CN108037117A - The remaining quick determination method of industrial hydrogen peroxide, kit in food - Google Patents
The remaining quick determination method of industrial hydrogen peroxide, kit in food Download PDFInfo
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Abstract
The present invention relates to the remaining quick determination method of industrial hydrogen peroxide in a kind of food, it is characterised in that comprises the following steps：It is prepared by sample solution：Food samples are soaked using dichloromethane solution, supernatant are taken after shaking, to obtain the final product；It is prepared by standard solution：Take 2 ethyl hydrazine standard items appropriate, dichloromethane dissolving, to obtain the final product；The concentrated sulfuric acid is added dropwise into the sample solution or standard solution, develops the color；Sodium hydroxide solution, phenolphthalein test solution, colour developing are added dropwise successively；Sodium hydroxide solution is added dropwise into the sample solution or standard solution, is stood after jog；5% malonate dichloro hexane mixed solution is added dropwise, heats, colour developing.Extracting solution used, reaction test solution are general chemistry reagent, and very safe, easy to operate, the experiment flow time is short, and analysis cost is low.
Description
Technical field
The present invention relates to field of food detection, the remaining quick detection of industrial hydrogen peroxide in more particularly to a kind of food
Method, kit.
Background technology
Edible hydrogen peroxide has wide spectrum, efficient, nontoxic, noresidue characteristic, and food is used in as production and processing auxiliary agent
In the production process of product, fruits and vegetables and beverage, disinfection, sterilization, bleaching etc. can be played the role of.At abroad, edible hydrogen peroxide conduct
Food processing aid is also widely used for the perforating agent of cheese, and bleaching meat products, tealeaves, nut, are used as starch, milk etc.
Modifying agent of protein etc..In addition, edible hydrogen peroxide is more used for the disinfection of food.It is but if double using industry
Oxygen water is the food " whitening " such as chicken feet, pork tripe for industrial hydrogen peroxide, then can cause industrial dioxygen as food processing aid
Water remains in food, and heavy metal and impurity therein are also harmful.
Whether it is one of main distinction of industrial hydrogen peroxide and food grade hydrogen peroxide containing Anthraquinones impurity, therefore,
The residual of anthraquinone analog compound in food is detected, the food method whether once industrial hydrogen peroxide is handled can be characterized.Mesh
Before, it is common to use the method for detection anthraquinone analog compound be HPLC methods, hydrolyzed by adding water and hydrochloric acid, after boiling water reflux
Cold filtration.Room temperature volatilizes after filtrate is extracted with ether again, liquid chromatographic detection anthraquinone after residue methanol is dissolved and filtered
The content of constituents；Or extract food with methanol, through acid hydrolysis oxidative, the anthraquinone of reference state is decomposed into free state, make also
The anthraquinone analog compounds such as the anthrol of ortho states, anthrone, dianthrone are oxidized to oxidation state, then through extracted by ether, with magnesium acetate methanol solution
Chromogenic assay.Above two is often big with detection method operation difficulty, and elapsed time length, is unfavorable for scene during food quality detection
Quick detection and analysis.
The content of the invention
Based on the above problem, it is an object of the invention to provide a kind of remaining quick inspection of industrial hydrogen peroxide in food
Survey method.
Concrete technical scheme is as follows：
The remaining quick determination method of industrial hydrogen peroxide, comprises the following steps in a kind of food：
It is prepared by sample solution：Food samples are soaked using dichloromethane, supernatant are taken after shaking, to obtain the final product；
It is prepared by standard solution：Take 2- ethyl hydrazine standard items appropriate, dichloromethane dissolving, to obtain the final product；
The concentrated sulfuric acid is added dropwise into a sample solution or standard solution, develops the color；It is molten that sodium hydroxide is added dropwise successively
Liquid, phenolphthalein test solution, colour developing；
Sodium hydroxide solution is added dropwise into sample solution another described or standard solution, is stood after jog；It is added dropwise
5% malonate dichloromethane solution, is heated, colour developing.
In wherein some embodiments, the concentrated sulfuric acid is 98% concentrated sulfuric acid, and the concentration of sodium hydroxide solution is
10mol/L, the phenolphthalein test solution concentration are 5g/L.
