CN102706872A - Combined reagent for detecting peroxide value of edible oil and fat and detection method thereof - Google Patents
Combined reagent for detecting peroxide value of edible oil and fat and detection method thereof Download PDFInfo
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- CN102706872A CN102706872A CN2012101950252A CN201210195025A CN102706872A CN 102706872 A CN102706872 A CN 102706872A CN 2012101950252 A CN2012101950252 A CN 2012101950252A CN 201210195025 A CN201210195025 A CN 201210195025A CN 102706872 A CN102706872 A CN 102706872A
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Abstract
The invention discloses a combined reagent for detecting the peroxide value of edible oil and fat and a detection method thereof. The combined reagent comprises a solvent, a reduction reagent and a chromogenic reagent, wherein the solvent is a polar organic solvent for dissolving a sample; the reduction reagent is used for reducing peroxide in the to-be-detected sample; and the oxidized reduction reagent reacts with the chromogenic reagent to produce a colored precipitated complex compound, namely ferric thiocyanate. The invention further discloses the detection method using the combined reagent. The detection method has the benefits that a colorimetry principle is adopted by the combined reagent, and the peroxide value of the to-be-detected sample is detected through reagent discoloration and chroma intercomparison, so that the detection method is simple, convenient and rapid and has high accuracy.
Description
Technical field
The present invention relates to a kind of detection method of peroxide value, relate in particular to a kind of edible oil and fat peroxide value and detect composite reagent and detection method thereof.
Background technology
Edible oil and fat are human diet important component parts, are one of human three big nutrients.Grease owing to receive factor affecting such as air, light, temperature, and is prone to take place autoxidation in storage, thereby produces various superoxide.Peroxide value is the important indicator of peroxide level in the measure oil, and in inspection for food hygiene, peroxide value is an important sanitary index.
Wherein hydroperoxides most importantly also have cyclic peroxide, the condensate of peroxy keypad, hydrogen peroxide etc. in addition.Peroxide value is represented the quantity of the hydroperoxides that the grease autoxidation initial stage forms, and its value is higher, and it is stronger to show that fatty acid carries out the degree of oxidation.When peroxide value begins obviously to raise, shown that grease is oxidized in a large number, the stability of grease reduces, and fatty acid becomes sour.The superoxide that is produced behind the Oxidation of Fat and Oils also can continue oxidized decomposition and cause becoming sour of grease rotten.Because the superoxide behind the Oxidation of Fat and Oils is very complicated, it is also very difficult directly to measure its concrete content.So measure the method for oil peroxidation thing at present all is to measure its indirect content mostly; Promptly utilize the peroxide thing to have the characteristics of oxidisability; Through using certain reductive agent such as hydroiodic acid (HI) etc.; Remove to reduce superoxide, come the content of superoxide in the secondary indication grease at last according to the oxidized amount of reductive agent.The existing method that peroxide value is detected has following several kinds:
Titrimetry: can the oxidation potassium iodide under acid (glacial acetic acid) condition according to superoxide; Thereby separate out iodine; Because of sodium thiosulfate can carry out quantitative reaction with iodine; So the iodine that can separate out with the standard solution titration of sodium thiosulfate, and calculate the peroxide value of grease according to the volume that consumes sodium thiosulfate standard solution.Because the not clear dominance of the volatility titration end-point of the reductibility of used KI reagent, the iodine of separating out and add indicator, make this method operation not only loaded down with trivial details but also be difficult for grasp sooner or later to measuring result's influence.
Spectrophotometric colourimetry: make solution painted thereby generate I2, at last through under the 410nm wavelength, measuring appearance liquid light absorption value and more quantitative with iodine standard serial solution light absorption value according to peroxide oxidation I-in the grease.
Test paper method: test paper method promptly prepares potassium iodide starch paper, and tested oil sample is dropped on it, and the spot diameter is advisable with 2-3mm, can confirm the content degree of peroxide value behind the 2min of dark place placement at room temperature according to the spot change color.This method is consuming time longer, and colour developing is not easy to differentiate.
Immobilized enzyme method: through the preparation of detection hydrogen peroxide test strips, but sample treatment confirms that also detecting requirement can not peracid or mistake alkali.
Summary of the invention
One of technical matters that the present invention will solve provides a kind of edible oil and fat peroxide value and detects composite reagent and detection method thereof; This composite reagent adopts colourimetry principle, through the reagent variable color circumstances in which people get things ready for a trip degree comparison of going forward side by side, to detect the peroxide value of testing sample; Simple and efficient, accuracy rate is high.
