CN101290323A - Cow milk and milk powder nitrite qualitative checking method and reagent kit - Google Patents
Cow milk and milk powder nitrite qualitative checking method and reagent kit Download PDFInfo
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- CN101290323A CN101290323A CNA2008101001025A CN200810100102A CN101290323A CN 101290323 A CN101290323 A CN 101290323A CN A2008101001025 A CNA2008101001025 A CN A2008101001025A CN 200810100102 A CN200810100102 A CN 200810100102A CN 101290323 A CN101290323 A CN 101290323A
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Abstract
The invention relates to a detection method, in particular to a method for qualitatively detecting nitrite in milk and dry milk, and also relates to a kit for the qualitative detection of the nitrite, belonging to the chemical composition detection technical field. The method for qualitatively detecting the nitrite in the milk and the dry milk has the following steps that: a griess reagent is added into the milk or the reconstituted milk and is mixed evenly; according to the change in the color of the milk sample, whether the milk is mixed with the nitrite is judged, and the detection limit of the method is 0.2mg/L.
Description
Technical field
The present invention relates to a kind of detection method, nitrite qualitative checking method in particularly a kind of cow's milk and the milk powder.Belong to the technical field that chemical analysis detects.
Background technology
Also there is not GB detection method at present about nitrite fast qualitative in cow's milk and the milk powder, GB quantitative methods accuracy height, but, be not suitable for on-line quick detection because detection time is long, the inspection technology requirement is high.It is one of important sanitary index of cow's milk and milk powder that nitrite detects.The present invention is the conventional fast qualitative method of inspection, shortens proving time, does not need equipment and hi-tech personnel's outfit, can be widely used in the online quality inspection of raw milk, fluid milk, milk powder.
Summary of the invention
The objective of the invention is: obtain nitrite qualitative checking method in a kind of cow's milk and the milk powder, belong to the conventional sense method, with low cost, convenient to operation, but widespread use.
Nitrite qualitative checking method in a kind of cow's milk of the present invention and the milk powder, wherein, detect according to following steps:
1) gets blank milk or reconstituted milk, be divided into 4-8 part, to wherein mixing sodium nitrite, make the sample that the concentration gradient that contains sodium nitrite increases progressively;
2) in the sample that concentration gradient increases progressively, add accord with regular rules in this thousand reagent;
3) observe change color behind the mixing;
4) according to color: white, the micro mist look, lightpink, pink colour, deep pink, pink are with the corresponding colorimetric card that is prepared into color of the content of sodium nitrite in milk or the reconstituted milk;
5) get milk to be measured or reconstituted milk sample, Ge Lisi thousand reagent are added, promptly can be corresponding go out the content range of the nitrite in milk to be measured or the reconstituted milk sample according to color.
Above-mentioned steps 2) and 5) in newborn sample to be measured or the reconstituted milk dative additional proportion of this thousand reagent be: 10: 0.1-5, preferred 10: 1.
The above-mentioned step of stating 2) and 5) in the preparation and the store method of Ge Lisi thousand reagent: tartrate, anhydrous sulfanilic acid, three kinds of medicines of alpha-naphthylamine are fully mixed and porphyrize with 89: 10: 1 ratio, and sealing is kept dry and is deposited in the brown bottle.
The above-mentioned mass concentration of stating adding sodium nitrite in the step 1) is the boundary with 0.2mg/L, is decremented to 0 downwards, and is upward to 2mg/L, preferred: 0.00mg/L, 0.10mg/L, 0.20mg/L, 0.50mg/L, 1.00mg/L, 2.00mg/L, 10.00mg/L.
The kit of method for preparing, the colorimetric card color on it is followed successively by: white, micro mist look, lightpink, pink colour, pink.
Above-mentioned steps 3) preferably in 30s-1min, observes change color behind the mixing in.
