and the halogen exchange reaction time is not less than 5 minutes.
3. The method for rapidly determining the peroxide value of the edible oil according to claim 1, wherein the step 1) comprises the following steps:
heating iodine simple substance and oleylamine at a molar ratio of 1mmol to 3-5 mmol under stirring for reaction, firstly heating to 110-130 ℃, then continuing heating to 190-210 ℃, stopping heating, and cooling; adding an organic solution for dilution to obtain an oleylamine iodine solution, and sealing and storing in a dark place; and (4) pumping the oil sample to be detected to react with the oleylamine iodide solution, and uniformly shaking to ensure that the reaction is complete.
4. The method of claim 1A method for rapidly determining the peroxide value of edible oil is characterized by comprising the following steps: the step 2) CsPbBr3The quantum dot is a quantum dot for fluorescence detection, and the shape of the quantum dot is a nanocrystalline cube.
5. The method for rapidly determining the peroxide value of the edible oil according to claim 1, wherein the step 2) comprises the following steps:
①, preparing cesium oleate, namely adding a cesium precursor into an octadecene solution dissolved with oleic acid, stirring and heating to 110-160 ℃ to completely dissolve the precursor, wherein the volume ratio of octadecene to oleic acid is 16: 1;
② preparing lead bromide precursor, adding lead bromide into octadecene solution dissolved with oleic acid and oleylamine, heating to 110-160 ℃ under stirring, wherein the volume ratio of octadecene to oleic acid to oleylamine is 10:1: 1;
③ Synthesis of CsPbBr by thermal injection3Extracting the cesium precursor solution in the step ①, quickly injecting the cesium precursor solution into the lead bromide precursor solution in the step ②, quickly placing the cesium precursor solution and the lead bromide precursor in an ice-water bath with the mol ratio of 1mmol to 3-4 mmol, shaking the cesium precursor solution and the lead bromide precursor without stopping, centrifugally extracting the product, discarding the supernatant, adding the organic solution again, centrifuging the organic solution again, and taking the supernatant to obtain CsPbBr3A saturated solution of (a);
④ mixing CsPbBr3Diluting the saturated solution, and adding the diluted saturated solution into the solution reacted in the step 1) to perform halogen exchange reaction.
6. The method for rapidly determining the peroxide value of the edible oil according to claim 1, wherein the method comprises the following steps: and 3) placing the halogen exchange reaction solution under an ultraviolet lamp to observe the fluorescence of the halogen exchange reaction solution, and comparing and judging the fluorescence with a peroxide value colorimetric card.
7. The method for rapidly determining the peroxide value of the edible oil according to claim 1, wherein the method comprises the following steps: in the step 4), a linear equation y is set to 0.0048x by using the m value and the wavelength shift value of the fluorescence emission peak, wherein y is the peroxide value of the edible oil, and x is the wavelength shift value of the fluorescence emission peak, the halogen exchange reaction solution is subjected to molecular fluorescence spectrum analysis, the emission wavelength of the halogen exchange reaction solution is measured, and the halogen exchange reaction solution is substituted into the linear equation to obtain the peroxide value.
8. The method for rapidly determining the peroxide value of the edible oil according to claim 1, wherein the method comprises the following steps: the step 3) adopts CsPbBr attached with peroxide value colorimetric card3Or the oleylamine iodine headspace bottle contains the halogen exchange reaction solution.
9. The method for rapidly determining the peroxide value of the edible oil according to claim 1, wherein the method comprises the following steps: the dosage ratio of the oil sample to be detected to the oleylamine iodide is 0.2-0.25 mL to 2.5 mmol.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006177778A (en) * 2004-12-22 2006-07-06 Kikkoman Corp Deterioration measuring method of oil and fat
JP4096108B2 (en) * 2004-03-22 2008-06-04 有限会社大分Ｔｌｏ Method for measuring the amount of peroxide in cooking oil
CN102706872A (en) * 2012-06-13 2012-10-03 安徽省农业科学院农产品加工研究所 Combined reagent for detecting peroxide value of edible oil and fat and detection method thereof
CN105241846A (en) * 2014-07-11 2016-01-13 马井芳 Method of detecting peroxide value of liquid-phase edible oil

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4096108B2 (en) * 2004-03-22 2008-06-04 有限会社大分Ｔｌｏ Method for measuring the amount of peroxide in cooking oil
JP2006177778A (en) * 2004-12-22 2006-07-06 Kikkoman Corp Deterioration measuring method of oil and fat
CN102706872A (en) * 2012-06-13 2012-10-03 安徽省农业科学院农产品加工研究所 Combined reagent for detecting peroxide value of edible oil and fat and detection method thereof
CN105241846A (en) * 2014-07-11 2016-01-13 马井芳 Method of detecting peroxide value of liquid-phase edible oil

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
利用THz时域谱技术和支持向量机回归法快速测定食用油的过氧化值和酸价;李向军 等;《中国粮油学报》;20100228;第25卷(第2期);全文 *
碘量法测定食用油中过氧化值的试剂影响;宋楠;《职业与健康》;20071231;第23卷(第23期);全文 *

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