CN101118219A - Rapid detecting method for detecting formaldehyde doped in flash milk - Google Patents

Rapid detecting method for detecting formaldehyde doped in flash milk Download PDF

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Publication number
CN101118219A
CN101118219A CNA2007101538577A CN200710153857A CN101118219A CN 101118219 A CN101118219 A CN 101118219A CN A2007101538577 A CNA2007101538577 A CN A2007101538577A CN 200710153857 A CN200710153857 A CN 200710153857A CN 101118219 A CN101118219 A CN 101118219A
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China
Prior art keywords
reagent
formaldehyde
former milk
milk
naoh
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CNA2007101538577A
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Chinese (zh)
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CN100510718C (en
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常建军
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Inner Mongolia Mengniu Dairy Group Co Ltd
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Inner Mongolia Mengniu Dairy Group Co Ltd
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Abstract

The present invention relates to a detecting method, in particular to a quick detecting method which can detect mixed formaldehyde in raw milk, and belongs to the technical field of chemical components detection. In the quick detecting method which can detect mixed formaldehyde in raw milk provided by the present invention, the proportion of reagent A, reagent V and weight of water is (10-14) to (0.5-1.5) to 100. The proportion of the weight of the raw milk and a mixed reagent is (4-8) to 1. After a period of time, whether formaldehyde exists can be qualitatively judged according to the color reaction. Only one kind of mixed reagent is needed to be prepared in the method and only one step operation of adding reagent is needed to be carried through. The color reaction is fast and only one minute is necessary. The measuring condition is relatively loose. The sensitivity is high and the cost is low.

