CN109283161A - A kind of method using peroxide value in fluorescent quenching method detection grease - Google Patents
A kind of method using peroxide value in fluorescent quenching method detection grease Download PDFInfo
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- CN109283161A CN109283161A CN201811093143.6A CN201811093143A CN109283161A CN 109283161 A CN109283161 A CN 109283161A CN 201811093143 A CN201811093143 A CN 201811093143A CN 109283161 A CN109283161 A CN 109283161A
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- Prior art keywords
- phthalocyanine
- grease
- derivatives
- peroxide
- peroxide value
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
Abstract
This disclosure relates to which a kind of method using peroxide value in fluorescent quenching method detection grease, is specifically used phthalocyanine as fluorescence photosensitizer, is detected the peroxide value of edible oil to the quantitative quenching ability of phthalocyanine fluorescence using peroxide in grease.Detection range 0.2-20meq/kg, sensitivity 0.2meq/kg.This method avoids existing national standards using organic solvents bring environmental pollutions such as glacial acetic acid isooctane, decreases existing national standard because of detection error caused by using starch reagent.
Description
Technical field
This disclosure relates to which peroxide refers to calibration method in a kind of detection grease, belong to food inspection or chemical analysis technology
Field.
Background
Fat be three big basic nutrients required for the main component and human normal vital movement of edible oil it
One, the fatty acid generated after fat splitting is the most direct energy source of human body, human body daily needed for energy 50-60% or more
Fat is needed to provide.Other than storage and supplying energy, a variety of fatty acid, including linoleic acid, linolenic acid etc. that grease provides
Essential fatty acid, maintain eubolism and in terms of play an important role.
The unsaturated fatty acid not waited containing 10-90% in various edible oils, both human bodies of linolenic and linoleic
Essential fatty acid also belongs to unsaturated fatty acid, and most unsaturated fatty acids contain the conjugated double bond structures of at least two or more, this
It is caused to be easy to be aoxidized by the oxygen in air, unsaturated fatty acid, which is oxidized, can generate peroxide, cause edible oil
Peroxide content gradually increases, this not only declines product special flavour and nutritive value, moreover it is possible to generate other noxious materials and
As the inducible factor of aging, carcinogenic etc., quality and eater's health to edible oil cause to seriously affect.
Unsaturated lipid compound in oil product can occur redox reaction with the oxygen in air and generate peroxide.It crosses
Oxidation number is one of the important indicator of international measurement edible oil quality, it directly reflects the superiority and inferiority of oil quality.Day
Before, the national standard method GB5009.227-2016 that the determination of POV in food oil uses is based on iodometric titration, and this method is wanted
It asks and is tested using chemical titration and potentiometric titration, needed using glacial acetic acid, isooctane and chloroform etc. are as molten
Agent, tests chloroform in the waste liquid of generation and isooctane is not soluble in water, belongs to hazardous waste, processing difficulty is big；In addition it surveys
Examination needs to use starch and potassium iodide as auxiliary reagent and indicator, and the configuration of starch solution is influenced by reagent quality, weight
Renaturation is very poor, and liquor kalii iodide and hypo solution are also easy to oxidize, cannot save for a long time；Chemical titration detection needs
Artificial observation color change is wanted to determine terminal, this has resulted in the presence of artificial subjective error.Thus this national standard method
It is not a very perfect detection method.
Patent 201410822047.6 discloses a kind of method using biological enzyme sensor detection peroxide value, uses
The content of the electrode detection peroxide of hydrogen oxide enzyme production, such method needs to prepare sensing electrode, and needs using biology
Enzyme preparation；The open improvement to national standard method of patent 201210324117.6 replaces chemistry titration using conductivity detection, but
It needs to be operated in glacial acetic acid and isooctane solution；Patent 201310166213.7 discloses a kind of by national standard chemistry point
The method that analysis is converted to test paper analysis, realizes the reduction and colour developing of peroxide on test paper, and test paper method is a kind of quick half
Quantitative method.
Summary of the invention
For background technique, present disclose provides a kind of sides using peroxide value in fluorescent quenching method detection grease
Method.The detection range of method of disclosure is wider, meets the detection of daily consumption oil quality and uses, can reach the test of national standard method
Accuracy.
The disclosure specifically uses following technical scheme:
In the first aspect of the disclosure, application of the phthalocyanine or derivatives thereof in detection grease in peroxide value is provided.
In the second aspect of the disclosure, a kind of method for detecting peroxide value in grease is provided, this method comprises: using
Phthalocyanine or derivatives thereof is quenched quantifying for fluorescence using peroxide in grease, detects edible oil as the photosensitizer that shines
Peroxide value index.
