CN102207466A - Rapid test kit for benzoyl peroxide (banned additive) in flour and preparation method thereof - Google Patents
Rapid test kit for benzoyl peroxide (banned additive) in flour and preparation method thereof Download PDFInfo
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- CN102207466A CN102207466A CN 201110084232 CN201110084232A CN102207466A CN 102207466 A CN102207466 A CN 102207466A CN 201110084232 CN201110084232 CN 201110084232 CN 201110084232 A CN201110084232 A CN 201110084232A CN 102207466 A CN102207466 A CN 102207466A
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Abstract
The invention discloses a rapid test kit for benzoyl peroxide (banned additive) in flour and a preparation method thereof. The test kit comprises a reaction reagent, a color-developing agent, a positive-control reagent stock solution and a standard colorimetric card; the reaction reagent is a ferrous ion acidic aqueous solution with the concentration of 100mg/L-300mg/L; the color-developing agent is a thiocyanate radical aqueous solution with the concentration of 0.5mol/L-0.75mol/L; the positive-control reagent stock solution is a benzoyl peroxide ethanol solution with the concentration of 500mg/L-1500mg/L; and the standard colorimetric card comprises a number of small comparator blocks, and each comparator block corresponds to a concentration of benzoyl peroxide. According to the invention, after the color of a sample to be tested is developed according to the operation method of the test kit, qualitative and semi-quantitative analyses are directly performed by contrast to the standard colorimetric card, and no large-sized analyzer is used in the entire process of sample analysis, therefore the operation process is simplified, and the time for analysis is shortened.
Description
Technical field
The present invention relates to quick detection kit and preparation method, be specifically related to violated adjuvant benzoyl peroxide quick detection kit of flour and preparation method.
Background technology
Benzoyl peroxide (Benzoyl Peroxide, BPO), chemical formula [C
6H
5C (O) O]
2, be a kind of organic peroxide, it has remarkable whitening effect to flour.1986, the safety evaluation of whole nation food additives technical committee for standardization (TCST) is passed through, list benzoyl peroxide in China " food additives use hygienic standard " (GB2760), allow to use in wheat flour processing as flour treating agent, bleaching agent, maximum is used to limit the quantity of and is 60mg/kg.But because the nutrition of benzoyl peroxide destroys flour, especially to beta carotene in the flour and V
EStronger destruction is arranged.The benzoic absorption of benzoyl peroxide oxidation product has increased the weight of burden of liver, easily causes multiple disease.In addition, existing fluor producing process is difficult to benzoyl peroxide is added evenly, and the as easy as rolling off a log benzoyl peroxide content part of causing exceeds standard.In February, 2011, seven departments such as the Ministry of Public Health dispatch a joint document, and from May 1st, 2011, forbid adding benzoyl peroxide in flour production.
About the detection of benzoyl peroxide content in the flour, national standard method is vapor-phase chromatography (GB 18415-2001) and high performance liquid chromatography (GB22325-2008).These two kinds the method detection limit is low, accuracy is high, favorable reproducibility.But these two kinds of method complex operations, length consuming time needs expensive gas chromatograph or liquid chromatograph, is not suitable for being used for flour benzoyl peroxide fast detecting and on-the site analysis.
The benzoyl peroxide detection method is reported more in periodical literature, mainly is divided into chemical qualitativity method, oxidimetry, spectrophotometric method, vapor-phase chromatography, high performance liquid chromatography, the chromatography of ions, electrochemical method and chemoluminescence method.The major defect that chemical qualitativity method and oxidimetry exist is that sensitivity and accuracy are lower.Though and spectrophotometric method, vapor-phase chromatography, high performance liquid chromatography, the chromatography of ions, electrochemical method and chemoluminescence method sensitivity and accuracy increase, but the general character shortcoming that these methods exist is the sample pre-treatments complexity, sample analysis time is long, needs expensive analytical instrument.
