CN101329280A - Fast testing method of hydrogen peroxide residue in milk-like liquid and testing reagent kit thereof - Google Patents
Fast testing method of hydrogen peroxide residue in milk-like liquid and testing reagent kit thereof Download PDFInfo
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- CN101329280A CN101329280A CNA2008101348149A CN200810134814A CN101329280A CN 101329280 A CN101329280 A CN 101329280A CN A2008101348149 A CNA2008101348149 A CN A2008101348149A CN 200810134814 A CN200810134814 A CN 200810134814A CN 101329280 A CN101329280 A CN 101329280A
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Abstract
The invention relates to a detection method, in particular to a quick detection method and a detection kit for residual hydrogen peroxide in milk, belonging to the field of chemical composition detection technique. The quick detection method for detecting the residual hydrogen peroxide in the milk comprises the steps as follows: quantitative potassium iodide and amylum are added into the milk sample; according to the colour change of the milk sample, whether residual hydrogen peroxide exists in the milk sample is judged and the content of the hydrogen peroxide is measured. The invention provides the detection kit prepared according to the method of the invention at the same time. The method of the invention has the advantages of low cost, convenient and quick operation and short detection time, has the detection limit of 2mg/L and is a quick half-quantitative detection method.
Description
Technical field
The present invention relates to a kind of Ruzhong and mingle the detection method of composition, the method for quick of particularly a kind of Ruzhong hydrogen peroxide residue and according to the detection kit of this method belongs to the technical field that chemical analysis detects.
Background technology
During purchase fresh milk, for making milk fresh-keeping, some illegal retailers can add hydrogen peroxide and mingle in milk, and the hydrogen peroxide of human body excess intake can cause many-sided harm.Yet it is very limited at present to mingle the national standard method of detection about milk, can not practical requirement, can not the better controlled adulterated milk go into factory.Also there is not standard detecting method in the national standard now about hydrogen peroxide residue in breast and the milk powder.
Milk purchase line Quality Control need adopt rapid and convenient, testing cost low, can carry out the detection method of complete detection.Though there is the detection method of some hydrogen peroxide residues using in the market, mostly be higher reagent strip method of testing cost or the lower chemical staining method of check sensitivity, all be unsuitable for the widespread use of milk purchase line Quality Control.As the hydrogen peroxide speed test paper about 300 yuan of every boxes of selling on the market of price (100), the expense of 1 sample of average every detection is 3 yuan, and for manufacturing enterprise, it has improved the detection cost greatly, is unsuitable for being extensive use of of manufacturing enterprise.
Summary of the invention
The object of the present invention is to provide the method for quick and the detection kit of a kind of Ruzhong hydrogen peroxide residue, it is with low cost, easy to operate fast, and phenomenon is obvious, highly sensitive, can carry out half-quantitative detection, can satisfy the extensive needs of manufacturing enterprise.
The method for quick of a kind of Ruzhong of the present invention hydrogen peroxide residue comprises the steps:
1) gets many parts of blank milk sample, to wherein mixing hydrogen peroxide, make the sample that the concentration gradient that contains hydrogen peroxide increases progressively;
2) in the sample that this concentration gradient increases progressively according to 10: (0.5-5) ratio adds potassium iodide, and behind the mixing, again according to 10: ratio (0.2-5) adds starch solution, observes change color after shaking up immediately;
3) according to the different colours that manifests that the hydrogen peroxide content in the newborn sample is corresponding with color, be prepared into colorimetric card;
4) get newborn sample to be measured, add potassium iodide, add starch solution behind the mixing, the colorimetric card for preparing in color that will manifest and the step 3) is compared, and obtains the content range of hydrogen peroxide in the newborn sample to be measured.
Above-mentioned steps 1) the concentration gradient scope of hydrogen peroxide is mass concentration 0mg/L-100mg/L in.
Preferably, the concentration gradient of described hydrogen peroxide is 0mg/L, 2mg/L, 5mg/L, 10mg/L, 25mg/L, 50mg/L.
