CN101226139A - Method for chemistry testing potassium bromate in flour, amendment or food - Google Patents

Method for chemistry testing potassium bromate in flour, amendment or food Download PDF

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Publication number
CN101226139A
CN101226139A CNA2008100492049A CN200810049204A CN101226139A CN 101226139 A CN101226139 A CN 101226139A CN A2008100492049 A CNA2008100492049 A CN A2008100492049A CN 200810049204 A CN200810049204 A CN 200810049204A CN 101226139 A CN101226139 A CN 101226139A
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China
Prior art keywords
potassium bromate
sample
organic solvent
flour
light absorption
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CNA2008100492049A
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Chinese (zh)
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白伟
王会君
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Xingtai Science Technology Industry Co Ltd Henan
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Xingtai Science Technology Industry Co Ltd Henan
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Priority to CNA2008100492049A priority Critical patent/CN101226139A/en
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Abstract

The invention discloses a chemical test method of potassium bromate in flour, modifying agent or food, which comprises (1), processing sample composed of adding alkali into sample, heating and ashing, dissolving in water, adding acid to adjust pH at 2-5, moving all solution into a centrifugal pipe, controlling the pH value at 1-2, centrifugally treating and taking supernatant fluid, (2), testing potassium bromate composed of adding the supernatant with oxidant, vibrating and adding organic solvent, vibrating, laying and laminating, using distilled water as blank, using spectrophotometer to check the light absorption value of the organic solvent layer and indicating that the sample contains potassium bromate when the light absorption value is not lower than 0.010. The oxidant is strong one and the organic solvent is non-polar or weak-polar organic one. The invention provides a novel, simple, quick, sensitive and stable method for chemically checking potassium bromate in flour, modifying agent or food.