The benzoyl peroxide detection method is more existing reports in patent documentation.Chinese patent publication number 1776409A, a kind of method that detects benzoyl peroxide content in the flour is disclosed, detecting principle is that the orange red complex compound that utilizes benzoyl peroxide that phenanthroline and ferrous sulphate are generated fades, and its fading extent and benzoyl peroxide concentration have correlativity.Chinese patent publication number 101042354A, quantitative analysis method for benzoyl peroxide in a kind of product wheat flour is disclosed, detecting principle is by the colorimetry principle, the prolongation of time is added in utilization along with benzoyl peroxide, benzoyl peroxide performance whitening effect, present-color material in the wheat flour reduces, and shoals with the color of alcohol immersion wheat flour gained solution, and original benzoyl peroxide addition has correlativity in its fading extent and the wheat flour.Yet above-mentioned two kinds of methods need image acquisition device, and need be based on the benzoyl peroxide assay software systems of computing machine colourity identification, and fading extent and benzoyl peroxide concentration correlativity are not strong, and accuracy in detection is not high.Chinese patent publication number 101210907A, the highly effective liquid phase chromatography detection method of benzoyl peroxide in a kind of wheat flour is disclosed, this method detection sensitivity and accuracy are higher, yet this method need be carried out complicated pre-treatment operation to sample, sample analysis time is longer, needs expensive high performance liquid chromatograph.Chinese patent publication number 101339136A, a kind of chemical luminous system and method for measuring benzoyl peroxide disclosed, detecting principle is to utilize benzoyl peroxide and luminol reaction to produce the optical radiation of wavelength for 425nm, this method detection limit is low, highly sensitive, yet this method needs Chemiluminescence Apparatus, and course of reaction needs divalent cobalt ion as catalytic specie, the operation steps complexity.
Summary of the invention
The objective of the invention is: violated adjuvant benzoyl peroxide quick detection kit of a kind of flour and preparation method thereof is provided, adopt this kit to detect benzoyl peroxide, simply, fast, accurately, do not need large-scale instrument and equipment, be fit to on-the-spot the qualitative judgement and the sxemiquantitative measurement, prevent the violated interpolation of benzoyl peroxide in flour, improve flour quality and guarantee food security.
Technical solution of the present invention is: this benzoyl peroxide quick detection kit is made up of reaction reagent, developer, positive control reagent storing solution and standard color comparison card.
The preparation method of quick detection kit is: described reaction reagent is the acidic aqueous solution of ferrous ion, the concentration of ferrous ion is at 100 mg/L to 300 mg/L, ferrous ion is provided by iron protochloride or iron ammonium sulfate or ferrous sulphate, the acidity of reaction reagent is provided by hydrochloric acid or sulfuric acid and keeps, reaction reagent is packaged in dark or the lighttight container, uses dropwise extrusion reaction reagent of hand squeeze receptacle; Described developer is the thiocyanate radical aqueous solution, thiocyanate radical is provided by ammonium thiocyanate or potassium rhodanide or sodium thiocyanate, the concentration of thiocyanate radical is at 0.5 mol/L to 0.75 mol/L, reaction reagent is packaged in the container, container is not limited to dark or lighttight container, can dropwise extrude developer with the hand squeeze receptacle; Described positive control reagent storing solution is the benzoyl peroxide ethanol solution, and the concentration of benzoyl peroxide is at 500 mg/L to 1500 mg/L, and positive control reagent storing solution is packaged in dark or the lighttight container; Described standard color comparison card comprises some rectangle color lumps, and each color lump is represented corresponding benzoyl peroxide concentration.
Wherein, the manufacturing process of standard color comparison card is: the benzoyl peroxide standard solution of system of disposition row variable concentrations, in each benzoyl peroxide standard solution, add a certain amount of reaction reagent and developer successively, chromogenic reaction takes place, according to the corresponding benzoyl peroxide concentration of standard solution of the depth of reaction back color, make standard color comparison card.
