CN104568929A - Rapid testing paper for testing hydrogen peroxide residue in foods - Google Patents

Rapid testing paper for testing hydrogen peroxide residue in foods Download PDF

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Publication number
CN104568929A
CN104568929A CN201310505497.8A CN201310505497A CN104568929A CN 104568929 A CN104568929 A CN 104568929A CN 201310505497 A CN201310505497 A CN 201310505497A CN 104568929 A CN104568929 A CN 104568929A
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China
Prior art keywords
paper
testing
test paper
residual peroxide
quick detection
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Pending
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CN201310505497.8A
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Chinese (zh)
Inventor
黄昆仑
许文涛
程楠
翟百强
徐瑗聪
董凯
罗云波
何景
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FUDEAN OF BEIJING TECHNOLOGY Co Ltd
China Agricultural University
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FUDEAN OF BEIJING TECHNOLOGY Co Ltd
China Agricultural University
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Priority to CN201310505497.8A priority Critical patent/CN104568929A/en
Publication of CN104568929A publication Critical patent/CN104568929A/en
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Abstract

The invention relates to rapid testing paper for testing hydrogen peroxide residue in foods, belonging to the food safety testing field. The rapid testing paper is composed of a paper base and a piece of color developing paper, and has simple structure and can be operated simply. A piece of 3mm chromatographic filter paper is used as a carrier, and the testing paper can rapidly realize semi-quantitative detection on the hydrogen peroxide residue within 3s; the optimal manufacturing process is selected, and the production period of the testing paper is shortened greatly; an enzymatic protective reagent is added to improve the stability and the storage life of the testing paper; the testing conclusion can be acquired by visual observation, no precious instruments are required for displaying, and a user can master without specialized training; and the price is low, the production cost is low, the testing paper is disposable and does not need to be maintained and overhauled, the precision is high, the repeatability is good, and the rapid testing paper is very suitable for supervision departments to rapidly detect and monitor in real time in field.