The preparation method of above-mentioned starch solution adds distilled water for taking by weighing soluble starch 1.0 grams, and dissolving is settled in the volumetric flask of 100ml.
The ratio that adds potassium iodide in the above-mentioned newborn sample to be measured is volume and mass ratio 10: (0.5-5).
Preferably, described newborn sample to be measured is 3ml, and the adding potassium iodide is 0.3-0.5g.
The ratio that adds starch solution in the above-mentioned newborn sample to be measured is 10: (0.2-5).
Preferably, described newborn sample to be measured is 3ml, adds 10g/L starch solution 3-5 and drips.
The quick detection kit of the hydrogen peroxide residue of method for preparing according to the present invention, described colorimetric card has different color ranges according to the difference of hydrogen peroxide content.
The color of above-mentioned colorimetric card is followed successively by: white, yellow, crocus, brown, bluish violet, blueness.
Described breast comprises dairy products, and these dairy products comprise cow's milk, yogurt etc.
Described detection kit comprises colorimetric card, potassium iodide and starch solution.
The method for quick and the detection kit of Ruzhong of the present invention hydrogen peroxide residue have following advantage:
1) with low cost.
Use the single sample drug expenditure of the inventive method specifically to be calculated as follows:
Starch: 0.0002 yuan/1 sample;
Potassium iodide: 0.1514 yuan/1 sample;
Amount to: 0.1516 yuan/1 sample.
The cost of drugs of single sample is about 0.15 yuan, compares with the hydrogen peroxide speed test paper of selling on the market, uses every test 1 duplicate samples of the inventive method, can save about 2.85 yuan, saved 95%, can reduce the detection cost significantly, be more suitable for being used for cow's milk and purchase online quality monitoring.
2) convenient to operation, proving time is short.The check time spent of single sample is about 1 minute, and is very efficient and convenient.
3) detection limit is low, is 2mg/L.
4) be rapid semi-quantitative detection method.Judge the hydrogen peroxide content scope fast according to the different colours sxemiquantitative that manifests.
5) detected artifacts is obvious, detection sensitivity is high.
Embodiment
Below in conjunction with specific embodiments method of the present invention is done more detailed description.It will be appreciated by those skilled in the art that following embodiment all is used for the present invention's scope required for protection is carried out the description of exemplary, summarize the relative scope of each parameter of the present invention, thereby it can not be interpreted as a kind of concrete restriction of the present invention with this.
Embodiment 1
The method for quick of a kind of Ruzhong hydrogen peroxide residue, detect according to following steps:
1, material:
100ml volumetric flask, 50ml beaker, 18 * 180 test tubes, 10ml calibrated pipet, 1ml calibrated pipet, water dropper, weighing scoop.
2, medicine and reagent:
Potassium iodide (analyzing pure); The 10g/L starch solution.
3, the preparation of colorimetric card:
A) artificially mix the hydrogen peroxide of variable concentrations in the blank cow's milk, make and contain hydrogen peroxide content and be respectively 0mg/L, 1mg/L, 2mg/L, 5mg/L, 10mg/L, 25mg/L, 50mg/L, the sample liquid of 100mg/L;
B) each 3mL of newborn sample that gets above-mentioned different gradients respectively adds potassium iodide 1 little spoon (about 0.3-0.5g) in test tube, after fully shaking up, splashes into the starch solution that 3-5 drips 10g/L again, and it is as shown in table 1 to shake up back observation change color:
Table 1
C) to 6 the representative points of sample liquid choice reaction color after the colour developing: white, yellow, crocus, brown, bluish violet, blueness, in time to take pictures, comparison film is edited, and adds the hydrogen peroxide content of each color correspondence and qualitatively judges the result.