Description

The chemical detection method of potassium bromate in flour, modifying agent or the food
Technical field
The present invention relates to a kind of detection method of potassium bromate, particularly relate to the chemical detection method of potassium bromate in flour, modifying agent or the food.
Background technology
Potassium bromate is a kind of oxygenant at a slow speed, and potassium bromate once was considered to one of best dough correctives in curing industry, is used in during bread cures, because there is very big problem in the security of potassium bromate, use now has been under an embargo at present.But owing to there is not safe, effective substitute, also have some little manufacturers stealthily to use potassium bromate, therefore, the potassium bromate that how to detect in flour, modifying agent, the food has great importance.At present very perfect to the qualitative-and-quantitative method of pure product potassium bromate in the world, but in the mixed system of complexity such as flour improver, flour, the method for testing of potassium bromate and imperfection.Such as: the method for qualitative and quantitative detection basically identical of bromate in the flour that U.S. AACC-48-42 and AOAC 956.03 release, wherein quilitative method is with flour powder plate acidifying KI solution development process (showing the stain method), this method is the general qualitative checking method of oxygenant, be not the detection method of potassium bromate special use, will be because of there be CaO in its final detection result in the flour 2Wait the oxygenant material of the legal use of other energy and cause erroneous judgement.Another measures flour now, modifying agent, the method of potassium bromate is the chromatography of ions in the food, the chromatography of ions need be used instrumentation, but equipment investment is bigger, just make the popularization and the application of this method have certain limitation, at present domestic most testing agencies are this equipment not, do not possess the ability of using the sulfate by ion chromatography potassium bromate, and can't operate especially domestic flour and food enterprise, flour enterprise can not detect whether contain potassium bromate in the modifying agent at any time, whether food enterprise contains potassium bromate in the detection faces powder raw material at any time, will cause big hidden danger to the market standard of potassium bromate forbidding.The method that does not also have at present potassium bromate in other easy, quick, sensitive, stable detection flour, modifying agent, the food.
Summary of the invention
The present invention seeks to overcome the deficiency of present technology, a kind of novelty, easy, quick, sensitive, stable method of potassium bromate in flour, modifying agent or the food being carried out chemical detection are provided.
For achieving the above object, the technology scheme of determining of the present invention is: the chemical detection method of potassium bromate in a kind of flour, modifying agent or the food may further comprise the steps:
1), the processing of sample: sample heats ashing after adding alkali, adds acid treatment after water-soluble the separating, and pH value is controlled at 1~2, the centrifuging and taking supernatant;
2), potassium bromate is measured: above-mentioned supernatant is added oxygenant, and the vibration back adds organic solvent, again vibration, placing layering, is blank with distilled water, detects the light absorption value of organic solvent layer with spectrophotometer, when light absorption value more than or equal to 0.010 the time, promptly think and contain potassium bromate in the sample;
Described oxygenant is a strong oxidizer;
Described organic solvent is the organic solvent of nonpolar or low pole.
The chemical detection method of potassium bromate in flour, modifying agent or the food preferably includes following steps:
1), the processing of sample: after sample adds alkali heating charing earlier complete, be heated to 500~600 ℃ of complete ashing then, water-soluble the separating in cooling back, adding the diluted acid adjust pH is 3~4, complete soln moves in the centrifuge tube, the pH value is controlled at 1~1.5, the centrifuging and taking supernatant;
2), potassium bromate is measured: above-mentioned supernatant adds oxygenant, the vibration back adds organic solvent, vibration again, place layering, organic solvent layer filters in cuvette with absorbent cotton, under 410nm, with spectrophotometric instrumentation light absorption value, is blank with distilled water, when light absorption value more than or equal to 0.010 the time, can think and contain potassium bromate in the sample;
Described alkali is potassium hydroxide or NaOH;
Described diluted acid is sulfuric acid, nitric acid or hydrochloric acid;
Described oxygenant is saturated chlorine water, potassium permanganate, potassium dichromate or hydrogen peroxide;
Described organic solvent is phenixin, chloroform, benzene or toluene.
The chemical detection method of potassium bromate in flour, modifying agent or the food most preferably may further comprise the steps:
1), sample thief hydro-oxidation sodium powder, put into evaporating dish behind the mixing, charing on electric furnace, after the charing fully, evaporating dish is transferred in the muffle furnace, in 520 ℃ of following ashing, after the ashing fully, cooling is with the water-soluble sample of separating after the ashing of 3-5ml, the sulfuric acid solution 1-2ml that adds 2mol/l again is 50-60 ℃ of low-grade fever, solution is transferred in the centrifuge tube, and respectively with low amounts of water and a small amount of 2mol/l acid solution flushing evaporating dish, washing lotion all changes in the 10ml centrifuge tube then, pH value is controlled at about 1, and the centrifuging and taking supernatant is standby.
2), potassium bromate is measured: above-mentioned supernatant is transferred in the separating funnel, dropwise drip saturated chlorine water, the vibration back adds phenixin, and layering is placed in vibration, organic solvent layer filters in cuvette with absorbent cotton, under 410nm,, be blank with distilled water with spectrophotometric instrumentation light absorption value, when light absorption value more than or equal to 0.010 the time, can think and contain potassium bromate in the sample.
Described sample thief wheat flour is in this way got the 50-200 gram, preferably with 100 grams; Modifying agent is got the 1-3 gram in this way, preferably with 2 grams; Food such as steamed bun, noodles, bread are got the 100-200 gram in this way, preferably with 150 grams.
