CN102353667B - Method for detecting content of benzoyl peroxide in flour - Google Patents
Method for detecting content of benzoyl peroxide in flour Download PDFInfo
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- CN102353667B CN102353667B CN 201110186681 CN201110186681A CN102353667B CN 102353667 B CN102353667 B CN 102353667B CN 201110186681 CN201110186681 CN 201110186681 CN 201110186681 A CN201110186681 A CN 201110186681A CN 102353667 B CN102353667 B CN 102353667B
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- benzoyl peroxide
- flour
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- color
- starch
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Abstract
The invention discloses a method for detecting the content of benzoyl peroxide in flour. The method comprises the following steps of adding an organic solvent into flour, fully stirring, carrying out immersion to obtain benzoyl peroxide extract, carrying out centrifugation of the benzoyl peroxide extract to obtain supernatant liquid, putting the supernatant liquid into a colorimetric pipe, adding a potassium iodide solution into the colorimetric pipe, adjusting a pH value of the mixed solution in the colorimetric pipe to a pH value of 2 by strong acid, placing the colorimetric pipe in the shadow until a reaction is balanced; adding a starch indicator into the colorimetric pipe, adding water into the colorimetric pipe for dilution of the mixed solution in the colorimetric pipe, and comparing a color of the diluted solution in the colorimetric pipe with colors of a standard colourimetric card to determine the content of benzoyl peroxide. The method is easy for operation, does not need a high-priced apparatus, reduces a detection cost and detection time, has low requirements for detection persons and a detection environment, can realize on-site detection, and is suitable for on-site analysis and large-area screening work.
Description
Technical field
The detection method of Determination of benzoyl peroxide in wheat in a kind of flour.
Background technology
Benzoyl peroxide is a kind of white powder, is insoluble in water, is soluble in the organic solvents such as ethanol, acetone, benzene, chloroform, ether, is a kind of high response oxidation material.Therefore its strong oxidizing property brightens and antisepsis flour, is used as a kind of flour whitening agent and modifying agent.Benzoyl peroxide can destroy the nutrition of flour; cause the natural components such as xenthophylls, the carotenoid forfeiture in the flour; and the benzoyl peroxide of excessive amount; short-term can make the people produce the intoxicating phenomenons such as nauseating, dizzy, neurasthenia, and long-term excessive edible meeting causes serious infringement to liver.
A plurality of ministries and commissions such as China Ministry of Public Health were at formal issue bulletin on March 1st, 2011, and requirement forbade adding whitening agent in Flour production since May 1.Detrmination of Benzoyl Peroxide is mainly the methods such as vapor-phase chromatography, liquid phase chromatography, spectrophotometric method in the existing flour.These methods are owing to complex operation, and detection time is long, use instrument expensive, require high reason to be difficult to carry out at the scene to operating personnel.
Summary of the invention
The technical problem to be solved in the present invention provides the detection method of Determination of benzoyl peroxide in wheat in a kind of flour.
For solving the problems of the technologies described above, the technical solution used in the present invention may further comprise the steps:
(1) flour is placed beaker, add organic solvent, fully stir and soak, obtain the extract of benzoyl peroxide, organic solvent is 95% ethanol (V/V) or absolute ethyl alcohol, and the consumption of described organic solvent is that every 1g flour needs the 2ml organic solvent.
(2) extract of described benzoyl peroxide is put into centrifuge tube, centrifugal 5-20 minute, centrifugal speed was 1000-4000rpm, obtains supernatant liquor.
(3) getting described supernatant liquor and put into color comparison tube, add the liquor kalii iodide of 100g/L, is 2 with strong acid for adjusting pH value, places shady place to molecular balance, and the consumption of described liquor kalii iodide is that the described supernatant liquor of every 1ml needs the 0.05-0.1ml liquor kalii iodide.
Strong acid is hydrochloric acid, sulfuric acid or phosphoric acid.
(4) starch indicator of adding 10g/L in the color comparison tube of step (3), the consumption of described starch indicator is that every 1ml supernatant liquor needs the 0.1-0.2ml starch indicator.
The preparation method of starch indicator is: soluble starch is transferred to thin pasty state with cold water, inject while stirring boiling water, fully stir the boiling water of adding starch to being transparence, place cooling, obtain starch indicator, the total amount of used cold water and boiling water is that every 1g soluble starch needs 100ml.