The disclosure third in terms of, provide it is a kind of for detecting the reagent of peroxide value in grease, the reagent be by
Phthalocyanine or derivatives thereof and dimethyl sulfoxide, N, N-dimethylformamide, one of methylene chloride composition.
Compared with the relevant technologies that the present inventor knows, the one of technical solution of the disclosure has following beneficial to effect
Fruit:
The method using peroxide value in fluorescent quenching detection grease of the disclosure avoids the system of complicated electrode sensor
The use of standby and unstable enzyme preparation, also there is better accuracy compared to test paper method.
Disclosed method detection range 0.2-20meq/kg, sensitivity 0.2meq/kg, accuracy are high.This method avoids
Existing national standard decreases existing national standard because using starch using organic solvents bring environmental pollutions such as glacial acetic acid isooctane
Detection error caused by reagent.
Detailed description of the invention
The Figure of description for constituting disclosure a part is used to provide further understanding of the disclosure, the signal of the disclosure
Property embodiment and its explanation for explaining the disclosure, do not constitute the improper restriction to the disclosure.
Fig. 1: the working curve of phosphorus phthalocyanine fluorescent quenching method detection edible oil peroxide value index.
Fig. 2: phosphorus phthalocyanine fluorescent quenching method detects the working curve of micro peroxide in edible oil.
Specific embodiment
It is noted that described further below be all exemplary, it is intended to provide further instruction to the disclosure.Unless another
It indicates, all technical and scientific terms used herein has usual with disclosure person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the disclosure.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation and/or their combination.
As background technique is introduced, detecting peroxide in grease in the prior art, to refer to that calibration method exists certain
Deficiency, in order to solve technical problem as above, the present disclosure proposes a kind of phthalocyanine or derivatives thereof peroxidating in detection grease
Application in value.
The excitation wavelength (330-360nm) of phthalocyanine substance and launch wavelength (680-750nm) not with the excitation of edible oil
Wavelength (250-300nm) and launch wavelength generate interference (350-450nm).During fluorescent quenching, Phthalocyanine structure and mistake
Oxide has better energy transfer efficiency, and peroxide is more effective and rapid to being quenched for phthalocyanine in edible oil, quantitative extent
Good, there is the disadvantages of quantitatively poor in other fluorescers (methylene blue and rhodamine etc.).In addition, its economy and environment friendly are strong
In other fluorescers such as rhodamine and methylene blue.
In one of the disclosure or some specific embodiments, phthalocyanine or derivatives thereof is with four benzo knot of azepine
The phthalocyanine and its derivative of structure, it is contemplated that the environmental problem of metal phthalocyanine and the accuracy of testing result and sensitivity, preferably
Nonmetallic phosphorus phthalocyanine compound, for example, tetraisopropoxide phosphorus phthalocyanine, four benzyloxy phosphorus phthalocyanines, four pyridine oxygroup phosphorus phthalocyanines
Or four octyloxy phosphorus phthalocyanines etc., structure is as follows:
R1、R2、R3、R4The group respectively represented is isopropoxy, benzyloxy, octyloxy or pyridine oxygroup etc..
Further, to further increase detection sensitivity and accuracy, tetraisopropoxide phosphorus phthalocyanine, R are selected1、R2、R3、
R4The group of representative is isopropoxy.
In one of the disclosure or some specific embodiments, grease is vegetable oil, animal oil or microbe-derived
Grease.Vegetable oil such as soybean oil, linseed oil, peanut oil etc., animal oil such as lard, butter, chicken fat etc..
In a typical embodiment of the disclosure, a kind of method for detecting peroxide value in grease, the party are provided
Method includes: to use phthalocyanine or derivatives thereof as luminous photosensitizer, and quantifying for fluorescence is quenched using peroxide in grease, inspection
Survey the peroxide value index of edible oil.
In one of the disclosure or some specific embodiments, method includes the following steps:
(1) detection reagent is prepared
Phthalocyanine or derivatives thereof is dissolved in dimethyl sulfoxide, N in N-dimethylformamide or methylene chloride, is detected
Reagent；
(2) working curve is quantitatively quenched in production
The oil sample containing different content peroxide is added in detection reagent respectively, tests its change in fluorescence,
The change curve of the fluorescence intensity of the oil sample of different content peroxide is obtained, working curve is quantitatively quenched in production；
(3) it detects
Oil sample to be detected is added in detection reagent, its change in fluorescence is tested, obtains fluorescence intensity change curve,
Working curve is quenched according to quantifying in step (2) and obtains the peroxide value of oil sample to be detected.
Further, in step (1), the concentration of phthalocyanine or derivatives thereof is 0.5-5 μm of ol/L in the detection reagent.