Description

Residual peroxide quick detection test paper in a kind of food
Technical field
The present invention relates to a kind of quick, sensitive, test paper of detecting residual peroxide in food easily, belong to field of detection of food safety.
Background technology
Hydrogen peroxide (Hydrogen peroxide) molecular formula is H2O2, molecular weight 34.01, and its aqueous solution is commonly called as hydrogen peroxide (Dioxowater).Present socio-economic development is more and more faster, people more and more pay close attention to healthy and food security, residual harm wherein about hydrogen peroxide day by day attracts much attention, now domestic had much about the edible report containing excess hydrogen peroxide Food poisoning cases, and lot of domestic and international research shows that hydrogen peroxide is found to have carcinogenicity from the eighties in 20th century, there is substantial connection with various active oxygen associated diseases simultaneously.The Ministry of Public Health of China formally implements GB2760-2011 " food additives use standard " on June 20th, 2011, wherein in food processing process once widely used hydrogen peroxide kick out of the usable range of food additives.State General Administration for Quality Supervision's No. 156 bulletin in 2011 clearly proposes, and the food enterprises prohibits the use hydrogen peroxide.
In food, the traditional detection method of residual peroxide can be divided into chemical analysis method and instrument analytical method substantially.For the sample of high concentration, general employing chemical titration analysis method, mainly contains permanganimetric method, iodimetric titration and cerium sulfate method etc.; For the sample of low concentration, conventional instrument analytical method has high performance liquid chromatography, ultraviolet spectrophotometry, flow injection-spectrophotometric method etc.Although detection method is so many, the abuse phenomenon of hydrogen peroxide in food still can not get effective control, Partial Food processing factory brightens in order to food, often adopt the hydrogen peroxide of the technical grade of high concentration to process food, as: shark's fin, dried fish, American pistachios, dried shrimp, coconut palm fruit, blackout chicken, duck, pork surface bleaching and protect look, to improve the outward appearance of product, the food of moldy metamorphism even soaks after bleaching through superoxol and again sells by some illegal retailers.Show in the food such as part dairy produce, beans fabricated product, Boiled chicken with salt, Chicken Feet with Pickled Peppers, all have the residual peroxide of excess in the food quality inspection report carried out at home; Also the hydrogen peroxide up to 1.5% is detected in the shark's fin of the Hong Kong Special Administrative Region.Trace it to its cause, be that these classic methods are consuming time slightly long, and cost is higher, to be unsuitable in basic unit and Site Detection universal use, therefore in food, quick, the Sensitive Detection of residual peroxide is a China's development of food industry and food security gordian technique difficult problem in the urgent need to address.
Since 20 beginnings of the century, a great revolution is that paper is applied in analysis design mothod, and nineteen fifty-two Martin and Synge is because invention paper chromatography is awarded the Nobel Prize.Paper becomes a platform attracted people's attention very much, and there is unique performance, comprising: manufacturing cost and use cost is cheap, have biodegradability and biocompatibility, easily coating trace, porous fibrous structure, by means of capillary force without the need to other power, be generally the optimal platform that white can provide colourimetry and Fluorometric assay.Current patent 200920139941.8 discloses the residual peroxide quick detection test paper with the development of potassium iodide-starch method, but the test paper response time is long, and testing result is not if observed immediately, affect by air oxidation etc., reactant color changes very soon, correctly can not judge result.Also have patent 200610011568.9 to disclose and develop residual peroxide quick detection test paper by enzyme-catalytic chromogenic reaction principle, but this test paper fabrication cycle is long, the term of validity is short, is unfavorable for that test paper is as the circulation of commodity and application.Therefore, must find that a kind of susceptibility is good, the response time is short, with short production cycle, the technology that there is considerable stability and storage life, have the very strong market competitiveness, be used for detecting fast the residual quantity of hydrogen peroxide in food.
Summary of the invention
The invention discloses a kind of quick, sensitive, test paper of detecting residual peroxide in food easily, can measure residual quantities of hydrogen peroxide in the various food of market sale quickly and easily, in 3s, read half-quantitative detection result.