The present invention has the following advantages:
1, kit utilizes the strong oxidizing property of benzoyl peroxide, ferrous ion in the reaction reagent is oxidized to ferric ion, ferric ion again in acid solution with developer in thiocyanate radical generation chromogenic reaction, generate orange red ferric rhodanate complex, the depth of orange red complex color and benzoyl peroxide content are correlativity, and kit chromogenic reaction sensitivity, reaction conditions gentleness, reaction velocity is fast, antijamming capability is strong, measurement result is accurate.
2, comprise a standard color comparison card in the kit, after the benzoyl peroxide testing sample solution develops the color according to the kit method of operating, contrast this standard color comparison card, need be by large-sized analytic instrument, do not need the operator to prepare the benzoyl peroxide standard solution, directly testing sample is qualitatively judged and semi-quantitative analysis, simplified operating process, shortened analysis time, being used for on-the-spot qualitative judgement flour to be measured and whether having added violated adjuvant benzoyl peroxide and on-the-spot half-quantitative detection flour benzoyl peroxide content, is to qualitatively judge, fast detecting, the effective means of on-the site analysis.
3, each compound concentrations process accurate Calculation in reaction reagent in the kit and the developer, contrast agents box using method, the operator carries out reaction reagent and developer pipettes when operating, need not pipette equipment by relevant liquid, only need to drip one and get final product, be fit to on-the-spot qualitatively judge and sxemiquantitative measurement flour in benzoyl peroxide.
Embodiment
Below in conjunction with embodiment the technology of the present invention solution is further described.
Embodiment 1: the kit preparation
1. preparation feedback reagent: accurately take by weighing 0.140 g, six ferrous sulfate hydrate ammonium ((NH
4)
2Fe (SO
4)
2* 6H
2O) in 100 ml volumetric flasks, be dissolved in water, add hydrochloric acid solution 2 ml of 10 mol/L again, be diluted with water to scale, be reaction reagent; Reaction reagent is packaged in dark or the lighttight container, uses dropwise extrusion reaction reagent of hand squeeze receptacle;
2. preparation developer: accurately take by weighing 6.074 g potassium rhodanides (KSCN) in 100 ml volumetric flasks, be dissolved in water, be diluted with water to scale again, be developer; Developer is packaged in the container, and container can be but be not limited to dark or lighttight container, can dropwise extrude developer with the hand squeeze receptacle;
3. prepare positive control reagent storing solution: accurately take by weighing 0.1 g benzoyl peroxide in 100 ml volumetric flasks, add anhydrous alcohol solution, be diluted to scale with absolute ethyl alcohol again, be positive control reagent storing solution; Positive control reagent storing solution is packaged in dark or the lighttight container;
4. preparation standard colorimetric card: with absolute ethyl alcohol respectively compound concentration be 0 mg/L, 1 mg/L, 2 mg/L, 3 mg/L, 4 mg/L, 5 mg/L, 6 mg/L, 7 mg/L, 8 mg/L, 9 mg/L, 10 mg/L, 12 mg/L, 15 mg/L, 20 mg/L, the benzoyl peroxide standard solution of 30 mg/L, the color comparison tube that to get 15 specifications be 10 ml, in each color comparison tube, add above-mentioned benzoyl peroxide standard solution 1 ml respectively, one of reaction reagent (about 40 ul), one of developer (about 40 ul), 50 ℃ of water-bath 10 min, camera is taken solution photo in each color comparison tube, makes standard color comparison card according to the corresponding benzoyl peroxide concentration of standard solution of solution colour in each color comparison tube.