(5) liquid in the color comparison tube in the dilute with water step (4), dilute strength are to be diluted to 5-10ml after the described supernatant liquor of every 1ml adds potassium iodide, adjusting pH value, adding starch indicator;
Color and the standard color comparison card that (6) will dilute liquid in the rear color comparison tube compare, obtain the content of benzoyl peroxide, the solid colour of the color of liquid and a certain standard color comparison card in described color comparison tube, illustrate that then benzoyl peroxide concentration equates with the concentration of the benzoyl peroxide of this standard color comparison card representative in the color comparison tube, if color between two standards, is then got the arithmetic mean of two standards.
The method for making of standard color comparison card is: the flour that will be added with the variable concentrations benzoyl peroxide is by testing with step of the present invention (1) to the identical method utilization of step (5) and the identical data of the present invention and instrument, record the color of liquid in the final color comparison tube, take described color as template, make standard color comparison card with the method for printing.
The present invention utilizes the oxidation-reduction quality of benzoyl peroxide, by visual colorimetry the benzoyl peroxide in the flour is carried out quantitative and semi-quantitative and measures.It is as follows that it detects principle:
(C
6H
5CO)
2O
2 + 2H
+ + 2I
- = I
2 + 2C
6H
5COOH
Under acid condition, benzoyl peroxide oxidation KI generates I
2, I
2Generate blue complex, the depth of complex compound color and I with starch reaction
2Concentration relevant, the depth of observing color with eyes by the tester is measured the content of benzoyl peroxide in the flour.Than the spectrophotometric method that adopts this reaction principle, owing to not using the relatively costly spectrophotometer of price, need not correct instrument, without cyclic washing and rinse cuvette, without the drawing curve, so greatly saved testing expense, reduced minute, reduced the requirement to tester and test environment, very suitable on-the site analysis and large-area screening are a kind of easy rapid assay methods.
Potassium iodide has multiple action in chromogenic reaction.Effect one: as reactant.As reactant, it is excessive that potassium iodide should keep, and when the potassium iodide consumption was less, the benzoyl peroxide reaction not exclusively.Effect two: reduce I
2Volatilization.In order to increase I
2At Stability in solution, reduce I
2The impact that causes of volatilization, need to add excessive potassium iodide, form stable I
3 -Reaction equation is as follows:
I
2 + I
- = I
3 -
Effect three: be conducive to the chromogenic reaction to iodine and starch.When without I
-The time, the sensitivity of colour developing.When the potassium iodide consumption was more, with increasing of potassium iodide consumption, the blue process that becomes purple appearred in solution.So the invention provides suitable excessive liquor kalii iodide consumption.
Work as I
2When mutually checking with starch, if the concentration of ethanol is higher, can greatly reduce the mutually sensitivity of check.When the concentration of ethanol greater than 50%(V/V) time, I
2Do not develop the color with starch.Because the present invention uses absolute ethyl alcohol or 95% ethanol (V/V) as extraction agent, so after dripping starch indicator, do not observe blueness, work as I
2Concentration can only observe I when higher
2Yellow.Because I
2Yellow very shallow, and human eye is not sharp to yellow, in order to improve the sensitivity of detection, the method that the present invention takes water that extract is diluted is removed ethanol to the impact of colour developing, makes test fluid be blue.But excessive extension rate can make the color of test solution excessively shallow.Consider the impact of two aspects, the invention provides suitable extension rate.
The beneficial effect that adopts technique scheme to produce is: the present invention is simple to operate, do not use expensive instrument, reduced testing cost and detection time, lower to the requirement of testing staff and testing environment, Site Detection be can realize, on-the site analysis and large-area screening are suitable for.
Embodiment
Embodiment 1:
(1) gets 5g flour and place beaker, add the ethanol (V/V) of 10ml95%, fully stir and soak, obtain the extract of benzoyl peroxide.
(2) extract of described benzoyl peroxide is put into centrifuge tube, centrifugal 5 minutes, centrifugal speed was 4000rpm, obtains supernatant liquor.
(3) getting the 2ml supernatant liquor and put into color comparison tube, add the liquor kalii iodide of 0.1ml100g/L, is 2 with the salt acid for adjusting pH value, places shady place reaction 20 minutes.
(4) starch indicator of adding 0.2ml10g/L in the color comparison tube of step (3).