4, sample determination:
Get newborn sample 3mL to be measured in test tube, add the little spoon of potassium iodide 1 (about 0.3-0.5g), after fully shaking up, splash into the starch solution that 3-5 drips 10g/L again, shake up the back observe change color and with above-mentioned steps 3 in the colorimetric card for preparing compare;
By the comparison result that newborn sample change color obtains, as shown in table 2:
Table 2
5, testing result:
The artificial hydrogen peroxide that mixes variable concentrations in the normal milk, by above-mentioned method detection, testing result is as shown in table 3 respectively:
Table 3
With carry out the hydrogen peroxide content scope that color comparison judges with colorimetric card and match.
6, method validation:
(1) checking of negative sample
Negative sample: normal milk.Get negative sample and detect testing result such as table 4 respectively as stated above:
Table 4
(2) detection limit checking
The artificial hydrogen peroxide that mixes variable concentrations in the normal milk, detection as stated above respectively, testing result is as shown in table 5:
Table 5
This method detects and is limited to 2mg/L.
Embodiment 2
The method for quick of a kind of Ruzhong hydrogen peroxide residue, detect according to following steps:
1, material:
100ml volumetric flask, 50ml beaker, 18 * 180 test tubes, 10ml calibrated pipet, 1ml calibrated pipet, water dropper, weighing scoop.
2, medicine and reagent:
Potassium iodide (analyzing pure); The 10g/L starch solution.
3, the preparation of colorimetric card:
A) artificially mix the hydrogen peroxide of variable concentrations in the blank cow's milk, make and contain hydrogen peroxide content and be respectively 0mg/L, 2mg/L, 5mg/L, 10mg/L, 25mg/L, the sample liquid of 50mg/L;
B) each 3mL of newborn sample that gets above-mentioned different gradients respectively adds potassium iodide 1 little spoon (about 0.15-0.20g) in test tube, after fully shaking up, splashes into the starch solution of 1 10g/L again, and it is as shown in table 6 to shake up back observation change color:
Table 6
C) to 6 points of sample liquid reaction color after the colour developing: white, yellow, crocus, brown, bluish violet, blueness, in time to take pictures, comparison film is edited, and adds the hydrogen peroxide content and the qualitative judgement result of each color correspondence.
4, sample determination:
Get newborn sample 3mL to be measured in test tube, add the little spoon of potassium iodide 1 (about 0.15-0.20g), after fully shaking up, splash into the starch solution of 1 10g/L again, shake up the back observe change color and with above-mentioned steps 3 in the colorimetric card for preparing compare;
By the comparison result that newborn sample change color obtains, as shown in table 7:
Table 7
5, testing result:
The artificial hydrogen peroxide that mixes variable concentrations in the normal milk, by above-mentioned method detection, testing result is as shown in table 8 respectively:
Table 8
With carry out the hydrogen peroxide content scope that color comparison judges with colorimetric card and match.
Embodiment 3
The method for quick of a kind of Ruzhong hydrogen peroxide residue, detect according to following steps:
1, material:
100ml volumetric flask, 50ml beaker, 18 * 180 test tubes, 10ml calibrated pipet, 1ml calibrated pipet, water dropper, weighing scoop.
2, medicine and reagent:
Potassium iodide (analyzing pure); The 10g/L starch solution.
3, the preparation of colorimetric card:
A) artificially mix the hydrogen peroxide of variable concentrations in the blank cow's milk, make and contain hydrogen peroxide content and be respectively 0mg/L, 1mg/L, 2mg/L, 5mg/L, 10mg/L, 25mg/L, 50mg/L, the sample liquid of 100mg/L;
B) each 3mL of newborn sample that gets above-mentioned different gradients respectively adds potassium iodide 1 little spoon (about 1.0-1.5g) in test tube, after fully shaking up, splashes into the 10g/L starch solution of 1.5mL again, and it is as shown in table 9 to shake up back observation change color:
Table 9
C) to 6 the representative points of sample liquid choice reaction color after the colour developing: white, yellow, crocus, brown, bluish violet, blueness, in time to take pictures, comparison film is edited, and adds the hydrogen peroxide content of each color correspondence and qualitatively judges the result.