Embodiment 2: the kit preparation
1. preparation feedback reagent: accurately take by weighing 0.356 g Iron dichloride tetrahydrate (FeCl
2* 4H
2O) in 1000 ml volumetric flasks, be dissolved in water, add hydrochloric acid solution 20 ml of 10 mol/L again, be diluted with water to scale, be reaction reagent; Reaction reagent is packaged in dark or the lighttight container, uses dropwise extrusion reaction reagent of hand squeeze receptacle;
2. preparation developer: accurately take by weighing 3.806 ammonium thiocyanate (NH
4SCN) in 100 ml volumetric flasks, be dissolved in water, be diluted with water to scale again, be developer; Developer is packaged in the container, and container can be but be not limited to dark or lighttight container, can dropwise extrude developer with the hand squeeze receptacle;
3. prepare positive control reagent storing solution: accurately take by weighing 0.125 g benzoyl peroxide in 250 ml volumetric flasks, add anhydrous alcohol solution, be diluted to scale with absolute ethyl alcohol again, be positive control reagent storing solution; Positive control reagent storing solution is packaged in dark or the lighttight container;
4. preparation standard colorimetric card: with absolute ethyl alcohol respectively compound concentration be 0 mg/L, 1 mg/L, 2 mg/L, 3 mg/L, 4 mg/L, 5 mg/L, 6 mg/L, 7 mg/L, 8 mg/L, 9 mg/L, the benzoyl peroxide standard solution of 10 mg/L, the color comparison tube that to get 11 specifications be 10 ml, in each color comparison tube, add above-mentioned benzoyl peroxide standard solution 1 ml respectively, one of reaction reagent (about 40 ul), one of developer (about 40 ul), 50 ℃ of water-bath 10 min, camera is taken solution photo in each color comparison tube, makes standard color comparison card according to the corresponding benzoyl peroxide concentration of standard solution of solution colour in each color comparison tube.
Embodiment 3: the kit preparation
1. preparation feedback reagent: accurately take by weighing 0.149 g green vitriol (Fe (SO
4)
2* 7H
2O) in 100 ml volumetric flasks, be dissolved in water, add sulfuric acid solution 2 ml of 10 mol/L again, be diluted with water to scale, be reaction reagent; Reaction reagent is packaged in dark or the lighttight container, uses dropwise extrusion reaction reagent of hand squeeze receptacle;
2. preparation developer: accurately take by weighing 6.080 g sodium thiocyanates (NaSCN) in 100 ml volumetric flasks, be dissolved in water, be diluted with water to scale again, be developer; Developer is packaged in the container, and container can be but be not limited to dark or lighttight container, can dropwise extrude developer with the hand squeeze receptacle;
3. prepare positive control reagent storing solution: accurately take by weighing 0.15 g benzoyl peroxide in 100 ml volumetric flasks, add anhydrous alcohol solution, be diluted to scale with absolute ethyl alcohol again, be positive control reagent storing solution; Positive control reagent storing solution is packaged in dark or the lighttight container;
4. preparation standard colorimetric card: with absolute ethyl alcohol respectively compound concentration be 0 mg/L, 1 mg/L, 2 mg/L, 4 mg/L, 6 mg/L, 8 mg/L, 10 mg/L, 12 mg/L, 14 mg/L, 16 mg/L, the benzoyl peroxide standard solution of 18 mg/L, the color comparison tube that to get 11 specifications be 10 ml, in each color comparison tube, add above-mentioned benzoyl peroxide standard solution 1 ml respectively, one of reaction reagent (about 40 ul), one of developer (about 40 ul), 50 ℃ of water-bath 10 min, camera is taken solution photo in each color comparison tube, makes standard color comparison card according to the corresponding benzoyl peroxide concentration of standard solution of solution colour in each color comparison tube.
