CN106596526A - Detection method for calcium peroxide content in flour - Google Patents
Detection method for calcium peroxide content in flour Download PDFInfo
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- CN106596526A CN106596526A CN201510694745.7A CN201510694745A CN106596526A CN 106596526 A CN106596526 A CN 106596526A CN 201510694745 A CN201510694745 A CN 201510694745A CN 106596526 A CN106596526 A CN 106596526A
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- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
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- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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Abstract
The invention discloses a detection method for the calcium peroxide content in flour, more particularly to a detection method for determining the calcium peroxide content in flour by using a Fenton reaction, and belongs to the field of analysis and detection. The method comprises: taking a proper amount of a uniform flour sample, extracting with dilute sulfuric acid, carrying out a color reaction under a 35-45 DEG C water bath condition, filtering the sample liquid through a membrane, detecting with an ultraviolet spectrophotometer, and carrying out quantitation through an external standard method. According to the present invention, the method is suitable for the determination of the calcium peroxide content in the flour, is simple and quick, does not interfere with the benzoyl peroxide, and meets the requirements of the analysis method.
Description
Technical field
The invention belongs to analyze detection field, it is related to a kind of detection method of calper calcium peroxide content in flour, more particularly, to a kind of detection method of calper calcium peroxide content in utilization Fenton reaction assay flour.
Background technology
Six ministries and commissions such as on 2 11st, 2011 Ministry of Public Health notify, from 1 day May in 2011, forbid adding benzoyl peroxide, calper calcium peroxide in Flour production, food additive companies must not produce and sell food additive benzoyl peroxide, calper calcium peroxide.And the also no suitable method of the measure of the calper calcium peroxide content in flour, the detection of calper calcium peroxide content is increasingly subject to the concern of people.
Calper calcium peroxide, also known as calcium dioxide, English name Calcium peroxide, white crystals, odorless, tasteless have hygroscopy, molecular formula CaO2, molecular weight 72.08,336 DEG C of fusing point, relative density (water=1) is 2.92, is insoluble in water, insoluble in ethanol, ether, is dissolved in acid, and No. CAS is 1305-79-9.Calper calcium peroxide is used as the quick dry agent of antibacterial, preservative, antacid, oils bleach and closing clay.It is used as additive in the manufacture such as food, dentifrice, cosmetics, it is also possible to make Oxide Cathode Materials.Agriculturally it is used as the Nonpoisonous disinfectant of seed and corn；It is additionally operable to aquaculture, fruit freshness preserving, direct sowing of rice and paper pulp, hair, bleaching of cloth etc.；Seed disinfectant is also served as, medicine manufacture, oils and fatss are bleached and be used as high temperature oxygen agent；It is also used as fishpond oxygenation agent.
Calper calcium peroxide dust is irritant to eye, nose, larynx and respiratory tract., there is Nausea and vomiting etc. in oral stimulating gastrointestinal road.Prolonged and repeated contact causes skin and Eye injury.Research shows, eats the flour meeting stimulating gastrointestinal road containing excessive calper calcium peroxide, cause stomach discomfort, long-term consumption then increase the liver metabolism burden of human body, cause chronic disease.
Fenton reacts：Hydrogen peroxide (H2O2) and ferrous ion Fe2+Mixed solution there is strong oxidizing property, can many known organic compound such as carboxylic acid, alcohol, esters be oxidized to inorganic states, oxidation effectiveness is fairly obvious.
At present, the analysis method of the calper calcium peroxide content reported has：Thermal decomposition method, permanganimetric method, indirect iodometric processes, EDTA methods etc., and these methods are only applicable to the analysis of calper calcium peroxide sterling, can not be used for the detection of calper calcium peroxide in flour.
It is to be reacted using Fenton that the present invention determines the Method And Principle of calper calcium peroxide content, and the hydrogen peroxide in calper calcium peroxide is changed into hydroxyl radical free radical, is reacted using the strong oxidizing property and organicvisualization reagent of hydroxyl radical free radical, so as to the anti-content for releasing calper calcium peroxide.The method is simple to operate, and benzoyl peroxide is not interfered with, and meets analysis method requirement.
The content of the invention
It is an object of the invention to provide in a kind of flour calper calcium peroxide content detection method.