Composition of the present invention: comprise paper substrate and colour developing scraps of paper two parts, the described colour developing scraps of paper are first through the immersion of reactant liquor A, soak time is 10-20s, in temperature 45-50 DEG C, dry 45-50min under the environment of vacuum tightness 100-110Pa, and then pass through the immersion of reactant liquor B, soak time is 10-20s, in temperature 45-50 DEG C, the environment of vacuum tightness 100-110Pa dries 25-30min; The described colour developing scraps of paper are fixedly connected with described substrate.
Preparation process of the present invention:
(1) preparation of reactant liquor A liquid: take pH value as the citrate buffer solution of 5.0 be solvent, with the horseradish peroxidase of 0.4-0.6g/L (HRP) for solute, adds enzyme stabilizers polyvinylpyrrolidone 5-10g/L;
(2) cutting of filter paper: the rectangle scraps of paper with paper-cutter, 3mm chromatography filter paper (hereinafter referred to as filter paper) being cut into 10cm × 15cm, is convenient to follow-up immersion liquid and oven dry;
(3) immersion of reactant liquor A liquid: the A liquid configured is poured in special glass ware, clamps the filter paper cut and soak 10-20s in A liquid, hang on dry boxboard with clip with tweezers;
(4) dry: disturbing making test paper lose result of use for preventing the oxygen molecule in air, the filter paper completing immersion liquid being put into vacuum drying chamber, reaches vacuum tightness 100-110Pa, temperature 45-50 DEG C, drying time 45-50min.
(5) preparation of reactant liquor B liquid: take absolute ethyl alcohol as solvent, the surfactant S20(TWEEN80 that 3,3', 5, the 5'-tetramethyl benzidines (TMB) of 1.0-2.0g/L are solute and 0.1%-3%) mixing;
(6) immersion of reactant liquor B liquid: the B liquid configured is poured in special glass ware, clamps the filter paper cut and soak 10-20s in B liquid, hang on dry boxboard with clip with tweezers;
(7) dry: the filter paper completing immersion liquid is put into vacuum drying chamber, reaches vacuum tightness 100-110Pa, temperature 45-50 DEG C, drying time 25-30min;
(8) storage of the colour developing scraps of paper: dried filter paper is the colour developing scraps of paper, is cut into the colour developing bar of 1cm × 15cm, often opens and can be cut to 10, be enclosed in valve bag, puts into the exsiccator filling drying agent and retains to be checked;
(9) making of paper substrate: the rectangle scraps of paper with paper-cutter, PP synthetic paper being cut into 7cm × 15cm, is convenient to the bonding of follow-up paper substrate and colour-development sheet and the cutting of test strips.
(10) bonding of paper substrate and colour-development sheet: the colour developing bar bonding agent of the 1cm × 15cm cut is binded in one end of the paper substrate of 7cm × 15cm, becomes test-paper;
(11) cutting of test strips: the test strips with paper cutter, the test-paper binded evenly being cut into 0.55cm × 7cm;
(12) storage of test strips: be sealed in storage in 4-20 DEG C of dry environment, must not direct sunlight be subject to.
The scope of application of the present invention: in food, the sxemiquantitative of residual peroxide detects fast; Sensing range: 0-50mg/L; Cleaning Principle: under hydrogen peroxide existence condition, the A liquid prepared by horseradish peroxidase, disodium ethylene diamine tetraacetate, the B liquid that energy catalysis is prepared by tetramethyl benzidine generates light blue material, and it generates depth of material color and the concentration of hydrogen peroxide is proportionate.
Sample preparation of the present invention: fluid sample can direct-detection; Solid sample should be pulverized and be mixed with the distilled water of equal quality, after soaking 5min, stirs and can detect liquid.
Method of operating of the present invention: get appropriate sample in the drying receptacle of cleaning, with the colour-development sheet region of submergence test paper for standard, takes out after submergence immediately, by colour-development sheet horizontal positioned upward, can carry out sxemiquantitative reading after 3s.
Result of the present invention judges: the color of test paper and standard color comparison card are compared, and numerical value corresponding to the color range identical with colorimetric card color is the detected value of this sample, and namely the color as test paper gets both intermediate value between two color ranges.
Feature of the present invention: be only made up of paper substrate and colour developing scraps of paper two parts, structure is all very simple with operation; With 3mm chromatography filter paper for carrier, test paper is enable to carry out half-quantitative detection rapidly to residual peroxide in 3s; Select optimum manufacture craft, greatly shorten the production cycle of test paper; Add enzymatic protective reagent, improve stability and the storage life of test paper; Rely on visual observation to draw test result, do not need with expensive instrument display, user does not need specialized training just can grasp; Low price simultaneously, production cost is low, and for single use and without the need to repair and maintenance, degree of accuracy is higher, and repeatability, the scene that is suitable for very much is detected real-time and monitors.