Embodiment 4: kit uses
Present embodiment is selected the kit of embodiment 1 preparation for use, illustrates that kit uses
1. benzoyl peroxide sample solution preparation: accurately take by weighing M g(0.5≤M≤1.5) flour to be measured is in containers such as conical flask or beaker or centrifuge tube, in container, add V ml(5≤V≤15 then) absolute ethyl alcohol, jog container 10 min or ultrasonic Extraction 2 min, flour to be measured is well-dispersed in the absolute ethyl alcohol, by the method for leaving standstill or filter method or centrifugal method, obtain the above ethanol solution of 1 ml, be the benzoyl peroxide sample solution;
2. kit detects:
(1) preparation positive control reagent working fluid: accurately pipette positive control reagent storing solution 1 ml in 100 ml volumetric flasks, be diluted to scale, be positive control reagent working fluid with absolute ethyl alcohol;
(2) get 3 test tubes or 3 color comparison tubes that specification is 10 ml,, pipette benzoyl peroxide sample solution 1 ml in the sample determination pipe respectively as sample determination pipe, negative control pipe and positive control pipe;
(3) add absolute ethyl alcohol 1ml to the negative control pipe;
(4) the heliotropism control tube adds 1 ml positive control reagent working fluid;
(5) in sample determination pipe, negative control pipe and positive control pipe, add a reaction reagent (about 40ul) respectively;
(6) in sample determination pipe, negative control pipe and positive control pipe, add a developer (about 40ul) respectively;
(7) sample determination pipe, negative control pipe and positive control Guan Jun react 10 min in 50 ℃ of water-baths;
(8) negative control pipe and standard color comparison card are compared, if benzoyl peroxide concentration greater than 1 mg/L, then points out this sample determination pipe measurement result inaccurate;
(9) positive control pipe and standard color comparison card are compared,, then point out this sample determination pipe measurement result inaccurate if benzoyl peroxide concentration is not equal to 10 mg/L;
(10) if negative control pipe and standard color comparison card compare, benzoyl peroxide concentration is less than 1 mg/L, positive control pipe and standard color comparison card are relatively simultaneously, benzoyl peroxide concentration equals 10 mg/L, then sample determination pipe and standard color comparison card are compared, and qualitatively judge on this basis and semi-quantitative analysis.
3. the result calculates:
(1) qualitatively judges in the flour to be measured whether added benzoyl peroxide
Benzoyl peroxide concentration tentatively qualitatively judges in the flour to be measured and has added benzoyl peroxide greater than 1 mg/L in the sample solution if sample determination pipe and standard color comparison card relatively, draw.
(2) benzoyl peroxide content in the half-quantitative detection flour to be measured
4. quality control:
Accurate for guaranteeing test result, negative control pipe and positive control pipe are set in the kit measurement method; According to this kit using method, if negative control pipe reference standard colorimetric card, benzoyl peroxide concentration is greater than 1 mg/L, illustrate then that kit had lost efficacy or prompting operation person's measurement operation process in the phenomenon of working specification appears not meeting, do not clean up such as conical flask, test tube, color comparison tube, transfer pipet etc., used absolute ethyl alcohol is contaminated or purity is not enough, and is contaminated etc. when sample solution prepares; According to this kit using method, if positive control pipe reference standard colorimetric card, benzoyl peroxide concentration is not equal to 10 mg/L, illustrate then that kit had lost efficacy or prompting operation person's measurement operation process in the phenomenon of working specification appears not meeting, do not clean up such as conical flask, test tube, color comparison tube, transfer pipet etc., used absolute ethyl alcohol is contaminated or purity is not enough, and is contaminated etc. when sample solution prepares.
Need to prove: the foregoing description is the unrestricted technical scheme of the present invention in order to explanation only, although the present invention is had been described in detail with reference to the foregoing description, those of ordinary skill in the art should understand: still can make amendment or be equal to replacement the present invention, and do not break away from any modification or partial replacement of the spirit and scope of the present invention, all should be encompassed in the middle of the claim scope of the present invention.
Claims (3)
1. the flour adjuvant benzoyl peroxide quick detection kit of violating a ban, it is characterized in that: this benzoyl peroxide quick detection kit is made up of reaction reagent, developer, positive control reagent storing solution and standard color comparison card.
2. the preparation method of the violated adjuvant benzoyl peroxide quick detection kit of flour according to claim 1, the preparation method who it is characterized in that this quick detection kit is: described reaction reagent is the acidic aqueous solution of ferrous ion, the concentration of ferrous ion is at 100 mg/L to 300 mg/L, ferrous ion is provided by iron protochloride or iron ammonium sulfate or ferrous sulphate, the acidity of reaction reagent is provided by hydrochloric acid or sulfuric acid and keeps, reaction reagent is packaged in dark or the lighttight container, uses dropwise extrusion reaction reagent of hand squeeze receptacle; Described developer is the thiocyanate radical aqueous solution, thiocyanate radical is provided by ammonium thiocyanate or potassium rhodanide or sodium thiocyanate, the concentration of thiocyanate radical is at 0.5 mol/L to 0.75 mol/L, reaction reagent is packaged in the container, container is not limited to dark or lighttight container, can dropwise extrude developer with the hand squeeze receptacle; Described positive control reagent storing solution is the benzoyl peroxide ethanol solution, and the concentration of benzoyl peroxide is at 500 mg/L to 1500 mg/L, and positive control reagent storing solution is packaged in dark or the lighttight container; Described standard color comparison card comprises several rectangle color lumps, and each color lump is represented corresponding benzoyl peroxide concentration.