Feature of the present invention includes：
(1) sample pre-treatments：Weigh 1～2g of flour sample (being accurate to 1mg), add 10～15mL, 1% dilute sulfuric acids, vortex 1min, mix on horizontal shaker, shaking reaction 10-15min, pH value of solution is adjusted to 7.0-8.0, plus tertiary effluent is settled to 50mL, 40mL extracting solution is taken after fully mixing to be placed in centrifuge tube, 8000r/min centrifugation 5min, take supernatant 5.00mL in 50mL color comparison tubes, add 0.001mol/L sulfuric acid solution 15-20mL, fully mix, add 0.0005mol/L 1～2mL of methylene blue solution, mix；
(2) chromogenic reaction：0.2～0.3g ferrous sulfate reagents being added in above-mentioned solution, 15～20min being reacted in being immediately placed in 35-45 DEG C of water-bath, is taken out after reaction completely, scale is settled to tertiary effluent, is shaken up, sample liquid crosses 0.45 μm of filter membrane, to be measured；
(3) ultraviolet spectrophotometer colorimetric：Return to zero by reference solution of tertiary effluent, determine light absorption value with 10mm glass or quartz colorimetric utensil at 665nm, be detection；
(4) calculate：External standard calibration curve method is quantitative, and the range of linearity is 0.00～0.50mg, calculates the content of object in sample as follows；
In formula：
X --- the content of determinand in sample, unit are milligrams per kilogram (mg/kg)；
C --- determinand content in the sample solution obtained from standard working curve, unit are milligram (mg)；
M --- sample quality is weighed, unit is gram (g)；
V1--- sample constant volume, unit are milliliter (mL)；
V2--- divide and take supernatant volume, unit is milliliter (mL)；
F --- extension rate；
Result of calculation retains three significant digits；
Beneficial effect：The measure of calper calcium peroxide content in flour is carried out using the method, sample is dissolved by 1% dilute sulfuric acid and the calper calcium peroxide in sample is changed into into hydrogen peroxide, be subsequently adding developer methylene blue solution, added ferrous sulfate reagent and Fenton reactions occur.The hydroxyl radical free radical that Fenton reactions are produced is by developer methylene blue oxidation consumption, so that the color of solution changes, obtains the content of calper calcium peroxide eventually through ultraviolet spectrophotometer colour developing.The inventive method is easy, quick, accurate.The results show the inventive method has preferably repeatability and the response rate for peroxidating calcium catalyst in flour sample.
Peroxidating calcium catalyst is not interfered with containing benzoyl peroxide in laboratory sample.
Figure of description
The standard curve of Fig. 1 calper calcium peroxides and absorbance
Specific embodiment
The present invention will be further described in conjunction with the embodiments, but never in any form the present invention is any limitation as, based on present invention teach that any change for being made or improvement, belong to protection scope of the present invention.
Embodiment 1
Calper calcium peroxide is demarcated：
0.15g (being accurate to 1mg) calper calcium peroxide is accurately weighed, is placed in 250mL conical flasks, add 50mL tertiary effluents, the dissolving of 15mL 2mol/L hydrochloric acid solutions to add 1mL 0.05mol/L MnSO4Solution, uses 0.02mol/L KMnO4Standard solution is titrated to micropowder color, colour-fast in 30s to be terminal.Calibration result, calper calcium peroxide content 64.0%.
Standard reserving solution and working solution
64.0% calper calcium peroxide 156.30mg being taken, adding 1% dilute sulfuric acids of 10mL, vortex 1min reaction 10min to be mixed on horizontal shaker, pH is adjusted to 7.0, is added water and be settled to 100mL, obtain 1000mg/L standard reserving solutions, stepwise dilution obtains the working solution of 0.10mg/L.Standard reserving solution and working solution matching while using.
It is prepared by standard curve：
Above-mentioned working solution 0,1.0,2.0 is drawn respectively, 3.0,4.0,5.0mL in 50mL color comparison tubes, 0.001mol/L sulfuric acid solution 15mL are added, is shaken up, is added 0.0005mol/L methylene blue solution 1mL, shake up, add 0.2g ferrous sulfate reagents, in being immediately placed in 37 DEG C of water-baths, react 15min, take out after reaction, tertiary effluent is settled to scale, shakes up, solution crosses 0.45 μm of filter membrane, returns to zero by reference solution of tertiary effluent, in 665nm (10mm glass cuvette) place's mensuration absorbance.Calper calcium peroxide standard curve absorbance is shown in Table 1.
1 calper calcium peroxide standard curve absorbance of table
With calper calcium peroxide content as abscissa X, absorbance is that vertical coordinate Y draws standard curve, sees accompanying drawing 1.Curvilinear equation is Y=-0.7187X+0.6597, and correlation coefficient is 0.9922.