The result of embodiment and discussion
The test of process, the inventor confirms thousand compositions and methods with Ge Lisi, the method for carrying out the qualitative conventional sense of nitrite has feasibility.And can widespread use.
Advantage of the present invention: detection method of the present invention is a kind of conventional sense method, and is with low cost, convenient to operation, but widespread use.
Method of the present invention is a kind of detection method; according to purport of the present invention; the detection of any use the inventive method all should fall into protection scope of the present invention, can't produce any restriction to detection method of the present invention because of the concrete detection data among the embodiment.
Embodiment
Embodiment 1
1) gets 7 parts of blank milk or reconstituted milks, add sodium nitrite, be mixed with the sample of following content; 0.00mg/L, 0.10mg/L, 0.20mg/L, 0.50mg/L, 1.00mg/L, 2.00mg/L, 10.00mg/L.
2) in the sample that concentration gradient increases progressively, add accord with regular rules in this thousand reagent; The additional proportion of this thousand reagent is in newborn sample to be measured or the reconstituted milk sample dative: 10: 1, wherein, the preparation and the store method of Ge Lisi thousand reagent are as follows: tartrate, anhydrous sulfanilic acid, three kinds of medicines of alpha-naphthylamine are fully mixed and porphyrize with 89: 10: 1 ratio, and sealing is kept dry and is deposited in the brown bottle.
3) observe change color behind the mixing; In 30s, observe change color.
4) according to color: white, the micro mist look, lightpink, pink colour, deep pink, pink are with the corresponding colorimetric card that is prepared into color of the content of sodium nitrite in milk or the reconstituted milk; Shown color and content of sodium nitrite contrast are: white or no change＜0.2mg/L, micro mist look 0.2-0.5mg/L, pink colour 0.5-1mg/L, deep pink 2-5mg/L, pink 5-10mg/L.
5) get milk to be measured or reconstituted milk sample, Ge Lisi thousand reagent are added, promptly can be corresponding go out the content range of the nitrite in milk to be measured or the reconstituted milk sample according to color.
Embodiment 2
1) gets blank milk or reconstituted milk 4-8 part, add sodium nitrite, be mixed with the sample that the gradient of 0-10.00mg/L sodium nitrite increases progressively; 0.00mg/L, 0.10mg/L, 0.20mg/L, 0.50mg/L, 1.00mg/L, 2.00mg/L, 5.00mg/L, 10.00mg/L.
2) in the sample that concentration gradient increases progressively, add accord with regular rules in this thousand reagent; The additional proportion of this thousand reagent is in newborn sample to be measured or the reconstituted milk sample dative: 10: 5, wherein, the preparation and the store method of Ge Lisi thousand reagent are as follows: tartrate, anhydrous sulfanilic acid, three kinds of medicines of alpha-naphthylamine are fully mixed and porphyrize with 89: 10: 1 ratio, and sealing is kept dry and is deposited in the brown bottle.
3) observe change color behind the mixing; In 1min, observe change color
4) according to color: white, the micro mist look, lightpink, pink colour, deep pink, pink are with the corresponding colorimetric card that is prepared into color of the content of sodium nitrite in milk or the reconstituted milk;
5) get milk to be measured or reconstituted milk sample, Ge Lisi thousand reagent are added, promptly can be corresponding go out the content range of the nitrite in milk to be measured or the reconstituted milk sample according to color.
Embodiment 3
1) gets 4 parts of blank milk or reconstituted milks, add sodium nitrite, be mixed with following sample; 0.00mg/L, 0.20mg/L, 2.00mg/L, 10.00mg/L;
2) in the sample that concentration gradient increases progressively, add accord with regular rules in this thousand reagent; The additional proportion of this thousand reagent is in newborn sample to be measured or the reconstituted milk sample dative: 10: 0.1, wherein, the preparation and the store method of Ge Lisi thousand reagent are as follows: tartrate, anhydrous sulfanilic acid, three kinds of medicines of alpha-naphthylamine are fully mixed and porphyrize with 89: 10: 1 ratio, and sealing is kept dry and is deposited in the brown bottle;
3) observe change color behind the mixing; In 45s, observe change color;
4) according to color: white, the micro mist look, pink colour, pink is with the corresponding colorimetric card that is prepared into color of the content of sodium nitrite in milk or the reconstituted milk;
5) get milk to be measured or reconstituted milk sample, Ge Lisi thousand reagent are added, promptly can be corresponding go out the content range of the nitrite in milk to be measured or the reconstituted milk sample according to color.