In wherein some embodiments, above-mentioned quick determination method comprises the following steps：
It is prepared by sample solution：Food samples are soaked using dichloromethane solution, supernatant are taken after shaking, to obtain the final product；
It is prepared by standard solution：Take 2- ethyl hydrazine standard items appropriate, dichloromethane dissolving, to obtain the final product；
The concentrated sulfuric acid is added dropwise into the sample solution or standard solution, develops the color, absorbance is measured under 530nm wavelength；
Sodium hydroxide solution, phenolphthalein test solution, colour developing are added dropwise successively；
Sodium hydroxide solution is added dropwise into the sample solution or standard solution, is stood after jog；It is added dropwise the third of 5%
Two acid esters dichloro hexane solution, are heated, colour developing.
In wherein some embodiments, prepared by above-mentioned standard product solution include：2- ethyl hydrazine standard items 1mg is taken to be dissolved in
10ml dichloromethane, gradient dilution, to obtain the final product.
In wherein some embodiments, the shaking is to shake 10-20s at room temperature.
It is described to be heated to be in wherein some embodiments：5-15min is heated in 60-80 DEG C.
The present invention also aims to provide the remaining quick testing reagent kit of industrial hydrogen peroxide in a kind of food.Tool
Body technique scheme is as follows：
The remaining quick detection kit of industrial hydrogen peroxide in a kind of food, including dichloromethane solution as described above,
The concentrated sulfuric acid, sodium hydroxide solution, phenolphthalein test solution, 5% malonate dichloro hexane solution, during dichloromethane storage with
Aqueous is sealed.
In wherein some embodiments, above-mentioned quick detection kit further includes 2- ethyl hydrazine standard items.
The remaining quick determination method of industrial hydrogen peroxide and kit have below beneficial to effect in food of the present invention
Fruit：
Anthraquinone analog compound residual is difficult to avoid that in industrial hydrogen peroxide preparation process, industrial in food of the present invention
The quick determination method of residual peroxide, using dichloro hexane Rapid Extraction determinand, anthraquinone analog compound is because of oxonium ion
In the presence of and there is faint alkalescence, the concentrated sulfuric acid can be dissolved in and into salt, and with coloured change, it reacts simple；Separately combine hydrogen
Sodium oxide molybdena and concentrated sulfuric acid neutralization reaction, the colour developing of phenolphthalein test solution then illustrate base excess, contain in further verification sample solution with it is dense
The material of sulfuric acid reaction.Meanwhile new sample solution is separately taken, tested using Anthraquinones and benzoquinones, the difference of naphthoquinones, to exclude
Interference of other quinones substances in quickly detection benzoquinones.Reaction test solution used in quick determination method of the present invention easily obtains
, experimental implementation is easy, quick, by chromogenic reaction can judging result, it is low without complicated instrument and equipment, cost
It is honest and clean, beneficial to local analysis.And it is mutually authenticated by two steps, convincingness is strong.
Further, the present invention takes measure absorbance and calibration curve method, the colour developing using anthraquinone and the concentrated sulfuric acid anti-
Should, preliminary quantitative test is done to industrial hydrogen peroxide Anthraquinones residual in food, method is simple and practicable.
The remaining quick detection kit of industrial hydrogen peroxide in food of the present invention, incorporates quick detection food
Reagent needed for middle industrial hydrogen peroxide so that detection is more convenient.
Brief description of the drawings
Fig. 1 is the standard curve that the 2- ethyl hydrazine standard items in embodiment 2 measure；
Fig. 2 is the mark curve that the 2- ethyl hydrazine standard items in embodiment 3 measure.
Embodiment
The present invention provides the method for quickly detecting and kit of residual peroxide in a kind of food, below in conjunction with
The present invention is further elaborated for embodiment.
Embodiment 1
Quickly to be detected using the method for the present invention, industrial hydrogen peroxide in sea cucumber sample is remaining quickly to be examined the present embodiment
Kit, qualitative analysis, includes following reagent in fast check reagent box：
Reagent A：Bottle dispenses, and 6ml dichloromethane is added in every bottle, then adds 1ml distilled water aqueous along wall and seal, and one
Secondary fast inspection uses a bottle reagent；
Reagent B：98% concentrated sulfuric acid (18.4mol/L)；
Reagent C：10mol/L sodium hydroxide solutions；
Reagent D：5g/L phenolphthalein test solutions；
Reagent E：The dichloromethane solution (v/v) of 5% malonate.
Detecting step is as follows：
(1) sea cucumber sample：The leacheate of 1ml sea cucumber samples is taken, is added in centrifuge tube；
(2) 1 bottle of reagent A is added to centrifuge tube, closes the lid, tighten, shake well or shake 10-20s energetically manually,
It is to be measured.Above-mentioned prepare liquid should prepare 2 parts.