Accompanying drawing explanation
Fig. 1 is plan structure schematic diagram of the present invention;
Fig. 2 is plan structure schematic diagram of the present invention;
Fig. 3 is standard color comparison card of the present invention (mg/L), colorimetric corresponding sexadecimal color code.
Embodiment
Preparation embodiment
Embodiment 1
First reactant liquor A and reactant liquor B is configured, in reactant liquor A solvent to be pH value be 5.0 citrate buffer solution, solute is the mixed liquor of the horseradish peroxidase (HRP) of 0.4g/L and the polyvinylpyrrolidone of 5g/L, in reactant liquor B, solvent is absolute ethyl alcohol, solute is 3 of 1.0g/L, 3', 5,5'-tetramethyl benzidine and 1mL S20(TWEEN80) mixed liquor.By 3mm chromatography filter paper soak time 10s in reactant liquor A, dry 45min, then in reactant liquor B, soak 10s under under the environment of vacuum tightness 100Pa, temperature 45 C, the environment in temperature 50 C, vacuum tightness 100Pa dries 25min.The filter paper handled well is binded on substrate, cuts into the test strips of 0.55cm × 7cm.Be sealed in storage in 4 DEG C of dry environments, must not direct sunlight be subject to.
Embodiment 2
First reactant liquor A and reactant liquor B is configured, in reactant liquor A solvent to be pH value be 5.0 citrate buffer solution, solute is the mixed liquor of the horseradish peroxidase (HRP) of 0.6g/L and the polyvinylpyrrolidone of 10g/L, in reactant liquor B, solvent is absolute ethyl alcohol, solute is 3 of 2.0g/L, 3', 5,5'-tetramethyl benzidine and 3mL S20(TWEEN80) mixed liquor.By 3mm chromatography filter paper soak time 20s in reactant liquor A, dry 50min, then in reactant liquor B, soak 20s under under the environment of vacuum tightness 110Pa, temperature 50 C, the environment in temperature 50 C, vacuum tightness 110Pa dries 30min.The filter paper handled well is binded on substrate, cuts into the test strips of 0.55cm × 7cm.Be sealed in storage in 4 DEG C of dry environments, must not direct sunlight be subject to.
Effect example
Embodiment 3
The famous brand name milk sample 20 part of buying from supermarket, gets appropriate sample respectively in the drying receptacle of cleaning, with the colour-development sheet region of submergence test paper for standard, takes out immediately after submergence, by colour-development sheet horizontal positioned upward, can carry out sxemiquantitative reading after 3s.The color of test paper and standard color comparison card are compared, numerical value corresponding to the color range identical with colorimetric card color is the detected value of this sample, and namely the color as test paper gets both intermediate value between two color ranges.Recording residual quantities of hydrogen peroxide in 20 parts of milk samples and be 0mg/L, is qualified samples.
Embodiment 4
The famous brand name Chicken Feet with Pickled Peppers sample 5 part of buying from supermarket, get 5g sample respectively and add distilled water 5g, get appropriate sample liquid in the drying receptacle of cleaning, with the colour-development sheet region of submergence test paper for standard, take out immediately after submergence, by colour-development sheet horizontal positioned upward, sxemiquantitative reading can be carried out after 3s.The color of test paper and standard color comparison card are compared, numerical value corresponding to the color range identical with colorimetric card color is the detected value of this sample, and namely the color as test paper gets both intermediate value between two color ranges.Recording residual quantities of hydrogen peroxide in 5 parts of Chicken Feet with Pickled Peppers samples and be 0mg/L, is qualified samples.
Embodiment 5
The famous brand name bubble green pepper crackling sample 1 part of buying from supermarket, get 5g sample respectively and add distilled water 5g, get appropriate sample liquid in the drying receptacle of cleaning, with the colour-development sheet region of submergence test paper for standard, take out immediately after submergence, by colour-development sheet horizontal positioned upward, sxemiquantitative reading can be carried out after 3s.The color of test paper and standard color comparison card are compared, numerical value corresponding to the color range identical with colorimetric card color is the detected value of this sample, and namely the color as test paper gets both intermediate value between two color ranges.Recording residual quantities of hydrogen peroxide in bubble green pepper crackling sample is 50mg/L, is failed test sample.
Method according to GB GB/T23499-2009 is verified, testing result is consistent with test paper result of the present invention, demonstrates practicality of the present invention and accuracy.