The preparation method of starch indicator is: get the 1g soluble starch and transfer to thin pasty state with cold water, inject while stirring boiling water, fully stir the boiling water of adding starch to being transparence, place cooling, obtain starch indicator, the total amount of used cold water and boiling water is 100ml.
(5) liquid in the middle color comparison tube of dilute with water step (4) is to 10ml.
Color and the standard color comparison card that (6) will dilute liquid in the rear color comparison tube compare, and the content that obtains benzoyl peroxide is 0.1g/kg.
If the solid colour of the color of liquid and a certain standard color comparison card in the color comparison tube, illustrate that then benzoyl peroxide concentration equates with the concentration of the benzoyl peroxide of this standard color comparison card representative in the color comparison tube, if color between two standards, is then got the arithmetic mean of two standards.
The method for making of standard color comparison card is: the flour that will be added with the variable concentrations benzoyl peroxide is by testing with step of the present invention (1) to the identical method utilization of step (5) and the identical data of the present invention and instrument, record the color of liquid in the final color comparison tube, take described color as template, make standard color comparison card with the method for printing.
Embodiment 2:
(1) gets 5g flour and place beaker, add the absolute ethyl alcohol of 10ml, fully stir and soak, obtain the extract of benzoyl peroxide.
(2) extract of described benzoyl peroxide is put into centrifuge tube, centrifugal 20 minutes, centrifugal speed was 1000rpm, obtains supernatant liquor.
(3) getting the 2ml supernatant liquor and put into color comparison tube, add the liquor kalii iodide of 0.2ml100g/L, is 2 with the sulphur acid for adjusting pH value, places shady place reaction 10 minutes.
(4) starch indicator of adding 0.4ml10g/L in the color comparison tube of step (3).
(5) liquid in the middle color comparison tube of dilute with water step (4) is to 20ml.
Color and the standard color comparison card that (6) will dilute liquid in the rear color comparison tube compare, and the content that obtains benzoyl peroxide is 0.08g/kg.
Other steps are with embodiment 1.
Embodiment 3:
(1) gets 5g flour and place beaker, add the absolute ethyl alcohol of 10ml, fully stir and soak, obtain the extract of benzoyl peroxide.
(2) extract of described benzoyl peroxide is put into centrifuge tube, centrifugal 10 minutes, centrifugal speed was 3000rpm, obtains supernatant liquor.
(3) getting the 2ml supernatant liquor and put into color comparison tube, add the liquor kalii iodide of 0.15ml100g/L, is 2 with the phosphorus acid for adjusting pH value, places shady place reaction 15 minutes.
(4) starch indicator of adding 0.3ml10g/L in the color comparison tube of step (3).
(5) liquid in the middle color comparison tube of dilute with water step (4) is to 15ml.
Color and the standard color comparison card that (6) will dilute liquid in the rear color comparison tube compare, and the content that obtains benzoyl peroxide is 0.06g/kg.
Other steps are with embodiment 1.
Claims (4)
1. the detection method of Determination of benzoyl peroxide in wheat in the flour is characterized in that may further comprise the steps:
(1) flour is placed beaker, add organic solvent, fully stir and soak, obtain the extract of benzoyl peroxide, organic solvent is 95% ethanol or absolute ethyl alcohol, and the consumption of described organic solvent is that every 1g flour needs the 2ml organic solvent;
(2) extract of described benzoyl peroxide is put into centrifuge tube, centrifugal 5-20 minute, centrifugal speed was 1000-4000rpm, obtains supernatant liquor;
(3) getting described supernatant liquor and put into color comparison tube, add the liquor kalii iodide of 100g/L, is 2 with strong acid for adjusting pH value, places shady place to molecular balance, and the consumption of described liquor kalii iodide is that the described supernatant liquor of every 1ml needs the 0.05-0.1ml liquor kalii iodide;
(4) starch indicator of adding 10g/L in the color comparison tube of step (3), the consumption of described starch indicator is that every 1ml supernatant liquor needs the 0.1-0.2ml starch indicator;
(5) liquid in the color comparison tube in the dilute with water step (4), dilute strength are to be diluted to 5-10ml after the described supernatant liquor of every 1ml adds potassium iodide, adjusting pH value, adding starch indicator;
Color and the standard color comparison card that (6) will dilute liquid in the rear color comparison tube compare, obtain the content of benzoyl peroxide, the solid colour of the color of liquid and a certain standard color comparison card in described color comparison tube, illustrate that then benzoyl peroxide concentration equates with the concentration of the benzoyl peroxide of this standard color comparison card representative in the color comparison tube, if color between two standards, is then got the arithmetic mean of two standards.