The detection of (3) first parts of prepare liquids：
3 drop reagent B are added into the centrifuge tube of prepare liquid, phenomenon is observed after jog；
8 drop reagent Cs, 4 drop reagent Ds are added dropwise again into mentioned reagent, phenomenon is observed after jog.
The detection of (4) second parts of prepare liquids：
4 drop reagent Cs are added into the centrifuge tube of prepare liquid, 1 minute is stood after jog；
4 drop reagent Es are added dropwise again into mentioned reagent, 60 DEG C of heating after five minutes, observe solution phenomenon.
As a result qualitative judgement is according to as shown in table 1：
Table 1
Because containing dichloro hexane and water in reagent A, therefore there is lamination, it is as follows to color reaction parsing in upper table：
First part of prepare liquid, i.e. step (3)：Two layers is in just colourless above and below the dropwise addition concentrated sulfuric acid of qualified sample, and hydrogen-oxygen is added dropwise
After changing sodium, phenolphthalein, just aobvious red, jog become colorless upper strata liquid level after mixing；Upper strata is after unqualified sample drop enriching sulfuric acid
Colourless, lower floor is in just yellow or yellowish-brown, and after sodium hydroxide, phenolphthalein is added dropwise, just aobvious red, jog are red after mixing for upper strata liquid level
Color does not disappear or only shoals a little, and lower floor's solution is become colorless by yellow or yellowish-brown.It is red deeper, represent target in solution
Thing component content is higher.
Second part of prepare liquid, i.e. step (4)：Qualified sample up and down two layers just in colourless, be added dropwise after sodium hydroxide without change
Change, solution is colourless after the dichloromethane solution of 5% malonate of dropwise addition and heating.The first of unqualified sample is in colourless, dropwise addition
Sodium hydroxide is unchanged, and solution is blue-green or bluish violet after the dichloromethane solution of 5% malonate of dropwise addition and heating.
Color reaction occurs for the qualitative detection of above-mentioned sample, as a result as follows：
Upper strata is colourless after the concentrated sulfuric acid is added dropwise in first part of prepare liquid, and lower floor is in just yellow or yellowish-brown, and hydroxide is added dropwise
After sodium, phenolphthalein, upper strata liquid level is just aobvious red, and jog is red after mixing not to disappear, and lower floor's solution is changed into nothing from yellow or yellowish-brown
Color.
Second part of prepare liquid is in just colourless, and dropwise addition sodium hydroxide is unchanged, and the dichloromethane that 5% malonate is added dropwise is molten
Liquid, and after heating, solution ... is blue-green.
The 2- ethyl hydrazine standard solutions for taking concentration to be 10ppm, are detected, the face in its result by above-mentioned steps
Colour response is consistent with sample solution.
In addition, through《GB/T 23672-2009 2- ethyl hydrazine》Method confirms that the sample solution contains 2- ethyl hydrazine
5mg/kg, the present embodiment qualitative results are consistent with its.
Embodiment 2
The present embodiment is remained quickly to be detected industrial hydrogen peroxide in sea cucumber sample using the method for the present invention, using as follows
Reagent：
Reagent A：Dichloromethane；During storage, sealed with aqueous；
Reagent B：98% concentrated sulfuric acid (18.4mol/L)；
Reagent C：10mol/L sodium hydroxide solutions；
Reagent D：5g/L phenolphthalein test solutions；
Reagent E：The dichloromethane solution (v/v) of 5% malonate.
Detecting step is as follows：
(1) prepared by sample solution：5g sea cucumber samples are taken, are shredded, 20ml dichloromethane is immersed, shakes energetically under room temperature
After shaking 20s, stand, take supernatant, to obtain the final product；
(2) prepared by standard solution：Take 2- ethyl hydrazine standard items appropriate, dichloromethane dissolving, gradient dilution, obtains
0.625th, 3.125,12.5,35.25,45, the 2- ethyl hydrazine standard solutions of 62.5ppm；
(3) the above-mentioned sample solutions of 7ml and the standard solution of each concentration are taken, 98% concentrated sulfuric acid of 0.92ml is added dropwise, fully
Observed after shaking, and absorbance, i.e. OD530 are measured under 530nm wavelength；1ml sodium hydroxide solutions and 4 drop phenol are added dropwise successively
Phthalein test solution, after fully shaking up, observation.