Further, in step (2), the volume ratio of the oil sample and detection reagent be (50-500) μ L:(1~
2)mL。
Further, in step (3), the volume ratio of the oil sample and detection reagent be (50-500) μ L:(1~
2)mL。
Further, it in step (3), if encountering the serious oil sample of oxidation, is detected after being diluted.
In a typical embodiment of the disclosure, provide it is a kind of for detecting the reagent of peroxide value in grease,
The reagent is by phthalocyanine or derivatives thereof and dimethyl sulfoxide, N, N-dimethylformamide, and one of methylene chloride forms,
Wherein, the concentration of phthalocyanine or derivatives thereof is 0.5-5 μm of ol/L.
In order to enable those skilled in the art can clearly understand the technical solution of the disclosure, below with reference to tool
The technical solution of the disclosure is described in detail in the embodiment of body.
The preparation of 1 working curve of embodiment
Tetraisopropoxide phosphorus phthalocyanine is dissolved in DMSO solvent, and concentration is 2 μm of ol/L, and selection commodity linseed oil is sample
Product are put into 63 DEG C of baking oven, are passed through air and heat 24 hours, draw oil sample every 4 hours primary, obtained oil sample uses national standard
Method tests peroxide value.Then the above-mentioned oil sample for adding 100 μ L in 2ml, tests it into the phosphorus phthalocyanine DMSO solution of preparation
Change in fluorescence, as shown in Figure 1.As can be seen that the fluorescence intensity of peroxide value and phosphorus phthalocyanine has within the scope of 1-20meq/kg
Good linear relationship, R2Greater than 0.996, standard deviation is less than 5%, compared to constant-current titration in national standard GB5009.227-2016
Detection range be about 0-35meq/KOH, it is contemplated that peroxide value qualification limit value is in 2- as defined in the quality standard of edible oil
5meq/kg, the range of linearity of the disclosure meet the detection of daily consumption oil quality enough and use.Because peroxide concentrations are with oil sample
Concentration dilution changes linearly, if encountering the serious oil sample of oxidation, detects after being diluted.
Embodiment 2
It is a kind of for detecting the reagent of peroxide value in grease, which is by tetraisopropoxide phosphorus phthalocyanine and N, N-diformazan
Base formamide composition, wherein the concentration of tetraisopropoxide phosphorus phthalocyanine is 5 μm of ol/L.
When detecting peroxide value in grease, the reagent is uniformly mixed with oil sample to be detected, tests the change of its fluorescence
Change, wherein the volume ratio of the reagent and oil sample to be detected is (1~2) mL:(50-500 μ L.
Embodiment 3
It is a kind of for detecting the reagent of peroxide value in grease, which is by four pyridine oxygroup phosphorus phthalocyanines and methylene chloride
Composition, wherein the concentration of four pyridine oxygroup phosphorus phthalocyanines is 3 μm of ol/L.
When detecting peroxide value in grease, the reagent is uniformly mixed with oil sample to be detected, tests the change of its fluorescence
Change, wherein the volume ratio of the reagent and oil sample to be detected is (1~2) mL:(50-500) μ L.
Embodiment 4
It is a kind of for detecting the reagent of peroxide value in grease, which is by four benzyloxy phosphorus phthalocyanines and methylene chloride
Composition, wherein the concentration of four benzyloxy phosphorus phthalocyanines is 3 μm of ol/L.
When detecting peroxide value in grease, the reagent is uniformly mixed with oil sample to be detected, tests the change of its fluorescence
Change, wherein the volume ratio of the reagent and oil sample to be detected is (1~2) mL:(50-500) μ L.
Embodiment 5
It is a kind of for detecting the reagent of peroxide value in grease, which is by four octyloxy phosphorus phthalocyanines and methylene chloride group
At, wherein the concentration of four octyloxy phosphorus phthalocyanines is 3 μm of ol/L.
When detecting peroxide value in grease, the reagent is uniformly mixed with oil sample to be detected, tests the change of its fluorescence
Change, wherein the volume ratio of the reagent and oil sample to be detected is (1~2) mL:(50-500) μ L.
6 sensitivity test of embodiment
National standard does not mention the sensitivity of its detection method, therefore the disclosure is quasi- using the test under the conditions of low-peroxide value
True degree illustrates the sensitivity of method of disclosure.
Selection commodity linseed oil is sample, is passed through at 63 DEG C of air and heats 6 hours, measures its peroxidating with national standard method
Value is 4.68, with dimethyl sulfoxide is respectively then that solvent is diluted to 20 times, 15 times, 10 times, 8 times and 7 times, utilizes national standard method
The peroxide value that two constant-current titrations are tested to obtain each dilute solution is 0.21,0.34,0.47,0.58,0.67meq/kg, then
Fluorescent quenching experiment, as a result as shown in fig. 2, it can be seen that under low concentration, fluorescent emission intensity are carried out using above-mentioned solution
Good linear relationship, R still can be maintained with peroxide value2Greater than 0.994, for standard deviation less than 7%, this illustrates disclosure side
The sensitivity of method detection can reach 0.1-0.2meq/kg, can reach the test accuracy of national standard method.