The present invention realizes through following technical scheme; The present invention includes solvent, go back original reagent, chromogenic reagent; Said solvent is the polar organic solvent of sample dissolution; The said original reagent of going back is used for reducing the superoxide of testing sample, saidly oxidized goes back original reagent and the chromogenic reagent reaction produces coloured precipitation and complexation thing, and said complex compound is a ferric rhodanate.
Said polar organic solvent remembers according to percent by volume, comprises 60～80% chloroform and 20～40% methyl alcohol.
The said original reagent of going back is remembered by weight percentage, comprises the hydrochloric acid of 80～85% iron protochlorides and 15～20%; The mass concentration of said iron protochloride is 3～4g/L, the volumetric molar concentration 0.1～0.3mol/L of hydrochloric acid.
Said chromogenic reagent is a potassium rhodanide solution, and the mass concentration of said potassium rhodanide is 250～350g/L.
A kind of edible oil and fat peroxide value detects the detection method of composite reagent, may further comprise the steps:
(1) takes by weighing liquid testing sample, use polar organic solvent to dissolve and constant volume;
(2) go back original reagent with dripping in the constant volume solution of step (1), re-use the polar organic solvent constant volume, and at room temperature leave standstill;
(3) solution with step (2) injects on the analysed film, under the natural ventilation condition, dries or drier;
(4) chromogenic reagent is splashed on the analysed film of step (3), and film to be analyzed fully develops the color;
(5) the analysed film reference standard colorimetric card of step (4) through colour developing compared, i.e. the approximate range of decidable testing sample peroxide value.
In the constant volume solution of said step (1), the mass concentration of testing sample is 1～200g/L.
In the said detection method, the volume of going back original reagent that every g testing sample drips is 0.4～50ml, and said volume ratio of going back original reagent and said chromogenic reagent is 1:10～1:13.
Said testing sample if occur solidifying or crystallization manifests, makes it melt to liquid earlier before detection.
The foundation of said standard color comparison card may further comprise the steps:
(a) reduced iron powder is added the dissolving of hydrochloric acid and hydrogen peroxide after, hydrogen peroxide is removed in heating, cooling back dilute with water mixing makes the iron standard reserving solution of 1.0mg/mL;
(b) after the solution that step (a) is made adds said polar organic solvent; The iron standard that makes 10ug/mL is used liquid; Draw the iron standard and use liquid 0,0.2,0.5,1.0,1.5,2.0,2.5,3.0,3.5,4.0mL, be equivalent to iron-holder 0,2,5,10,15,20,25,30,35,40ug respectively, above-mentioned iron standard is used in the liquid add the said original reagent of going back respectively; Use the polar organic solvent constant volume, and at room temperature leave standstill;
(c) solution after will leaving standstill injects respectively on the analysed film, adds chromogenic reagent after the air dry, and analysed film is fully developed the color, and makes standard color comparison card.
Beneficial effect of the present invention is,
1, adopt the method for colorimetric analysis, make easy and simple to handlely, the testing result intuitive is good;
2, used detectable kind is less, is convenient to assembling and carries;
3, detection time is shorter, easy and simple to handle;
4, can simultaneously a plurality of grease samples be developed the color and detect, colour developing evenly, and is convenient and swift, is easy to on-the-spot the detection.
Embodiment
Elaborate in the face of embodiments of the invention down, present embodiment provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment being to implement under the prerequisite with technical scheme of the present invention.
Embodiment 1
The kit of present embodiment comprises solvent, goes back original reagent, chromogenic reagent, stopple coupon, reactor, chromogenic device, syringe, analysed film, standard color comparison card; Reactor is the common response vessel; Chromogenic device has at least one, has four in the present embodiment, and each chromogenic device comprises last siphunculus, lower through-tube, loam cake and the lower cover that is communicated with successively, and last siphunculus is fixed on and covers, and lower through-tube is fixed on down and covers, and analysed film is held between loam cake and the lower cover.
Said solvent is the polar organic solvent of sample dissolution, and the said original reagent of going back is used for reducing the superoxide of testing sample, saidly oxidized goes back original reagent and the chromogenic reagent reaction produces coloured precipitation and complexation thing, and said complex compound is a ferric rhodanate.
Polar organic solvent remembers according to percent by volume, comprises 60% chloroform and 40% methyl alcohol.