4, sample determination:
Get newborn sample 3mL to be measured in test tube, add the little spoon of potassium iodide 1 (about 1.0-1.5g), after fully shaking up, splash into the 10g/L starch solution of 1.5mL again, shake up the back observe change color and with above-mentioned steps 3 in the colorimetric card for preparing compare;
By the comparison result that newborn sample change color obtains, as shown in table 10:
Table 10
5, testing result:
The artificial hydrogen peroxide that mixes variable concentrations in the normal milk, by above-mentioned method detection, testing result is as shown in table 11 respectively:
Table 11
With carry out the hydrogen peroxide content scope that color comparison judges with colorimetric card and match.
Embodiment 4
The quick detection kit of a kind of Ruzhong hydrogen peroxide residue prepares colorimetric card in this kit according to following steps:
1, artificially mixes the hydrogen peroxide of variable concentrations in the blank cow's milk, make and contain hydrogen peroxide content and be respectively 0mg/L, 1mg/L, 2mg/L, 5mg/L, 10mg/L, 25mg/L, 50mg/L, the sample liquid of 100mg/L;
2, each 3mL of newborn sample that gets above-mentioned different gradients respectively is in test tube, adds 1 spoonful of potassium iodide (, quantitative little spoon, about 0.3-0.5g), after fully shaking up, splashes into the starch solution that 3-5 drips 10g/L again, and it is as shown in table 12 to shake up back observation change color:
Table 12
3, to 6 the representative points of sample liquid choice reaction color after the colour developing: white, yellow, crocus, brown, bluish violet, blueness, in time take pictures, comparison film is edited, and adds the hydrogen peroxide content of each color correspondence and qualitatively judges the result, obtains colorimetric card.
4, above-mentioned colorimetric card, quantitative little spoon, potassium iodide reagents, 10g/L starch solution are formed detection kit.
5, get three cow's milk to be measured, every part of 3mL of yogurt sample, use quantitative little bale-out potassium iodide, add in the newborn sample, fully shake up, splash into 3-5 and drip starch solution, shake up the back and observe color,, obtain hydrogen peroxide content such as table 13 in the newborn sample with the colorimetric card comparison:
Table 13
The preparation method is easy for this kit, uses amount of reagent little, is easy to carry, and cheap, detection speed is fast, is applicable to the detection of a large amount of samples.
Using method of the present invention and detection kit to detect the required drug expenditure of single sample specifically is calculated as follows:
Starch: 0.0002 yuan/1 sample;
Potassium iodide: 0.1514 yuan/1 sample;
Amount to: 0.1516 yuan/1 sample.
The cost of drugs of single sample is about 0.15 yuan, compares with the hydrogen peroxide speed test paper of selling on the market, uses every test 1 duplicate samples of the inventive method, can save about 2.85 yuan, saved 95%, can reduce the detection cost significantly, be more suitable for being used for cow's milk and purchase online quality monitoring.
The check time spent of single sample is about 1 minute, and is very efficient and convenient.
Claims (10)
1. the method for quick of a Ruzhong hydrogen peroxide residue is characterized in that: comprise the steps:
1) gets many parts of blank milk sample, to wherein mixing hydrogen peroxide, make the sample that the concentration gradient that contains hydrogen peroxide increases progressively;
2) in the sample that this concentration gradient increases progressively according to 10: (0.5-5) ratio adds potassium iodide, and behind the mixing, again according to 10: ratio (0.2-5) adds starch solution, observes change color after shaking up immediately;
3) according to the different colours that manifests that the hydrogen peroxide content in the newborn sample is corresponding with color, be prepared into colorimetric card;
4) get newborn sample to be measured, add potassium iodide, add starch solution behind the mixing, the colorimetric card for preparing in color that will manifest and the step 3) is compared, and obtains the content range of hydrogen peroxide in the newborn sample to be measured.