Embodiment 4
1) gets 6 parts of blank milk or reconstituted milks, add sodium nitrite, be mixed with the sample that the gradient of 0-10.00mg/L sodium nitrite increases progressively; 0.00mg/L, 0.20mg/L, 0.50mg/L, 2.00mg/L, 10.00mg/L.
2) in the sample that concentration gradient increases progressively, add accord with regular rules in this thousand reagent; The additional proportion of this thousand reagent is in newborn sample to be measured or the reconstituted milk sample dative: 10: 0.1-5, wherein, the preparation and the store method of Ge Lisi thousand reagent are as follows: tartrate, anhydrous sulfanilic acid, three kinds of medicines of alpha-naphthylamine are preferably fully mixed and porphyrize with 89: 10: 1 ratio, and sealing is kept dry and is deposited in the brown bottle.
3) observe change color behind the mixing; In 30s-1min, observe change color
4) according to color: white, the micro mist look, lightpink, deep pink, pink are with the corresponding colorimetric card that is prepared into color of the content of sodium nitrite in milk or the reconstituted milk;
5) get milk to be measured or reconstituted milk sample, Ge Lisi thousand reagent are added, promptly can be corresponding go out the content range of the nitrite in milk to be measured or the reconstituted milk sample according to color.
Embodiment 5
Nitrite qualitative checking method in a kind of cow's milk and the milk powder, detect according to following steps:
1. material:
5ml calibrated pipet, test tube, medicine spoon.
2. reagent:
Tartrate, anhydrous sulfanilic acid, alpha-naphthylamine.
3. medicine preparation:
Ge Lisi thousand reagent: tartrate (C
4H
6O
6) 89 the gram, anhydrous sulfanilic acid (C
6H
4(NH
2) (S0
3H)) 10 grams, alpha-naphthylamine (C
6H
7NH
2) 1 gram, three kinds of reagent are weighed up the back respectively fully mix, in beveller, be ground into the white powder of the uniform and delicate of no visible particle, sealing is kept dry and is deposited in the brown bottle, and this solid reagent becomes Ge Lisi thousand reagent.The reagent for preparing is preferably in the week and finishes using, and stops using immediately after the reagent variable color.
4. running program:
4.1 get cow's milk or reconstituted milk 3ml in test tube.
4.2 Ge Lisi thousand reagent with the about 0.3g of unified special-purpose medicine bale-out one flat spoon add in the test tube, avoid the reagent wall built-up.
4.3 behind the vibration mixing immediately (in 1 minute) observe newborn sample change color in the test tube.
4.4 when detecting, do negative control simultaneously.