Description

Formaldehyde doped method for quick in a kind of former milk
Technical field
The present invention relates to a kind of detection method, formaldehyde doped method for quick in particularly a kind of former milk.Belong to the technical field that chemical analysis detects.
Background technology
At present in China, the phenomenon that former milk is mingled is prohibited repeatly and is not ended, and more and more serious and general.Because formaldehyde has the corrosion-proof and sterilization effect, under the ordering about of interests, some milk families add the microbiological indicator of formaldehyde when reaching milk collection in former milk, who does not know that formaldehyde is the material than high toxicity, preferentially control on the list formaldehyde at China's toxic chemical and are in second.Formaldehyde is defined as carcinogenic and teratogenesis shape material by the World Health Organization (WHO), is the allergen of generally acknowledging, also is one of potential strong mutagen, and it can destroy biological cell albumen, can cause diseases such as human allergy, enteron aisle irritant reaction, food poisoning.
Fast detecting to formaldehyde in the former milk has corresponding several detection method at present, as acetylacetone method, HNO 3And H 2SO 4Method, FeCl 3Method, FeCl 3And dense H 2SO 4Method, variable color acid system, the luxuriant and rich with fragrance sound of vomiting of iron-neighbour quinoline development process, but, the quality of former milk can not be guaranteed because of being not easy to safe operation, the colour developing shortcoming that phenomenon is not obvious or sensitivity is not high.At present the fast detecting box that is used for detecting formaldehyde in the former milk is specially arranged also on the market in addition, but price comparison is expensive.So at this phenomenon, the inventor proceeds from reality, and considers restriction and security, the convenience consideration from operating of milk collection time, has developed formaldehyde quick detection reagent in the former milk voluntarily, its phenomenon is obvious, highly sensitive, and with low cost, easy and safe to operate.
Summary of the invention
The objective of the invention is: develop formaldehyde doped method for quick in a kind of former milk, its phenomenon is obvious, highly sensitive, and with low cost, easy and safe to operate.
Technical scheme of the present invention is as follows:
Because reagent (phloroglucin) reacts with formaldehyde, generate the material that has color of high molecular under catalyst V reagent (NaOH) catalysis.In the prior art never the people this reaction is used in the formaldehyde doped method for quick of former milk, through long experiment with sum up, obtained method of the present invention.
Formaldehyde doped method for quick in a kind of former milk of the present invention, wherein, detect according to following steps:
1. A reagent is dissolved in a certain amount of water, add the V reagent preparation and obtain mix reagent, wherein, above-mentioned A reagent and V reagent are respectively NaOH and phloroglucin, NaOH, phloroglucin and water weight ratio example are: (10-14): (0.5-1.5): 100, preferably (11-13): (0.8-1.2): 100, most preferably 12: 1: 100;
2. above-mentioned mix reagent is added in the detected former milk sample, the part by weight of former milk and mix reagent is (4-8): 1, preferred (5-7): 1, most preferably be: 6: 1;
3. whether wait for a period of time, qualitatively judging according to chromogenic reaction has formaldehyde to exist.Preferably at least 1 minute.
1, principle
A reagent (phloroglucin) reacts with formaldehyde under catalyst V reagent (NaOH) catalysis, generates the material that has color of high molecular.
2, reaction reagent
A reagent and V reagent are mixed into mix reagent in certain proportion.The concrete prescription of mix reagent is:
Take by weighing 12g NaOH earlier and be dissolved in the 100mL water, be made into 12% sodium hydroxide solution; And then take by weighing the 1g phloroglucin, be dissolved in 100mL 12% NaOH (NaOH) solution.
3, qualitative detection step:
Directly the former milk sample of 3ml is joined in the test tube, add the compounding of the above-mentioned institute of 0.5ml again and close reagent, not vibration, the chromogenic reaction in 1min bottom the visual observations test tube.
Preferably make a blank test tube during detection, can help paired observation like this.
4, the result judges
The milk sample of bottom does not develop the color in the test tube, and formaldehyde does not detect;
The milk sample of bottom shows light red in the test tube, contains a small amount of formaldehyde;
The milk sample of bottom shows orange red in the test tube, contains a large amount of formaldehyde.
Annotate: if contain trace, a spot of formaldehyde in the milk sample, light red can occur in the middle bottom of test tube, the time ratio of color fade is shorter, approximately about 1min.If contain relatively large formaldehyde in the milk sample, can deepen in the middle bottom colors of test tube, even whole milk sample all is orange red.
The result of embodiment and discussion
1, mix reagent concentration determines
Found through experiments, the concentration of A reagent changes, and the color of reaction and display is almost constant, and when finding that the A reagent concentration is high, color fading is very fast.When finding that simultaneously the V reagent concentration increases, the color of reaction and display is almost constant, but the solution developing time is too fast, and the time of fading is also fast.So the suitable concentration of A reagent and V reagent has been determined in a large amount of experiment of inventor's process, and is simultaneously also both economical.
2, the mix reagent consumption determines
Found through experiments, when former milk sample solution and mix reagent amount ratio were controlled at 3: 0.5 left and right sides, colour developing relatively was easy to observe.When also find drawing former milk testing sample solution and mix reagent, get liquid measure and need not require very accurately, the effect of chromogenic reaction is the same, and is like this, just just looser to operating personnel's operation requirement.
3, qualitative test standard colors row and detection limit determines
Table 1
The content of formaldehyde (μ g/ml) in the former milk sample Color Qualitative results
0 1.9 3.8 7.6 9.5 19.6 Milky milky pale pink pink colour light red is orange red Negative weak positive
As can be seen from Table 1, detecting of the method is limited to 3.8 μ g/ml.
4, with market in the detection milk sold the quick kit of content of formaldehyde compare
Table 2
The content of formaldehyde (μ g/ml) in the former milk sample The autogamy mix reagent The fast detecting box
0 1.9 3.8 7.6 9.5 19.6 Milky milky pale pink pink colour light red is orange red Milky milky pale pink (phenomenon is not obvious) pink colour light red is orange red
As can be seen from Table 2, the mix reagent of autogamy is higher than the sensitivity of the quick detection reagent of selling on the market.And find that in experimentation the mix reagent fading time of autogamy is slower than kit, more helps operating personnel's observation.
Advantage of the present invention:
This method only need be prepared a kind of mix reagent, has only a step to add the reagent operation, and chromogenic reaction is fast, only needs about 1 minute, and condition determination is relatively also loose; And highly sensitive, cost is low, in former milk detects, disturb also little, detection limit 3.8 μ g/ml.For big-and-middle-sized dairy products enterprise, be formaldehyde doped method in the former milk of a kind of fast detecting that is highly suitable for popularizing.
Embodiment
Embodiment 1
Take by weighing 12g NaOH earlier and be dissolved in the 100mL water, be made into 12% sodium hydroxide solution; And then take by weighing the 1g phloroglucin, be dissolved in 100mL 12% NaOH (NaOH) solution.
Directly the former milk sample of 3ml is joined in the test tube, add the compounding of the above-mentioned institute of 0.5ml again and close reagent, not vibration, the chromogenic reaction in 1min bottom the visual observations test tube.
Preferably make a blank test tube during detection, can help paired observation like this.
Testing result is as follows:
The content of formaldehyde (μ g/ml) in the former milk sample Color Qualitative results
0 1.8 3.9 7.5 9.3 19.9 Milky milky pale pink pink colour light red is orange red Negative weak positive
Embodiment 2
Take by weighing 14g NaOH earlier and be dissolved in the 100mL water, be made into 14% sodium hydroxide solution; And then take by weighing the 0.5g phloroglucin, be dissolved in 100mL 14% NaOH (NaOH) solution.
Directly the former milk sample of 8ml is joined in the test tube, add the compounding of the above-mentioned institute of 0.5ml again and close reagent, not vibration, the chromogenic reaction in 1min bottom the visual observations test tube.
Preferably make a blank test tube during detection, can help paired observation like this.
Testing result is as follows:
Formaldehyde contains in the former milk sample Color Qualitative results
Amount (μ g/ml)
0 1.9 4.5 8.2 9.9 20.9 Milky milky pale pink pink colour light red is orange red Negative weak positive
Embodiment 3
Take by weighing 10g NaOH earlier and be dissolved in the 100mL water, be made into 14% sodium hydroxide solution; And then take by weighing the 1.5g phloroglucin, be dissolved in 100mL 10% NaOH (NaOH) solution.
Directly the former milk sample of 2ml is joined in the test tube, add the compounding of the above-mentioned institute of 0.5ml again and close reagent, not vibration, the chromogenic reaction in 1min bottom the visual observations test tube.
Preferably make a blank test tube during detection, can help paired observation like this.
Testing result is as follows:
The content of formaldehyde (μ g/ml) in the former milk sample Color Qualitative results
0 1.8 4.0 7.6 9.0 18.9 Milky milky pale pink pink colour light red is orange red Negative weak positive
Embodiment 4
Take by weighing 10g NaOH earlier and be dissolved in the 100mL water, be made into 14% sodium hydroxide solution; And then take by weighing the 0.5g phloroglucin, be dissolved in 100mL 10% NaOH (NaOH) solution.
Directly the former milk sample of 2.5ml is joined in the test tube, add the compounding of the above-mentioned institute of 0.5ml again and close reagent, not vibration, the chromogenic reaction in 1min bottom the visual observations test tube.
Preferably make a blank test tube during detection, can help paired observation like this.
Testing result is as follows:
The content of formaldehyde (μ g/ml) in the former milk sample Color Qualitative results
0 1.6 4.1 7.2 9.6 19.9 Milky milky pale pink pink colour light red is orange red Negative weak positive
This method only need be prepared a kind of mix reagent, has only a step to add the reagent operation, and chromogenic reaction is fast, only needs about 1 minute, and condition determination is relatively also loose; And highly sensitive, cost is low, in former milk detects, disturb also little, detection limit 3.8 μ g/ml.For big-and-middle-sized dairy products enterprise, be formaldehyde doped method in the former milk of a kind of fast detecting that is highly suitable for popularizing.