Also original reagent is remembered by weight percentage, comprises the hydrochloric acid of 80% iron protochloride and 20%;
The mass concentration of iron protochloride is 3g/L, the volumetric molar concentration 0.1mol/L of hydrochloric acid.
Chromogenic reagent is a potassium rhodanide solution, and the mass concentration of said potassium rhodanide is 250g/L.
The foundation of the standard color comparison card of present embodiment may further comprise the steps:
(a) the 0.1g reduced iron powder is put into the beaker of 100 mL; After adding 10mL hydrochloric acid (10mol/L) and 1mL hydrogen peroxide (percent by volume 30%) dissolving then; Remove excessive hydrogen peroxide after the heated and boiled, move into the 100mL volumetric flask behind the cool to room temperature, be diluted with water to scale; Mixing makes the iron standard reserving solution of 1.0mg/mL;
(b) after the solution that step (a) is made adds said polar organic solvent; The iron standard that makes 10ug/mL is used liquid; Draw the iron standard and use liquid 0,0.2,0.5,1.0,1.5,2.0,2.5,3.0,3.5,4.0mL, be equivalent to iron-holder 0,2,5,10,15,20,25,30,35,40ug respectively, above-mentioned iron standard is used in the liquid add the said original reagent of going back respectively; Use the polar organic solvent constant volume, and at room temperature leave standstill;
(c) solution after will leaving standstill injects respectively on the analysed film, adds chromogenic reagent after the air dry, and analysed film is fully developed the color, and makes standard color comparison card.
The edible oil and fat peroxide value detects the detection method of composite reagent in the present embodiment, may further comprise the steps:
(1) takes by weighing liquid testing sample 0.01g, use polar organic solvent to dissolve and be settled to 5mL, mixing;
(2) get constant volume solution 1 mL of step (1), drip and go back original reagent 0.4ml, re-use polar organic solvent and be settled to 5mL, and at room temperature left standstill 15 minutes;
(3) analysed film is put into reactor; Then the solution of step (2) is injected on the analysed film, under the natural ventilation condition, dry or hair-dryer cold wind dries up, said analysed film is polyvinylidene fluoride microporous filtering film (a F type); Specification is: 25mm, aperture: 0.45um;
(4) analysed film of step (3) is put in the chromogenic device, then chromogenic reagent is splashed in the chromogenic device, guarantee that analysed film is soaked into by chromogenic reagent fully, reaction is more than 10 minutes, and film to be analyzed fully develops the color;
(5) the analysed film reference standard colorimetric card of step (4) through colour developing compared, i.e. the approximate range of decidable testing sample peroxide value.
Embodiment 2
In the present embodiment, polar organic solvent remembers according to percent by volume, comprises 65% chloroform and 35% methyl alcohol.
Also original reagent is remembered by weight percentage, comprises the hydrochloric acid of 85% iron protochloride and 15%;
The mass concentration of iron protochloride is 3.5g/L, the volumetric molar concentration 0.2mol/L of hydrochloric acid.
Chromogenic reagent is a potassium rhodanide solution, and the mass concentration of said potassium rhodanide is 300g/L.
In the step (1) of the detection method of edible oil and fat peroxide value detection composite reagent, take by weighing testing sample 0.05g in the present embodiment; In the step (2), drip and go back original reagent 10ml.
Other embodiments are identical with embodiment 1.
Embodiment 3:
In the present embodiment, polar organic solvent remembers according to percent by volume, comprises 80% chloroform and 20% methyl alcohol.
Also original reagent is remembered by weight percentage, comprises the hydrochloric acid of 83% iron protochloride and 17%;
The mass concentration of iron protochloride is 4g/L, the volumetric molar concentration 0.3mol/L of hydrochloric acid.
Chromogenic reagent is a potassium rhodanide solution, and the mass concentration of said potassium rhodanide is 350g/L.
In the step (1) of the detection method of edible oil and fat peroxide value detection composite reagent, take by weighing testing sample 1g in the present embodiment, in the step (2), drip and go back original reagent 50ml.
Other embodiments are identical with embodiment 1.
Embodiment 4:
In the present embodiment, polar organic solvent remembers according to percent by volume, comprises 70% chloroform and 30% methyl alcohol.
Also original reagent is remembered by weight percentage, comprises the hydrochloric acid of 84% iron protochloride and 16%;
The mass concentration of iron protochloride is 3.6g/L, the volumetric molar concentration 0.25mol/L of hydrochloric acid.