4.5 judge according to following table:
| Breast sample color | Semi-quantitative results | Qualitatively judge the result |
| White or no change | ＜0.2mg/L | Negative |
| The micro mist look | 0.2mg/L | Positive |
| Pink colour | 0.5-1mg/L | Positive |
| Deep pink | 2-5mg/L | Positive |
| Pink | 5-10mg/L | Positive |
4.6 testing result:
| Sample number into spectrum | Breast sample color | Semi-quantitative results | Qualitatively judge the result |
| Sample 1 | White | ＜0.2mg/L | Negative |
| Sample 2 | Pink colour | 0.2mg/L | Positive |
| Sample 3 | White | ＜0.2mg/L | Negative |
| Sample 4 | White | ＜0.2mg/L | Negative |
| Sample 5 | White | ＜0.2mg/L | Negative |
Embodiment 6
Get nitrite feminine gender (used the table sizing technique to detect and confirm the back) milk sample, artificially add the sodium nitrite of variable concentrations, detect with corresponding method, the result is as follows in checking:
| Numbering | Content of sodium nitrite, mg/L | Breast sample color | The result judges |
| 1 | 0.00 | White | Negative |
| 2 | 0.10 | Slight pink colour, but be difficult for debating look | Negative |
| 3 | 0.20 | The micro mist look | Positive |
| 4 | 0.50 | Lightpink | Positive |
| 5 | 0.80 | Pink colour | Positive |
| 6 | 1.00 | Pink colour | Positive |
| 7 | 2.00 | Deep pink | Positive |
| 8 | 10.00 | Pink | Positive |
Embodiment 7
The inventive method and the contrast of GB/T 5413.32-1997 GB sizing technique.
1. select 2 in 5 of the milk samples of different categories and reconstituted milk sample, carry out the testing result contrast:
| Sample number into spectrum | National Standard Method | The inventive method | The result of determination degree of conformity |
| Cow's milk 1 | Do not detect | ＜0.2mg/L | Conform to |
| Cow's milk 2 | Do not detect | ＜0.2mg/L | Conform to |
| Cow's milk 3 | Do not detect | ＜0.2mg/L | Conform to |
| Cow's milk 4 | 0.003 | ＜0.2mg/L | Conform to |
| Cow's milk 5 | Do not detect | ＜0.2mg/L | Conform to |
| Reconstituted milk 6 | Do not detect | ＜0.2mg/L | Conform to |
| Reconstituted milk 7 | 3.8mg/L | 2-5mg/L | Conform to |
2. calculate drug inspection cost and the contrast of check time spent with single single sample:
| Classification | National Standard Method | Ge Lisi thousand reagent methods |
| The drug inspection cost | 10 yuan | 0.5 unit |
| The check time spent | 4-5 hour | 2 minutes |
Claims (7)
1. nitrite qualitative checking method in cow's milk and the milk powder is characterized in that: detect according to following steps:
1) gets blank milk or reconstituted milk 4-8 part, add sodium nitrite, be mixed with the sample that the gradient of 0-10.00mg/L sodium nitrite increases progressively;
2) in the sample that concentration gradient increases progressively, add accord with regular rules in this thousand reagent;
3) observe change color behind the mixing;
4) according to color: white, the micro mist look, lightpink, pink colour, deep pink, pink are with the corresponding colorimetric card that is prepared into color of the content of sodium nitrite in milk or the reconstituted milk;
5) get milk to be measured or reconstituted milk sample, Ge Lisi thousand reagent are added, promptly can be corresponding go out the content range of the nitrite in milk to be measured or the reconstituted milk sample according to color.
2. detection method as claimed in claim 1 is characterized in that: described step 2) and 5) in newborn sample to be measured or the reconstituted milk sample dative additional proportion of this thousand reagent be: 10: 0.1-5, preferred 10: 1.
3. detection method as claimed in claim 1 or 2, it is characterized in that: in described step 2) and 5) in the preparation and the store method of Ge Lisi thousand reagent: tartrate, anhydrous sulfanilic acid, three kinds of medicines of alpha-naphthylamine are preferably fully mixed and porphyrize with 89: 10: 1 ratio, and sealing is kept dry and is deposited in the brown bottle.
4. detection method as claimed in claim 1 is characterized in that: preferably observe change color in the described step 3) behind the mixing in 30s-1min.
5. detection method as claimed in claim 1 is characterized in that: the mass concentration that adds sodium nitrite in the described step 1) is the boundary with 0.2mg/L, is decremented to 0 downwards, upward to 10mg/L.