2. the detection method of Determination of benzoyl peroxide in wheat in a kind of flour as claimed in claim 1 is characterized in that, described strong acid is hydrochloric acid, sulfuric acid or phosphoric acid.
3. the detection method of Determination of benzoyl peroxide in wheat in a kind of flour as claimed in claim 1, it is characterized in that, the preparation method of described starch indicator is: soluble starch is transferred to thin pasty state with cold water, inject while stirring boiling water, fully stir the boiling water of adding starch to being transparence, place cooling, obtain starch indicator, the total amount of used cold water and boiling water is that every 1g soluble starch needs 100ml.
4. the detection method of Determination of benzoyl peroxide in wheat in a kind of flour as claimed in claim 1, it is characterized in that, the method for making of standard color comparison card is: the flour that will be added with the variable concentrations benzoyl peroxide by with claim 1 in step (1) identical data and instrument to the identical method utilization of step (5) and the claim 1 test, record the color of liquid in the final color comparison tube, take described color as template, make standard color comparison card with the method for printing.
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|---|---|---|---|
| CN 201110186681 CN102353667B (en) | 2011-07-05 | 2011-07-05 | Method for detecting content of benzoyl peroxide in flour |
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|---|---|---|---|
| CN 201110186681 CN102353667B (en) | 2011-07-05 | 2011-07-05 | Method for detecting content of benzoyl peroxide in flour |
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| CN102353667A CN102353667A (en) | 2012-02-15 |
| CN102353667B true CN102353667B (en) | 2013-01-09 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102749325B (en) * | 2012-07-09 | 2014-08-13 | 兰州大学 | Application of 3,3',5,5'-tetramethyl benzidine in detecting benzoyl peroxide added to flour |
| CN103487527A (en) * | 2013-10-11 | 2014-01-01 | 内蒙古出入境检验检疫局检验检疫技术中心 | Method for determining benzoyl peroxide in milk powder and milk powder product |
| CN103792233B (en) * | 2014-03-04 | 2015-11-25 | 河南工业大学 | Pick-up unit and detection method while potassium bromate and benzoyl peroxide in wheat flour |
| CN105044023A (en) * | 2015-08-06 | 2015-11-11 | 黑龙江大学 | Method for quickly detecting content of benzoyl peroxide in flour in nondestructive mode and application thereof |
| CN105928886A (en) * | 2016-04-18 | 2016-09-07 | 浙江省林业科学研究院 | Rapid detection reagent and method for adsorptivity of biomass charcoal material |
| CN106706620B (en) * | 2016-12-15 | 2019-05-03 | 厦门海荭兴仪器股份有限公司 | A kind of benzoyl peroxide rapid detection method |
| CN106872451B (en) * | 2016-12-28 | 2019-10-29 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | The semi-quantitative detection method of benzoyl peroxide in starch-kalium iodide reagent and preparation method thereof, test paper, kit and flour |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1444034A (en) * | 2003-04-28 | 2003-09-24 | 陕西师范大学 | Detection device of benzoperoxide in flour and detection method |
| CN1776409A (en) * | 2005-12-05 | 2006-05-24 | 中国农业大学 | Method for detecting benzoperoxide content of flour |
| CN101210907A (en) * | 2006-12-28 | 2008-07-02 | 天津市食品研究所有限公司 | Wheat flour benzoyl peroxide highly effective liquid phase chromatography detection method |
| CN102004094A (en) * | 2010-09-14 | 2011-04-06 | 陕西师范大学 | Method for detecting content of benzoyl peroxide in flour |
-
2011
- 2011-07-05 CN CN 201110186681 patent/CN102353667B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1444034A (en) * | 2003-04-28 | 2003-09-24 | 陕西师范大学 | Detection device of benzoperoxide in flour and detection method |
| CN1776409A (en) * | 2005-12-05 | 2006-05-24 | 中国农业大学 | Method for detecting benzoperoxide content of flour |
| CN101210907A (en) * | 2006-12-28 | 2008-07-02 | 天津市食品研究所有限公司 | Wheat flour benzoyl peroxide highly effective liquid phase chromatography detection method |
| CN102004094A (en) * | 2010-09-14 | 2011-04-06 | 陕西师范大学 | Method for detecting content of benzoyl peroxide in flour |
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