Chromogenic reagent is a potassium rhodanide solution, and the mass concentration of said potassium rhodanide is 330g/L.
In the step (1) of the detection method of edible oil and fat peroxide value detection composite reagent, take by weighing testing sample 0.5g in the present embodiment, in the step (2), drip and go back original reagent 30ml.
Other embodiments are identical with embodiment 1.
Claims (10)
1. an edible oil and fat peroxide value detects composite reagent; It is characterized in that; Comprise solvent, go back original reagent, chromogenic reagent, said solvent is the polar organic solvent of sample dissolution, the said original reagent of going back is used for reducing the superoxide of testing sample; Saidly oxidized go back original reagent and the chromogenic reagent reaction produces coloured precipitation and complexation thing, said complex compound is a ferric rhodanate.
2. edible oil and fat peroxide value according to claim 1 detects composite reagent, it is characterized in that, said polar organic solvent remembers according to percent by volume, comprises 60～80% chloroform and 20～40% methyl alcohol.
3. edible oil and fat peroxide value according to claim 1 detects composite reagent, it is characterized in that the said original reagent of going back is remembered by weight percentage, comprises the hydrochloric acid of 80～85% iron protochlorides and 15～20%; The mass concentration of said iron protochloride is 3～4g/L, the volumetric molar concentration 0.1～0.3mol/L of hydrochloric acid.
4. edible oil and fat peroxide value according to claim 1 detects composite reagent, it is characterized in that said chromogenic reagent is a potassium rhodanide solution, and the mass concentration of said potassium rhodanide is 250～350g/L.
5. the detection method like any edible oil and fat peroxide value detection composite reagent in the claim 1～4 is characterized in that, may further comprise the steps:
(1) takes by weighing liquid testing sample, use polar organic solvent to dissolve and constant volume;
(2) go back original reagent with dripping in the constant volume solution of step (1), re-use the polar organic solvent constant volume, and at room temperature leave standstill;
(3) solution with step (2) injects on the analysed film, under the natural ventilation condition, dries or drier;
(4) chromogenic reagent is splashed on the analysed film of step (3), and film to be analyzed fully develops the color;
(5) the analysed film reference standard colorimetric card of step (4) through colour developing compared, i.e. the approximate range of decidable testing sample peroxide value.
6. detection method according to claim 5 is characterized in that, in the constant volume solution of said step (1), the mass concentration of testing sample is 1～200g/L.
7. detection method according to claim 5 is characterized in that, in the said detection method, the volume of going back original reagent that every g testing sample drips is 0.4～50ml, and said volume ratio of going back original reagent and said chromogenic reagent is 1:10～1:13.
8. detection method according to claim 6 is characterized in that, said testing sample if occur solidifying or crystallization manifests, makes it melt to liquid earlier before detection.
9. detection method according to claim 5 is characterized in that, the foundation of said standard color comparison card may further comprise the steps:
(a) reduced iron powder is added the dissolving of hydrochloric acid and hydrogen peroxide after, hydrogen peroxide is removed in heating, cooling back dilute with water mixing makes the iron standard reserving solution of 1.0mg/mL;
(b) after the solution that step (a) is made adds said polar organic solvent; The iron standard that makes 10ug/mL is used liquid; Draw the iron standard and use liquid 0,0.2,0.5,1.0,1.5,2.0,2.5,3.0,3.5,4.0mL, be equivalent to iron-holder 0,2,5,10,15,20,25,30,35,40ug respectively, above-mentioned iron standard is used in the liquid add the said original reagent of going back respectively; Use the polar organic solvent constant volume, and at room temperature leave standstill;
(c) solution after will leaving standstill injects respectively on the analysed film, adds chromogenic reagent after the air dry, and analysed film is fully developed the color, and makes standard color comparison card.
10. detection method according to claim 5 is characterized in that, said analysed film is the Kynoar filter membrane.