(4) 7ml sample solutions and the standard solution of each concentration separately are taken, 1ml hydroxides is added dropwise thereto with rubber head dropper
Sodium solution, stands 1min after jog；4 5% malonate dichloro hexane solution of drop are added dropwise, 60 DEG C of heating 5min, observe color.
(5) standard curve is drawn, calculates anthraquinone content in sample.
As a result according to as shown in table 1, its quantitative testing result is as shown in table 2, is drawn according to standard solution for qualitative judgement
Standard curve is as shown in Figure 1：
Table 2
Observation result step (3) in the present embodiment detection process to sample solution is added dropwise after the concentrated sulfuric acid just in colourless, drop
Liquid level is red after adding phenolphthalein, and after jog is uniform, red disappears, and solution becomes colorless, and solution becomes after the heating in step (4)
For blue-green.
The present embodiment Plays solution is different according to concentration, measures range of absorbency between 0.209 to 2.158, draws
It is y=10.611x to obtain standard curve2+7.0878x-1.9325.During because of absorbance more than 0.2, error is smaller, therefore,
The test limit of this forwarding method is up to 0.625ppm.
The OD530 values that the present embodiment measures sample solution are 0.028, its absorbance is far below 0.2, not in standard curve
Therefore, the 2- ethyl hydrazine more than test limit can not be contained in the sample, but contain benzoquinones or naphthoquinones class thing in measurement range
Matter.
Use《GB/T 23672-2009 2- ethyl hydrazine》Detection method, confirm that above-mentioned sample solution does not contain 2-
Ethyl hydrazine, confirms that the method for the present invention is accurately feasible.
Embodiment 3
The present embodiment is remained quickly to be detected industrial hydrogen peroxide in Chicken Feet with Pickled Peppers sample using the method for the present invention, its institute
With reagent with embodiment 1.
Step is as follows：
(1) prepared by sample solution：5g Chicken Feet with Pickled Peppers samples are taken, are shredded, immerse 50ml dichloromethane solutions, room temperature condition
Under shake 20s energetically after, filtering, take supernatant, to obtain the final product；
(2) prepared by standard solution：Take 2- ethyl hydrazine standard items appropriate, dichloromethane dissolving, gradient dilution, obtains
0.625th, 3.125,12.5,35.25,45, the 2- ethyl hydrazine standard solutions of 62.5ppm；
(3) the above-mentioned sample solutions of 5ml and the standard solution of each concentration are taken, the 98% dense sulphur of 0.46ml is added dropwise thereto
Acid, is observed after shake well, and absorbance, i.e. OD530 are measured under 530nm wavelength；It is molten that 0.5ml sodium hydroxides are added dropwise successively
Liquid and 3 drop phenolphthalein test solutions, after fully shaking up, observation；
(4) 5ml sample solutions and the standard solution of each concentration separately are taken, 0.5ml hydrogen-oxygens is added dropwise thereto with rubber head dropper
Change sodium solution, 1min is stood after jog；6 5% malonate dichloro hexane mixed solutions of drop are added dropwise, 60 DEG C of heating 5min, see
Examine.
(5) standard curve is drawn, calculates anthraquinone content in sample.
As a result according to as shown in table 1, its quantitative testing result is as shown in table 3, is drawn according to standard solution for qualitative judgement
Standard curve is as shown in Figure 2：
Table 3
Observation result step (3) in the present embodiment detection process to sample solution is added dropwise after the concentrated sulfuric acid just in colourless, drop
Liquid level is red after adding phenolphthalein, and after jog is uniform, red disappears, and solution becomes colorless, and solution is after the heating in step (4)
It is colourless, eliminate the interference of benzoquinones and naphthoquinones material.
The present embodiment Plays solution is different according to concentration, measures range of absorbency between 0.21 to 2.157, draws
It is y=10.652x to obtain standard curve2+6.9885x-1.8858.During because of absorbance more than 0.2, error is smaller, therefore,
The test limit of this forwarding method is up to 0.625ppm.
The OD530 values that the present embodiment measures sample solution are 1.128, substitute into above-mentioned standard curve equation, it is molten to try to achieve sample
Anthraquinone analog compound (in terms of 2- ethyl hydrazine) in liquid, concentration 19.55ppm, so as to which Chicken Feet with Pickled Peppers sample is calculated
Middle anthraquinone (in terms of 2- ethyl hydrazine) content.