The method of potassium bromate replaces chromatography of ions qualitative detection with chemical method in detection flour provided by the invention, modifying agent or the food.We's ratio juris is that potassium bromate at high temperature is decomposed into bromide ion, and the bromide ion strong oxidizer is oxidized to bromine simple substance under the acid condition, bromine simple substance be dissolved in nonpolar or weakly polar organic solvent in develop the color, measure absorbance down with spectrophotometer 410nm.This invention can merge with state compulsory standard, and state compulsory standard is the BrO in the test sample 3 -Find by a large amount of tests, bromide that flour itself contains and bromate are very low, chromogenic reaction is not exerted an influence, so all should being external interpolation, the source of the detected bromine of chromogenic reaction introduces, and bromide does not all have improved effect to all kinds of flour and flour-made food, just can not become adding ingredient yet, its unique source is the bromate that adds, in addition, self partly or entirely is converted into bromide under the oxidation of bromate in flour-made foods such as bread, so the present invention more can accurately judge whether added bromate in its process than the method for directly measuring bromate.Actual conditions in conjunction with China's flour improver and flour industry, in line with the exercisable principle of enterprise, a kind of new quilitative method of developing, the present invention is owing to final mensuration is simple substance bromine, therefore be not only applicable to the qualitative of potassium bromate in flour improver and the flour, be applicable to the mensuration of potassium bromate in the flour-made food such as bread too.The interference that adaptability of the present invention is good, be not subjected to other material in modifying agent or the flour, accuracy height qualitatively, the qualitative lower limit that detects can reach 2PPM.In addition, it is little, easy and simple to handle that the present invention tests investment, and the normal experiment personnel of enterprise, conventional experimental facilities all can be operated.
Embodiment
Embodiment 1,
1, the processing of sample
Get 100g and contain the bromate flour sample, add the 0.1gNaOH powder, put into evaporating dish behind the mixing, charing on electric furnace, after the charing fully, evaporating dish is transferred in the muffle furnace, in 500 ℃ of following ashing, after the ashing fully, cooling with the water-soluble sample of separating after the ashing of 4ml, adds the H of 2mol/l again 2SO 42mL, regulating pH is 3, low-grade fever to 60 ℃ on electric furnace is transferred to solution in the 10ml centrifuge tube, uses the H of low amounts of water and 2mol/l then respectively 2SO 4The flushing evaporating dish, washing lotion all changes in the 10ml centrifuge tube, and the pH value is controlled at about 1.Centrifugal 10min under the 2800r/min state, it is standby to get supernatant.
2, potassium bromate is measured
Above-mentioned supernatant is transferred in the 60ml separating funnel, drips the saturated chlorine water of 0.1ml new system, the vibration back adds the 5ml phenixin, and layering is placed in vibration, and organic solvent layer filters in cuvette with absorbent cotton, under 410nm, with spectrophotometric instrumentation light absorption value.With distilled water water is blank, and light absorption value is 0.013, thinks to contain potassium bromate in the sample.With chromatography of ions same flour is measured simultaneously, measurement result is for containing bromate 2ppm.
Embodiment 2,
1, the processing of sample
Get 2 grams and contain the bromate modifying agent, add the 0.1gKOH powder, put into evaporating dish behind the mixing, charing on electric furnace, after the charing fully, evaporating dish is transferred in the muffle furnace, in 520 ℃ of following ashing, after the ashing fully, cooling with the water-soluble sample of separating after the ashing of 3ml, adds the H of 2mol/l again 2SO 41-2ml, regulating pH is 4, low-grade fever to 50 ℃ on electric furnace is transferred to solution in the 10ml centrifuge tube, uses the H of low amounts of water and 2mol/l then respectively 2SO 4The flushing evaporating dish, washing lotion all changes in the 10ml centrifuge tube, and the pH value is controlled at about 1.Centrifugal 10min under the 2800r/min state, it is standby to get supernatant.
2, potassium bromate is measured
Above-mentioned supernatant is transferred in the 60mL separating funnel, adds the 2mol/l liquor potassic permanganate of 0.1ml, the vibration back adds the 5ml chloroform, and layering is placed in vibration, and organic solvent layer filters in cuvette with absorbent cotton, under 410nm, with spectrophotometric instrumentation light absorption value.Is blank with distilled water, light absorption value is 0.025, thinks to contain bromate in the sample.With chromatography of ions same modifying agent is measured simultaneously, measurement result is for containing bromate 1.5%.
Embodiment 3,
1, the processing of sample
Get steamed bun 150 grams that are added with potassium bromate, add the 0.1gNaOH powder, put into evaporating dish behind the mixing, charing on electric furnace, after the charing fully, evaporating dish is transferred in the muffle furnace, in 600 ℃ of following ashing, after the ashing fully, cooling with the water-soluble sample of separating after the ashing of 5ml, adds the hydrochloric acid 1-2ml of 2mol/l again, regulating pH is 4, low-grade fever to 50 ℃ on electric furnace is transferred to solution in the 10ml centrifuge tube, then respectively with the hydrochloric acid flushing evaporating dish of low amounts of water and 2mol/l, washing lotion all changes in the 10ml centrifuge tube, and the pH value is controlled at 1.5.Centrifugal 10min under the 2800r/min state, it is standby to get supernatant.
2, potassium bromate is measured
Above-mentioned supernatant is transferred in the 60ml separating funnel, adds the 0.1ml hydrogen peroxide, the vibration back adds 5ml benzene, and layering is placed in vibration, and organic solvent layer filters in cuvette with absorbent cotton, under 410nm, with spectrophotometric instrumentation light absorption value.Is blank with distilled water, light absorption value is 0.020, thinks to contain bromate in the sample.With chromatography of ions same modifying agent is measured simultaneously, measurement result is for containing bromate 1%.
Embodiment 4,
1, the processing of sample
Get noodles 150 grams that are added with potassium bromate, add the 0.1gKOH powder, put into evaporating dish behind the mixing, charing on electric furnace, after the charing fully, evaporating dish is transferred in the muffle furnace, in 540 ℃ of following ashing, after the ashing fully, cooling with the water-soluble sample of separating after the ashing of 4ml, adds the nitric acid 1-2ml of 2mol/L again, regulating pH is 3.5, low-grade fever to 55 ℃ on electric furnace is transferred to solution in the 10ml centrifuge tube, then respectively with the nitric acid flushing evaporating dish of low amounts of water and 2mol/l, washing lotion all changes in the 10ml centrifuge tube, and the pH value is controlled at 2.Centrifugal 10min under the 2800r/min state, it is standby to get supernatant.
2, potassium bromate is measured
Above-mentioned supernatant is transferred in the 60ml separating funnel, adds the 0.1mL potassium dichromate, the vibration back adds 5ml toluene, and layering is placed in vibration, and organic solvent layer filters in cuvette with absorbent cotton, under 410nm, with spectrophotometric instrumentation light absorption value.Is blank with distilled water, light absorption value is 0.030, thinks to contain bromate in the sample.With chromatography of ions same modifying agent is measured simultaneously, measurement result is for containing bromate 1.6%.