Embodiment 2：
The determination of detection limit：Calculated using deducting the concentration value corresponding with 0.01 absorbance after blank value as detection limit, detection is limited to 14mg/kg.
Embodiment 3：
Commercially available benzoyl peroxide reagent 1.0002g and 1.0008g are weighed, 1% dilute sulfuric acids of 10mL, vortex 1min is added, mix on horizontal shaker, shaking reaction 10min adjusts pH value of solution to 7.0, plus tertiary effluent water is settled to 50mL, 40mL is taken after fully mixing to be placed in centrifuge tube, 8000r/min centrifugation 5min, take supernatant 5.00mL in 50mL color comparison tubes, add 0.001mol/L sulfuric acid solution 15mL, fully mix, add 0.0005mol/L methylene blue solution 1mL, mix；
0.2g ferrous sulfate reagents are added in above-mentioned solution, in being immediately placed in 37 DEG C of water-baths, 15min is reacted, is taken out after reaction, tertiary effluent is settled to scale, shakes up, and sample liquid crosses 0.45 μm of filter membrane.Return to zero by reference solution of tertiary effluent, at 665nm, 10mm glass cuvette determines its light absorption value respectively 0.6618 and 0.6628, basically identical with blank sample absorbance.If not interfering with to peroxidating calcium catalyst containing benzoyl peroxide in illustrating sample.
Embodiment 4：
The standard substance 4.77mg that the calibrated calcium oxide contents of Jing are 64.0% is weighed, 1% dilute sulfuric acids of 10mL, vortex 1min is added, mix on horizontal shaker, shaking reaction 10min adjusts pH to 7.0, add water and be settled to 50mL, 40mL is taken after fully mixing to be placed in centrifuge tube, 8000r/min centrifugation 5min, take supernatant 5.00mL in 50mL color comparison tubes, add 0.001mol/L sulfuric acid solution 15mL, fully mix, add 0.0005mol/L methylene blue solution 1mL, mix；
0.2g ferrous sulfate reagents are added in above-mentioned solution, in being immediately placed in 37 DEG C of water-baths, 15min is reacted, is taken out after reaction, tertiary effluent is settled to scale, shakes up, and sample liquid crosses 0.45 μm of filter membrane.Return to zero by reference solution of tertiary effluent, 10mm glass cuvette determines its light absorption value at the 665nm.
The content for being computed calper calcium peroxide is 2.60mg, and the response rate is 85.2%.
Embodiment 5：
Commercially available flour 1.0012g is weighed, 1% dilute sulfuric acids of 10mL, vortex 1min is added, mix on horizontal shaker, shaking reaction 10min adjusts pH value of solution to 7.0, plus tertiary effluent water is settled to 50mL, 40mL is taken after fully mixing to be placed in centrifuge tube, 8000r/min centrifugation 5min, take supernatant 5.00mL in 50mL color comparison tubes, add 0.001mol/L sulfuric acid solution 15mL, fully mix, add 0.0005mol/L methylene blue solution 1mL, mix；
0.2g ferrous sulfate reagents are added in above-mentioned solution, in being immediately placed in 37 DEG C of water-baths, 15min is reacted, is taken out after reaction, tertiary effluent is settled to scale, shakes up, and sample liquid crosses 0.45 μm of filter membrane.Return to zero by reference solution of tertiary effluent, at 665nm, it is 0.6681 that 10mm glass cuvette determines its light absorption value, basically identical with blank sample absorbance.Calper calcium peroxide is not contained in the flour.
Embodiment 6：
Weigh above-mentioned negative commercially available flour (sample weighting amount is shown in Table 2), it is separately added into the standard substance that the calibrated calcium oxide contents of Jing are 64.0% (mark-on amount is shown in Table 2), add 1% dilute sulfuric acids of 10mL, vortex 1min, mix on horizontal shaker, shaking reaction 10min, pH value of solution is adjusted to 7.0, plus tertiary effluent is settled to 50mL, 40mL is taken after fully mixing to be placed in centrifuge tube, 8000r/min is centrifuged 5min, supernatant 5.00mL is taken in 50mL color comparison tubes, add 0.001mol/L sulfuric acid solution 15mL, fully mix, add 0.0005mol/L methylene blue solution 1mL, mix；
0.2g ferrous sulfate reagents are added in above-mentioned solution, in being immediately placed in 37 DEG C of water-baths, 15min is reacted, is taken out after reaction, tertiary effluent is settled to scale, shakes up, and sample liquid crosses 0.45 μm of filter membrane.Return to zero by reference solution of tertiary effluent, at 665nm, 10mm glass cuvette determines its light absorption value.