7 detection example of embodiment
Selection commodity edible oil sample is several, and chooses the oil sample after frying, utilizes the method (inspection in embodiment 1
Test agent is the mixed liquor of tetraisopropoxide phosphorus phthalocyanine and DMSO, and concentration is 2 μm of ol/L) and national standard method progress peroxide value
As a result as shown in table 1 below detection carries out difference analysis to two groups of data using SPSS software, the results showed that this two groups of data
Notable difference is not present in 0.05 confidence level, shows that the result of two kinds of detection methods does not have significant difference.
1 method of disclosure of table and national standard method compare some edible oil sample peroxide value test results
Above-described embodiment is the preferable embodiment of the disclosure, but embodiment of the present disclosure is not by above-described embodiment
It limits, made changes, modifications, substitutions, combinations, simplifications under other any spiritual essence and principles without departing from the disclosure,
It should be equivalent substitute mode, be included within the protection scope of the disclosure.
Claims (10)
1. a kind of application of the phthalocyanine or derivatives thereof in detection grease in peroxide value.
2. application as described in claim 1, it is characterized in that: the phthalocyanine is phosphorus phthalocyanine.
3. application as described in claim 1, it is characterized in that: phthalocyanine or derivatives thereof is the phthalocyanine with four benzo structure of azepine
And its derivative；
Further, phthalocyanine or derivatives thereof isWherein, R1、R2、
R3、R4The group respectively represented is isopropoxy, benzyloxy, octyloxy or pyridine oxygroup.
4. application as described in claim 1, it is characterized in that: grease is vegetable oil, animal oil or microbe-derived grease.
5. it is a kind of detection grease in peroxide value method, characterized in that this method comprises: use phthalocyanine or derivatives thereof as
Shine photosensitizer, is quenched using peroxide in grease to quantifying for fluorescence, detects the peroxide value index of edible oil.
6. method as claimed in claim 5, characterized in that method includes the following steps:
(1) detection reagent is prepared
Phthalocyanine or derivatives thereof is dissolved in dimethyl sulfoxide, N in N-dimethylformamide or methylene chloride, obtains detection reagent；
(2) working curve is quantitatively quenched in production
The oil sample containing different content peroxide is added in detection reagent respectively, its change in fluorescence is tested, obtains
Working curve is quantitatively quenched in the change curve of the fluorescence intensity of the oil sample of different content peroxide, production；
(3) it detects
Oil sample to be detected is added in detection reagent, its change in fluorescence is tested, obtains fluorescence intensity change curve, according to
Quantifying in step (2) is quenched working curve and obtains the peroxide value of oil sample to be detected.
7. method as claimed in claim 6, it is characterized in that: in step (1), phthalocyanine or derivatives thereof in the detection reagent
Concentration is 0.5-5 μm of ol/L.
8. method as claimed in claim 6, it is characterized in that: in step (2), the volume ratio of the oil sample and detection reagent
Example is L:(1~2 (50-500) μ) mL.
9. a kind of for detecting the reagent of peroxide value in grease, it is characterized in that: the reagent be by phthalocyanine or derivatives thereof and
Dimethyl sulfoxide, N, N-dimethylformamide, one of methylene chloride composition, wherein the concentration of phthalocyanine or derivatives thereof is
0.5-5μmol/L。
10. reagent as claimed in claim 9, it is characterized in that: phthalocyanine or derivatives thereof is tetraisopropoxide phosphorus phthalocyanine, four benzene first
Oxygroup phosphorus phthalocyanine, four pyridine oxygroup phosphorus phthalocyanines or four octyloxy phosphorus phthalocyanines.
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| CN110412094A (en) * | 2019-06-21 | 2019-11-05 | 广州钰芯传感科技有限公司 | A kind of high temperature resistant interdigital electrode, preparation method and the application of the protection of glass glaze outer surface |
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| CN110412094A (en) * | 2019-06-21 | 2019-11-05 | 广州钰芯传感科技有限公司 | A kind of high temperature resistant interdigital electrode, preparation method and the application of the protection of glass glaze outer surface |
| CN110412094B (en) * | 2019-06-21 | 2021-12-21 | 广州钰芯传感科技有限公司 | High-temperature-resistant interdigital electrode with glass glaze outer surface protection, and preparation method and application thereof |
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| CN109283161B (en) | 2021-04-02 |
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