Claims (8)

1. residual peroxide quick detection test paper in a food, it is characterized in that: be made up of paper substrate and the colour developing scraps of paper, the described colour developing scraps of paper are in advance through the immersion of reactant liquor A, soak time is 10-20s, in temperature 45-50 DEG C, dry 45-50min under the environment of vacuum tightness 100-110Pa, and then by the immersion of reactant liquor B, soak time is 10-20s, in temperature 45-50 DEG C, the environment of vacuum tightness 100-110Pa dries 25-30min; The described colour developing scraps of paper are fixedly connected with described substrate.
2. residual peroxide quick detection test paper in a kind of food according to claim 1, it is characterized in that: described paper substrate material is PP synthetic paper, developing paper sheet material is 3mm chromatography filter paper.
3. residual peroxide quick detection test paper in a kind of food according to claim 1, it is characterized in that: in described reactant liquor A, solvent is damping fluid, solute is the horseradish peroxidase (HRP) of 0.4-0.6g/L and the enzymatic protective reagent mixed liquor of 5-10g/L; In described reactant liquor B, solvent is absolute ethyl alcohol, and solute is the surfactant mixed liquor of 3,3' of 1.0-2.0g/L, 5,5'-tetramethyl benzidines (TMB) and 0.1%-3%.
4. residual peroxide quick detection test paper in a kind of food according to claim 3, is characterized in that: buffer solution is including, but not limited to citrate buffer solution, PBS phosphate buffer, Tris hydrochloride buffer and borate buffer solution.
5. residual peroxide quick detection test paper in a kind of food according to claim 3, is characterized in that: enzymatic protective reagent is including, but not limited to polyvinylpyrrolidone, bovine serum albumin(BSA) (BSA) and glycerine.
6. residual peroxide quick detection test paper in a kind of food according to claim 3, it is characterized in that: surfactant is including, but not limited to S9(Tetronic1307), S14(TRITON X-100), S19(TWEEN20), S20(TWEEN80) and S21 (BRIJ35), and their mixed system.
7. residual peroxide quick detection test paper in a kind of food according to claim 1, it is characterized in that: the blueness of standard color comparison card is divided into 5 class from shallow to deep, they respectively in corresponding detected sample residual peroxide actual concentrations be 0mg/L, 5mg/L, 10mg/L, 20mg/L, 50mg/L.
8. residual peroxide quick detection test paper in asking described in 1 a kind of food according to right, is characterized in that: the specification of described test strips is long 5-10cm, wide 0.5-1cm, is preferably the specification of long 7cm, wide 0.55cm.
CN201310505497.8A 2013-10-24 2013-10-24 Rapid testing paper for testing hydrogen peroxide residue in foods Pending CN104568929A (en)

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Cited By (16)

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Publication number Priority date Publication date Assignee Title
CN105067611A (en) * 2015-08-20 2015-11-18 北京福德安科技有限公司 Quick test paper for hardness of water
CN105606604A (en) * 2016-01-08 2016-05-25 昆明泊银科技有限公司 Rapid hydrogen peroxide test paper and preparation method thereof
CN106525831A (en) * 2016-11-03 2017-03-22 百奥森(江苏)食品安全科技有限公司 Test paper for detecting hydrogen peroxide in food
CN106770241A (en) * 2016-12-15 2017-05-31 张育宁 Test paper component of Vitamin C content and preparation method thereof in detection liquid food
CN107356588A (en) * 2017-06-30 2017-11-17 济南大学 The superoxide radical and hydrogen peroxide paper substrate detection method of a kind of simple and sensitive
CN107831161A (en) * 2017-12-06 2018-03-23 广东轻工职业技术学院 Small molecule containing acetate is used as the new application of catalyst as class peroxidase
CN107917910A (en) * 2017-11-16 2018-04-17 武汉轻工大学 It is a kind of to be used to detect class enzyme test peper of hydrogen peroxide and its preparation method and application
CN108548814A (en) * 2018-04-19 2018-09-18 长春万成生物电子工程有限公司 The detection method of bromine content in Test paper of bromine content and preparation method thereof and water
CN108802365A (en) * 2018-05-31 2018-11-13 湖南远璟生物技术有限公司 A kind of preparation method of progesterone enzyme conjugates
CN109856124A (en) * 2018-12-13 2019-06-07 迪瑞医疗科技股份有限公司 A kind of hydrogen peroxide detection drying chemical reagent paper and preparation method thereof
CN110031459A (en) * 2019-05-10 2019-07-19 中国农业大学 A kind of hydrogen peroxide quick detection test paper based on monatomic nano enzyme
CN110514654A (en) * 2018-05-21 2019-11-29 中国农业科学院北京畜牧兽医研究所 The rapid detection method of lactoperoxidase in a kind of cow's milk
CN112730397A (en) * 2020-12-24 2021-04-30 上海三爱思试剂有限公司 Test paper for rapidly determining hydrogen peroxide content and preparation method thereof
WO2022020379A1 (en) * 2020-07-20 2022-01-27 Veriteque Usa, Inc. Gun shot residue field kit
CN114280040A (en) * 2021-11-18 2022-04-05 中国农业科学院油料作物研究所 Test strip for detecting peroxide value of edible oil, preparation method and application thereof
CN115754288A (en) * 2022-11-15 2023-03-07 广东和信健康科技有限公司 Sample pad treatment solution and application thereof