3. the preparation method of the violated adjuvant benzoyl peroxide quick detection kit of flour according to claim 2, it is characterized in that: wherein, the manufacturing process of standard color comparison card is: the benzoyl peroxide standard solution of preparing serial variable concentrations, in each benzoyl peroxide standard solution, add a certain amount of reaction reagent and developer successively, chromogenic reaction takes place, according to the corresponding benzoyl peroxide concentration of standard solution of the depth of reaction back color, make standard color comparison card.
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102706872A (en) * | 2012-06-13 | 2012-10-03 | 安徽省农业科学院农产品加工研究所 | Combined reagent for detecting peroxide value of edible oil and fat and detection method thereof |
CN106706620A (en) * | 2016-12-15 | 2017-05-24 | 厦门海荭兴仪器股份有限公司 | Rapid benzoyl peroxide detection method and kit |
CN110426390A (en) * | 2019-09-18 | 2019-11-08 | 广州智汇生物科技有限公司 | The detection method of benzoyl peroxide in a kind of flour |
CN111751367A (en) * | 2020-07-13 | 2020-10-09 | 上海仪电科学仪器股份有限公司 | Method for measuring hydrogen peroxide content based on spectrophotometry |
CN111812086A (en) * | 2020-08-04 | 2020-10-23 | 河南省产品质量监督检验院 | Trisodium trithiocyanate rapid detection test paper and preparation method and detection method thereof |
CN112881380A (en) * | 2021-01-22 | 2021-06-01 | 中新苏州工业园区清城环境发展有限公司 | Method and device for detecting different concentrations of sodium persulfate in acidic water environment and using method |
CN114486872A (en) * | 2022-01-27 | 2022-05-13 | 巨进科 | Semi-quantitative detection method for ascorbic acid in wheat flour and application thereof |
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102706872A (en) * | 2012-06-13 | 2012-10-03 | 安徽省农业科学院农产品加工研究所 | Combined reagent for detecting peroxide value of edible oil and fat and detection method thereof |
CN106706620A (en) * | 2016-12-15 | 2017-05-24 | 厦门海荭兴仪器股份有限公司 | Rapid benzoyl peroxide detection method and kit |
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 |
CN110426390A (en) * | 2019-09-18 | 2019-11-08 | 广州智汇生物科技有限公司 | The detection method of benzoyl peroxide in a kind of flour |
CN110426390B (en) * | 2019-09-18 | 2022-08-05 | 广州智汇生物科技有限公司 | Method for detecting benzoyl peroxide in flour |
CN111751367A (en) * | 2020-07-13 | 2020-10-09 | 上海仪电科学仪器股份有限公司 | Method for measuring hydrogen peroxide content based on spectrophotometry |
CN111812086A (en) * | 2020-08-04 | 2020-10-23 | 河南省产品质量监督检验院 | Trisodium trithiocyanate rapid detection test paper and preparation method and detection method thereof |
CN112881380A (en) * | 2021-01-22 | 2021-06-01 | 中新苏州工业园区清城环境发展有限公司 | Method and device for detecting different concentrations of sodium persulfate in acidic water environment and using method |
CN114486872A (en) * | 2022-01-27 | 2022-05-13 | 巨进科 | Semi-quantitative detection method for ascorbic acid in wheat flour and application thereof |
CN114486872B (en) * | 2022-01-27 | 2024-01-19 | 巨进科 | Semi-quantitative detection method and application of ascorbic acid in wheat flour |
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