Use《GB/T 23672-2009 2- ethyl hydrazine》Detection method, detection obtain 2- in above-mentioned sample solution
The concentration of ethyl hydrazine is 19.28ppm, and the error with the method for the present invention data measured is 0.14%, can receive model in error
Within enclosing.
Embodiment described above only expresses the several embodiments of the present invention, its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the present invention's
Protection domain.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (8)
1. the remaining quick determination method of industrial hydrogen peroxide in a kind of food, it is characterised in that comprise the following steps：
It is prepared by sample solution：Food samples are soaked using dichloromethane, supernatant are taken after shaking, to obtain the final product；
It is prepared by standard solution：Take 2- ethyl hydrazine standard items appropriate, dichloromethane dissolving, to obtain the final product；
The concentrated sulfuric acid is added dropwise into the sample solution, standard solution, develops the color；Sodium hydroxide solution, phenolphthalein test solution are added dropwise successively,
Colour developing；The molar ratio of the sodium hydroxide and the concentrated sulfuric acid is 2:1；
Sodium hydroxide solution is added dropwise into the sample solution or standard solution, is stood after jog；5% malonate is added dropwise
Dichloromethane solution, is heated, colour developing.
2. quick determination method according to claim 1, it is characterised in that the concentrated sulfuric acid is 98% concentrated sulfuric acid, described
Concentration of sodium hydroxide solution is 10mol/L, and the phenolphthalein test solution concentration is 5g/L.
3. quick determination method according to claim 2, it is characterised in that comprise the following steps：
It is prepared by sample solution：Food samples are soaked using dichloromethane, supernatant are taken after shaking, to obtain the final product；
It is prepared by standard solution：Take 2- ethyl hydrazine standard items appropriate, dichloromethane dissolving, to obtain the final product；
The concentrated sulfuric acid is added dropwise into the sample solution or standard solution, develops the color, absorbance is measured under 530nm wavelength；Successively
Sodium hydroxide solution, phenolphthalein test solution, colour developing is added dropwise；
Sodium hydroxide solution is added dropwise into the sample solution or standard solution, is stood after jog；5% malonate is added dropwise
Dichloro hexane solution, is heated, colour developing.
4. quick determination method according to claim 3, it is characterised in that the standard solution is prepared as：Take 2- second
Base anthraquinone standard items 1mg is dissolved in 10ml dichloromethane, gradient dilution, to obtain the final product.
5. according to claim 1-4 any one of them quick determination methods, it is characterised in that the shaking is to shake at room temperature
10-20s。
6. according to claim 1-4 any one of them quick determination methods, it is characterised in that described to be heated to be：In 60-80 DEG C
Heat 5-15min.
7. the remaining quick detection kit of industrial hydrogen peroxide in a kind of food, it is characterised in that including dichloromethane, dense sulphur
Acid, sodium hydroxide solution, phenolphthalein test solution, 5% malonate dichloro hexane solution, with aqueous when the dichloromethane stores
Envelope.
8. quick detection kit according to claim 7, it is characterised in that further include 2- ethyl hydrazine standard items.
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| CN201711228263.8A CN108037117B (en) | 2017-11-29 | 2017-11-29 | Method and kit for rapidly detecting industrial hydrogen peroxide residue in food |
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| CN201711228263.8A CN108037117B (en) | 2017-11-29 | 2017-11-29 | Method and kit for rapidly detecting industrial hydrogen peroxide residue in food |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112649556A (en) * | 2020-11-13 | 2021-04-13 | 新疆大学 | Method for rapidly measuring concentration of hydrogen peroxide |
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| CN101451957A (en) * | 2008-12-17 | 2009-06-10 | 上海和黄药业有限公司 | Method for detecting anthraquinone content in medicaments |
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| CN101451957A (en) * | 2008-12-17 | 2009-06-10 | 上海和黄药业有限公司 | Method for detecting anthraquinone content in medicaments |
| CN103760160A (en) * | 2014-01-25 | 2014-04-30 | 福州大学 | Colorimetric detection method of hydrogen peroxide |
| CN104280516A (en) * | 2014-09-20 | 2015-01-14 | 中山鼎晟生物科技有限公司 | Rapid detection kit and detection method for phenolphthalein in diet food |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112649556A (en) * | 2020-11-13 | 2021-04-13 | 新疆大学 | Method for rapidly measuring concentration of hydrogen peroxide |
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