2. detection method as claimed in claim 1 is characterized in that: the concentration gradient scope of hydrogen peroxide is mass concentration 0mg/L-100mg/L in the described step 1).
3. detection method as claimed in claim 2 is characterized in that: the concentration gradient of described hydrogen peroxide is 0mg/L, 2mg/L, 5mg/L, 10mg/L, 25mg/L, 50mg/L.
4. as any described detection method among the claim 1-3, it is characterized in that: the preparation method of described starch solution adds distilled water for taking by weighing soluble starch 1.0 grams, and dissolving is settled in the volumetric flask of 100ml.
5. as any described detection method among the claim 1-3, it is characterized in that: the ratio that adds potassium iodide in the described newborn sample to be measured is volume and mass ratio 10: (0.5-5).
6. detection method as claimed in claim 5 is characterized in that: described newborn sample to be measured is 3ml, and the adding potassium iodide is 0.3-0.5g.
7. as any described detection method among the claim 1-3, it is characterized in that: the ratio that adds starch solution in the described newborn sample to be measured is 10: (0.2-5).
8. detection method as claimed in claim 7 is characterized in that: described newborn sample to be measured is 3ml, adds 10g/L starch solution 3-5 and drips.
9. one kind with the hydrogen peroxide residue quick detection kit as method preparation as described among the claim 1-3 any, and it is characterized in that: described colorimetric card has different color ranges according to the difference of hydrogen peroxide content.
10. use detection kit as claimed in claim 9 for one kind, it is characterized in that: the color of described colorimetric card is followed successively by: white, yellow, crocus, brown, bluish violet, blueness.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102478524A (en) * | 2010-11-29 | 2012-05-30 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for evaluating effectiveness of melamine test strip in dairy product detection |
| CN103913521A (en) * | 2013-12-05 | 2014-07-09 | 烟台东诚生化股份有限公司 | Novel method for detecting hydrogen peroxide residues in heparin sodium |
| CN104040321A (en) * | 2011-11-23 | 2014-09-10 | 卡尔马克瑞典股份公司 | Testing system arrangement and method for testing |
| US9228953B2 (en) | 2011-11-23 | 2016-01-05 | Calmark Sweden Ab | Testing system and method for testing |
| CN107328767A (en) * | 2017-05-25 | 2017-11-07 | 新希望乳业股份有限公司 | The quick determination method of peroxidase in a kind of guaranteed milk |
| CN110514654A (en) * | 2018-05-21 | 2019-11-29 | 中国农业科学院北京畜牧兽医研究所 | A kind of rapid detection method of lactoperoxidase in milk |
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2008
- 2008-07-31 CN CNA2008101348149A patent/CN101329280A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102478524A (en) * | 2010-11-29 | 2012-05-30 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for evaluating effectiveness of melamine test strip in dairy product detection |
| CN104040321A (en) * | 2011-11-23 | 2014-09-10 | 卡尔马克瑞典股份公司 | Testing system arrangement and method for testing |
| US9228953B2 (en) | 2011-11-23 | 2016-01-05 | Calmark Sweden Ab | Testing system and method for testing |
| CN103913521A (en) * | 2013-12-05 | 2014-07-09 | 烟台东诚生化股份有限公司 | Novel method for detecting hydrogen peroxide residues in heparin sodium |
| CN103913521B (en) * | 2013-12-05 | 2015-07-08 | 烟台东诚药业集团股份有限公司 | Novel method for detecting hydrogen peroxide residues in heparin sodium |
| CN107328767A (en) * | 2017-05-25 | 2017-11-07 | 新希望乳业股份有限公司 | The quick determination method of peroxidase in a kind of guaranteed milk |
| CN110514654A (en) * | 2018-05-21 | 2019-11-29 | 中国农业科学院北京畜牧兽医研究所 | A kind of rapid detection method of lactoperoxidase in milk |
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