Claims (3)

1. the chemical detection method of potassium bromate in a flour, modifying agent or the food is characterized in that, may further comprise the steps:
1), the processing of sample: sample heats ashing after adding alkali, adds acid treatment after water-soluble the separating, and pH value is controlled at 1~2, the centrifuging and taking supernatant;
2), potassium bromate is measured: above-mentioned supernatant is added oxygenant, and the vibration back adds organic solvent, again vibration, placing layering, is blank with distilled water, detects the light absorption value of organic solvent layer with spectrophotometer, when light absorption value more than or equal to 0.010 the time, promptly think and contain potassium bromate in the sample;
Described oxygenant is a strong oxidizer;
Described organic solvent is the organic solvent of nonpolar or low pole.
2. the chemical detection method of potassium bromate is characterized in that in flour as claimed in claim 1, modifying agent or the food, may further comprise the steps:
1), the processing of sample: after sample adds alkali heating charing earlier complete, be heated to 500~600 ℃ of complete ashing then, water-soluble the separating in cooling back, adding the diluted acid adjust pH is 3~4, complete soln moves in the centrifuge tube, the pH value is controlled at 1~1.5, the centrifuging and taking supernatant;
2), potassium bromate is measured: above-mentioned supernatant adds oxygenant, the vibration back adds organic solvent, vibration again, place layering, organic solvent layer filters in cuvette with absorbent cotton, under 410nm, with spectrophotometric instrumentation light absorption value, is blank with distilled water, when light absorption value more than or equal to 0.010 the time, can think and contain potassium bromate in the sample;
Described alkali is potassium hydroxide or NaOH;
Described diluted acid is sulfuric acid, nitric acid or hydrochloric acid;
Described oxygenant is saturated chlorine water, potassium permanganate, potassium dichromate or hydrogen peroxide;
Described organic solvent is phenixin, chloroform, benzene or toluene.
3. the chemical detection method of potassium bromate is characterized in that in flour as claimed in claim 2, modifying agent or the food, may further comprise the steps:
1), sample thief hydro-oxidation sodium powder, put into evaporating dish behind the mixing, charing on electric furnace, after the charing fully, evaporating dish is transferred in the muffle furnace, in 520 ℃ of following ashing, after the ashing fully, cooling is with the water-soluble sample of separating after the ashing of 3-5ml, the sulfuric acid solution 1-2ml that adds 2mol/l again is 50-60 ℃ of low-grade fever, solution is transferred in the centrifuge tube, and respectively with low amounts of water and a small amount of 2mol/l acid solution flushing evaporating dish, washing lotion all changes in the 10ml centrifuge tube then, the pH value is controlled at about 1, and the centrifuging and taking supernatant is standby.
2), potassium bromate is measured: above-mentioned supernatant is transferred in the separating funnel, dropwise drip saturated chlorine water, the vibration back adds phenixin, and layering is placed in vibration, organic solvent layer filters in cuvette with absorbent cotton, under 410nm,, be blank with distilled water with spectrophotometric instrumentation light absorption value, when light absorption value more than or equal to 0.010 the time, can think and contain potassium bromate in the sample.
CNA2008100492049A 2008-02-01 2008-02-01 Method for chemistry testing potassium bromate in flour, amendment or food Pending CN101226139A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101887022A (en) * 2010-06-21 2010-11-17 泉州市产品质量检验所 Rapid detection method and reagent of bromate in water
CN103245658A (en) * 2013-04-23 2013-08-14 山西省食品质量安全监督检验研究院 Fast detection method of bromate in bread
CN104297229A (en) * 2014-09-06 2015-01-21 济南大学 Making method and application of polythiophene derivative electrochemiluminescence sensor
CN112834492A (en) * 2020-12-31 2021-05-25 广州安诺科技股份有限公司 Detection reagent and kit for rapidly detecting potassium bromate

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101887022A (en) * 2010-06-21 2010-11-17 泉州市产品质量检验所 Rapid detection method and reagent of bromate in water
CN103245658A (en) * 2013-04-23 2013-08-14 山西省食品质量安全监督检验研究院 Fast detection method of bromate in bread
CN103245658B (en) * 2013-04-23 2015-07-29 山西省食品质量安全监督检验研究院 The method for quick of bromate in a kind of bread
CN104297229A (en) * 2014-09-06 2015-01-21 济南大学 Making method and application of polythiophene derivative electrochemiluminescence sensor
CN112834492A (en) * 2020-12-31 2021-05-25 广州安诺科技股份有限公司 Detection reagent and kit for rapidly detecting potassium bromate

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Open date: 20080723