Between 66.9%～69.0%, experimental result is shown in Table 2 to the recovery of standard addition of six groups of experiments.
2 recovery of standard addition experimental result of table
* the quality of calper calcium peroxide, purity 64.0% are added.
Claims (2)
1. in a kind of flour calper calcium peroxide content detection method, it is characterised in that the detection method of described calper calcium peroxide includes：
(1) sample pre-treatments：Flour 1～2g of sample accurately being weighed, being added 10～15mL, 1% dilute sulfuric acids to be vortexed and is mixed extraction, 10～15min is extracted in the shaking on horizontal shaker, then extracting liquid pH value is adjusted to 7.0～8.0, V is settled to tertiary effluent1ML, takes 40mL extracting solution after fully mixing and is placed in centrifuge tube, 8000r/min centrifugation 5min, takes supernatant V2ML in 50mL color comparison tubes adds 0.001mol/L 15～20mL of dilution heat of sulfuric acid, fully mixes, add 1～2mL chromogenic reagent solutions, mix；
(2) chromogenic reaction：0.2g～0.3g ferrous sulfate reagents are added in above-mentioned solution, 15～20min in being immediately placed in 35～45 DEG C of water-baths, is reacted, question response completely, is settled to scale with tertiary effluent, shakes up, and sample liquid crosses 0.45 μm of filter membrane, to be measured；
(3) UV spectrophotometer measuring：Return to zero by reference solution of tertiary effluent, with 10mm glass or quartz colorimetric utensil at the 665nm mensuration absorbance；
(4) calculate：External standard calibration curve method is quantitative, and the range of linearity is 0.00～0.50mg, calculates the content of object in sample as follows；
In formula：
X --- the content of determinand in sample, unit are milligrams per kilogram (mg/kg)；
C --- determinand content in the sample solution obtained from standard working curve, unit are milligram (mg)；
M --- sample quality is weighed, unit is gram (g)；
V1--- sample constant volume, unit are milliliter (mL)；
V2--- divide and take supernatant volume, unit is milliliter (mL)；
F --- extension rate；
Result of calculation retains three significant digits；
(5) detection limit：The detection of the method is limited to 14mg/kg.
2. sample pretreatment process according to claim 1, it is characterised in that in methods described, developer are 0.0005mol/L methylene blue solutions.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109444121A (en) * | 2018-10-16 | 2019-03-08 | 河南工业大学 | The detection kit and detection method of calper calcium peroxide in a kind of flour |
Citations (5)
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| CN102944550A (en) * | 2012-10-15 | 2013-02-27 | 上海谱尼测试技术有限公司 | Detection kit for calcium peroxide in flour and detection method for calcium peroxide |
| CN103196908A (en) * | 2013-02-21 | 2013-07-10 | 孙兴权 | Analysis and detection method for calcium peroxide in wheat flour |
| CN103674939A (en) * | 2012-09-14 | 2014-03-26 | 中国科学院青岛生物能源与过程研究所 | Mimic enzyme test paper for detecting hydrogen peroxide and application thereof |
| CN103983643A (en) * | 2014-06-03 | 2014-08-13 | 河南工业大学 | Kit for rapidly detecting calcium peroxide in wheat flour and detecting method of kit |
| CN103983592A (en) * | 2014-06-06 | 2014-08-13 | 哈尔滨工业大学 | Method for detecting concentration of hydroxyl radicals in solution |
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Patent Citations (5)
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| CN103674939A (en) * | 2012-09-14 | 2014-03-26 | 中国科学院青岛生物能源与过程研究所 | Mimic enzyme test paper for detecting hydrogen peroxide and application thereof |
| CN102944550A (en) * | 2012-10-15 | 2013-02-27 | 上海谱尼测试技术有限公司 | Detection kit for calcium peroxide in flour and detection method for calcium peroxide |
| CN103196908A (en) * | 2013-02-21 | 2013-07-10 | 孙兴权 | Analysis and detection method for calcium peroxide in wheat flour |
| CN103983643A (en) * | 2014-06-03 | 2014-08-13 | 河南工业大学 | Kit for rapidly detecting calcium peroxide in wheat flour and detecting method of kit |
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Non-Patent Citations (3)
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| ABRAHAM NORTHUP等: "Calcium peroxide (CaO2) for use in modified Fenton chemistry", 《JOURNAL OF HAZARDOUS MATERIALS》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109444121A (en) * | 2018-10-16 | 2019-03-08 | 河南工业大学 | The detection kit and detection method of calper calcium peroxide in a kind of flour |
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