Claims (3)

1. formaldehyde doped method for quick in the former milk is characterized in that: detect according to following steps:
1) A reagent is dissolved in a certain amount of water, add the V reagent preparation and obtain mix reagent, wherein, above-mentioned A reagent and V reagent are respectively NaOH and phloroglucin, and NaOH, phloroglucin and water weight ratio example are: (10-14): (0.5-1.5): 100;
2) above-mentioned mix reagent is added in the detected former milk sample, the part by weight of former milk and mix reagent is (4-8): 1;
3) whether wait for a period of time, qualitatively judging according to chromogenic reaction has formaldehyde to exist.
2. formaldehyde doped method for quick in the former milk as claimed in claim 1 is characterized in that: routine preferred 12: 1: 100 of A reagent, V reagent and water weight ratio.
3. formaldehyde doped method for quick in the former milk as claimed in claim 1 is characterized in that: the part by weight of former milk and mix reagent is preferably: 6: 1.
CNB2007101538577A 2007-09-14 2007-09-14 Rapid detecting method for detecting formaldehyde doped in flash milk Active CN100510718C (en)

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103076321A (en) * 2012-11-26 2013-05-01 江苏中烟工业有限责任公司徐州卷烟厂 Method for detecting formaldehyde in water-based adhesive used for cigarette by continuous flow analyzer
CN109224844A (en) * 2018-10-23 2019-01-18 江苏省计量科学研究院 A kind of preparation method of the sphere material of double catalyzed coloration removing formaldehyde gas molecules

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103076321A (en) * 2012-11-26 2013-05-01 江苏中烟工业有限责任公司徐州卷烟厂 Method for detecting formaldehyde in water-based adhesive used for cigarette by continuous flow analyzer
CN103076321B (en) * 2012-11-26 2015-09-30 江苏中烟工业有限责任公司徐州卷烟厂 A kind of Continuous Flow Analysis instrument detects the method for formaldehyde in smoke aqueous gel
CN109224844A (en) * 2018-10-23 2019-01-18 江苏省计量科学研究院 A kind of preparation method of the sphere material of double catalyzed coloration removing formaldehyde gas molecules
CN109224844B (en) * 2018-10-23 2021-06-25 江苏省计量科学研究院 Preparation method of spherical material for removing formaldehyde gas molecules through double-catalysis color development

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