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Cited By (12)
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| CN103901021A (en) * | 2012-12-25 | 2014-07-02 | 中国科学院兰州化学物理研究所 | Kit for rapid identification of waste edible oil |
| CN104390971A (en) * | 2013-07-29 | 2015-03-04 | 衢州市易凡设计有限公司 | Engine oil detection method |
| CN105241846A (en) * | 2014-07-11 | 2016-01-13 | 马井芳 | Method of detecting peroxide value of liquid-phase edible oil |
| CN105241832A (en) * | 2015-10-12 | 2016-01-13 | 天津科技大学 | Grease peroxide value detection method |
| CN106198419A (en) * | 2016-08-03 | 2016-12-07 | 哈尔滨普凡农牧有限公司 | Detect reagent and the method for α, β unsaturated aldehyde content in oil plant or oils and fats |
| CN106525556A (en) * | 2016-10-31 | 2017-03-22 | 百奥森（江苏）食品安全科技有限公司 | Method for detecting acid value and peroxidation value in canned sardines |
| CN107831126A (en) * | 2017-12-14 | 2018-03-23 | 广州傲农生物科技有限公司 | A kind of assay method of oil peroxidation value and its application |
| CN109342418A (en) * | 2018-12-07 | 2019-02-15 | 云南商测质量检验技术服务有限公司 | Peroxide value quick testing reagent and its application method in a kind of food |
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| CN110268261A (en) * | 2017-02-14 | 2019-09-20 | 莎罗雅株式会社 | Percarboxylic acids concentration decision means and the indicator solution prepared for it |
| CN112326640A (en) * | 2019-08-05 | 2021-02-05 | 浙江农林大学 | Test paper for rapidly and directly reading and developing detection of lipid peroxide value, preparation method thereof, preparation method of standard colorimetric card and application thereof |
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Cited By (17)
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| CN103901021A (en) * | 2012-12-25 | 2014-07-02 | 中国科学院兰州化学物理研究所 | Kit for rapid identification of waste edible oil |
| CN103901021B (en) * | 2012-12-25 | 2016-06-29 | 中国科学院兰州化学物理研究所 | A kind of test kit of the waste and old edible oil of quick discriminating |
| CN103245660B (en) * | 2013-05-07 | 2015-09-30 | 浙江大学 | A kind of edible oil and fat determination of POV composite reagent and detection method |
| CN103245660A (en) * | 2013-05-07 | 2013-08-14 | 浙江大学 | Edible oil peroxide value measurement combined reagent and detection method |
| CN104390971A (en) * | 2013-07-29 | 2015-03-04 | 衢州市易凡设计有限公司 | Engine oil detection method |
| CN105241846A (en) * | 2014-07-11 | 2016-01-13 | 马井芳 | Method of detecting peroxide value of liquid-phase edible oil |
| CN105241832A (en) * | 2015-10-12 | 2016-01-13 | 天津科技大学 | Grease peroxide value detection method |
| CN106198419B (en) * | 2016-08-03 | 2018-12-07 | 哈尔滨普凡农牧有限公司 | Detect the reagent and method of alpha, beta-unsaturated aldehyde content in oil plant or grease |
| CN106198419A (en) * | 2016-08-03 | 2016-12-07 | 哈尔滨普凡农牧有限公司 | Detect reagent and the method for α, β unsaturated aldehyde content in oil plant or oils and fats |
| CN106525556A (en) * | 2016-10-31 | 2017-03-22 | 百奥森（江苏）食品安全科技有限公司 | Method for detecting acid value and peroxidation value in canned sardines |
| CN110268261A (en) * | 2017-02-14 | 2019-09-20 | 莎罗雅株式会社 | Percarboxylic acids concentration decision means and the indicator solution prepared for it |
| US11333610B2 (en) | 2017-02-14 | 2022-05-17 | Saraya Co., Ltd. | Percarboxylic acid concentration determination tool and indicator solution used in preparing same |
| CN107831126A (en) * | 2017-12-14 | 2018-03-23 | 广州傲农生物科技有限公司 | A kind of assay method of oil peroxidation value and its application |
| CN109342418A (en) * | 2018-12-07 | 2019-02-15 | 云南商测质量检验技术服务有限公司 | Peroxide value quick testing reagent and its application method in a kind of food |
| CN110146496A (en) * | 2019-05-28 | 2019-08-20 | 厦门大学 | A kind of method of quick measurement edible oil peroxide value |
| CN110146496B (en) * | 2019-05-28 | 2020-04-03 | 厦门大学 | Method for rapidly determining peroxide value of edible oil |
| CN112326640A (en) * | 2019-08-05 | 2021-02-05 | 浙江农林大学 | Test paper for rapidly and directly reading and developing detection of lipid peroxide value, preparation method thereof, preparation method of standard colorimetric card and application thereof |
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Application publication date: 20121003 |