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Cited By (18)

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Publication number Priority date Publication date Assignee Title
CN105067611A (en) * 2015-08-20 2015-11-18 北京福德安科技有限公司 Quick test paper for hardness of water
CN105606604A (en) * 2016-01-08 2016-05-25 昆明泊银科技有限公司 Rapid hydrogen peroxide test paper and preparation method thereof
CN106525831A (en) * 2016-11-03 2017-03-22 百奥森(江苏)食品安全科技有限公司 Test paper for detecting hydrogen peroxide in food
CN106770241A (en) * 2016-12-15 2017-05-31 张育宁 Test paper component of Vitamin C content and preparation method thereof in detection liquid food
CN106770241B (en) * 2016-12-15 2018-02-06 张育宁 Detect test paper component of Vitamin C content and preparation method thereof in liquid food
CN107356588A (en) * 2017-06-30 2017-11-17 济南大学 The superoxide radical and hydrogen peroxide paper substrate detection method of a kind of simple and sensitive
CN107917910A (en) * 2017-11-16 2018-04-17 武汉轻工大学 It is a kind of to be used to detect class enzyme test peper of hydrogen peroxide and its preparation method and application
CN107831161A (en) * 2017-12-06 2018-03-23 广东轻工职业技术学院 Small molecule containing acetate is used as the new application of catalyst as class peroxidase
CN108548814A (en) * 2018-04-19 2018-09-18 长春万成生物电子工程有限公司 The detection method of bromine content in Test paper of bromine content and preparation method thereof and water
CN110514654A (en) * 2018-05-21 2019-11-29 中国农业科学院北京畜牧兽医研究所 The rapid detection method of lactoperoxidase in a kind of cow's milk
CN108802365A (en) * 2018-05-31 2018-11-13 湖南远璟生物技术有限公司 A kind of preparation method of progesterone enzyme conjugates
CN109856124A (en) * 2018-12-13 2019-06-07 迪瑞医疗科技股份有限公司 A kind of hydrogen peroxide detection drying chemical reagent paper and preparation method thereof
CN110031459A (en) * 2019-05-10 2019-07-19 中国农业大学 A kind of hydrogen peroxide quick detection test paper based on monatomic nano enzyme
WO2022020379A1 (en) * 2020-07-20 2022-01-27 Veriteque Usa, Inc. Gun shot residue field kit
CN112730397A (en) * 2020-12-24 2021-04-30 上海三爱思试剂有限公司 Test paper for rapidly determining hydrogen peroxide content and preparation method thereof
CN114280040A (en) * 2021-11-18 2022-04-05 中国农业科学院油料作物研究所 Test strip for detecting peroxide value of edible oil, preparation method and application thereof
CN115754288A (en) * 2022-11-15 2023-03-07 广东和信健康科技有限公司 Sample pad treatment solution and application thereof
CN115754288B (en) * 2022-11-15 2023-08-29 广东和信健康科技有限公司 Sample pad treatment fluid and application thereof

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Application publication date: 20150429

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