6. detection method as claimed in claim 4 is characterized in that: preferred 0.00mg/L, 0.10mg/L, 0.20mg/L, 0.50mg/L, 1.00mg/L, 2.00mg/L, 10.00mg/L.
7. one kind with the nitrite detection kit as method preparation among the claim 1-5, and it is characterized in that: the colorimetric card color on it is followed successively by: white, micro mist look, lightpink, pink colour, deep pink, pink.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101001025A CN101290323A (en) | 2008-05-20 | 2008-05-20 | Cow milk and milk powder nitrite qualitative checking method and reagent kit |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101001025A CN101290323A (en) | 2008-05-20 | 2008-05-20 | Cow milk and milk powder nitrite qualitative checking method and reagent kit |
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ID=40034676
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|---|---|---|---|
| CNA2008101001025A Pending CN101290323A (en) | 2008-05-20 | 2008-05-20 | Cow milk and milk powder nitrite qualitative checking method and reagent kit |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101806746A (en) * | 2010-04-20 | 2010-08-18 | 内蒙古蒙牛乳业（集团）股份有限公司 | Rapid testing method of zinc salt in milk |
| CN101893575A (en) * | 2010-04-08 | 2010-11-24 | 新疆农业大学 | Method for rapidly testing nitrite in fresh milk |
| CN101413897B (en) * | 2008-12-01 | 2010-12-08 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method and reagent kit for detecting nitrite shield reagent in milk |
| CN103529031A (en) * | 2013-11-01 | 2014-01-22 | 内蒙古农业大学 | Semi-solid-type nitrite rapid detection tube and method for preparing same |
| CN104458712A (en) * | 2013-09-18 | 2015-03-25 | 云南健牛生物科技有限公司 | Rapid detection method of nitrite in blood and urine with high sensitivity |
| CN105651768A (en) * | 2015-12-29 | 2016-06-08 | 内蒙古蒙牛乳业（集团）股份有限公司 | Color developing agent composition and application thereof as well as method for detecting nitritein sample |
| 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 |
| CN108152286A (en) * | 2018-02-11 | 2018-06-12 | 广东出入境检验检疫局检验检疫技术中心 | A kind of kit and its detection method of quick qualification determination nitrite in cubilose content |
| CN111721756A (en) * | 2019-03-18 | 2020-09-29 | 中国农业科学院北京畜牧兽医研究所 | Alkaline phosphatase activity detection kit and detection method |
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2008
- 2008-05-20 CN CNA2008101001025A patent/CN101290323A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101413897B (en) * | 2008-12-01 | 2010-12-08 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method and reagent kit for detecting nitrite shield reagent in milk |
| CN101893575A (en) * | 2010-04-08 | 2010-11-24 | 新疆农业大学 | Method for rapidly testing nitrite in fresh milk |
| CN101806746A (en) * | 2010-04-20 | 2010-08-18 | 内蒙古蒙牛乳业（集团）股份有限公司 | Rapid testing method of zinc salt in milk |
| CN104458712A (en) * | 2013-09-18 | 2015-03-25 | 云南健牛生物科技有限公司 | Rapid detection method of nitrite in blood and urine with high sensitivity |
| CN103529031A (en) * | 2013-11-01 | 2014-01-22 | 内蒙古农业大学 | Semi-solid-type nitrite rapid detection tube and method for preparing same |
| CN105651768A (en) * | 2015-12-29 | 2016-06-08 | 内蒙古蒙牛乳业（集团）股份有限公司 | Color developing agent composition and application thereof as well as method for detecting nitritein sample |
| 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 |
| CN108152286A (en) * | 2018-02-11 | 2018-06-12 | 广东出入境检验检疫局检验检疫技术中心 | A kind of kit and its detection method of quick qualification determination nitrite in cubilose content |
| CN111721756A (en) * | 2019-03-18 | 2020-09-29 | 中国农业科学院北京畜牧兽医研究所 | Alkaline phosphatase activity detection kit and detection method |
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