CN102735739A - Electrochemical method for detecting banned additive urotropin in food - Google Patents
Electrochemical method for detecting banned additive urotropin in food Download PDFInfo
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- CN102735739A CN102735739A CN2012102317750A CN201210231775A CN102735739A CN 102735739 A CN102735739 A CN 102735739A CN 2012102317750 A CN2012102317750 A CN 2012102317750A CN 201210231775 A CN201210231775 A CN 201210231775A CN 102735739 A CN102735739 A CN 102735739A
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Abstract
The invention relates to an electrochemical method for detecting banned additive urotropin in food, which comprises the following steps of: respectively and simultaneously inserting a working electrode carbon paste electrode, a reference electrode saturated calomel electrode and a counter electrode platinum sheet into 0.1mol.L-1PBS (Phosphate Buffer Solution) buffer solution to carry out differential pulse voltammetry scanning to obtain the oxidation peak current value of the urotropin, wherein the pH of the buffer solution is 6, the buffer solution contains a series of urotropin standard solution in different concentrations, and the oxidation peak current value and the concentration of the urotropin have a good linear relationship; with the same method, the oxidation peak current value of the sample solution is obtained; and according to a standard curve and a corresponding linear regression equation, the density of the urotropin in the sample is obtained. The method is simple in operation, is convenient and quick and has a low detection cost, and the urotropin can be directly detected.
Description
Technical field
The present invention relates to the food inspection technical field, particularly a kind of electrochemical detection method that detects the adjuvant urotropine of violating a ban in the food.
Background technology
Urotropine (HMTA) another name hexamethylene tetramine, it can be used as corrosion inhibiter, hardening agent, anti-piping compound and germifuge etc.Urotropine itself is a low toxicity, but under the condition of weak acid, urotropine can decomposite the formaldehyde with toxicity, and formaldehyde is also reducible in vivo simultaneously is methyl alcohol, so also show the toxicological effect of methyl alcohol.The kidney of human body, liver, nervous centralis, immunologic function, digestive system etc. all there is infringement.
Because in recent years; Domestic repeatedly the report detects urotropine and causes a series of food security incident from food such as bean curd stick, bean vermicelli, rice noodles, aquatic products; Therefore urotropine is classified as in the non-edible material from soybeans and the food additives list that is prone to abuse of illegal interpolation " in the food maybe " already, is expressly forbidden adding in the middle of the food or uses in the processed food process.
At present both at home and abroad the detection method of relevant urotropine mainly contains neutralisation, Nesslerization, non-aqueous titration, ultraviolet spectrophotometry, vapor-phase chromatography, high performance liquid chromatography, reversed-phased high performace liquid chromatographic method etc., in the above-mentioned method or complicated operation or used expensive instrument.Ma Huailing etc. (Ma Huailing, Xu Maotian, Song Shengmei etc. beta-schardinger dextrin--H
2O
2There is polarogram catalysis method mensuration hexamethylenetetramine [J] down, assay office, 2005,7 (7): 32～34) reported once that urotropine was a kind of non-electroactive compound, and during individualism, can not directly measure, beta-schardinger dextrin--H with electrochemical method
2O
2Exist down, adopt the polarogram catalysis method to measure hexamethylenetetramine.And (girth profit such as girth profit; Luo Chuannan, Shou Chongqi etc. cyclodextrin-hexamethylenetetramine supramolecular complex electrochemical research and application [J], analytical chemistry; 2003,5 (5): 566～568) studied cyclodextrin and hexamethylenetetramine supramolecular complex electrochemical behavior.Thereby above-mentioned electrochemical method all is to form supramolecular complex indirect detection urotropine through urotropine and beta-schardinger dextrin-, and the DME that uses simultaneously can pollute environment.So the content of setting up urotropine in the simple fast directly method mensuration food is very to be necessary.
Summary of the invention
The technical matters that the present invention will solve is to detecting at present the adjuvant urotropine method complicated operation of violating a ban, and cost provides a kind of simple to operate than problems such as height, and is fast convenient, and it is low to detect cost, the electrochemical method that can directly detect urotropine simultaneously.
In order to address the above problem, the technical scheme that the present invention adopts is: a kind of electrochemical method that detects the adjuvant urotropine of violating a ban in the food is characterized in that may further comprise the steps:
(1) preparation of working electrode
Accurately take by weighing dag that mass ratio is 97:3 and paraffin wax in beaker; Be heated to the complete fusion of paraffin; With continuous stirring of glass bar both are mixed simultaneously, to be cooled to room temperature, said mixture is inserted in the electrode; After electrode surface compressed and polish, promptly get the working electrode carbon paste electrode after rinsing well with deionized water;
(2) drafting of typical curve
With the working electrode carbon paste electrode in the step (1), contrast electrode saturated calomel electrode with the electrode platinized platinum is inserted pH simultaneously is 6 the 0.1molL that contains a series of variable concentrations urotropine standard solution
-1Carry out electro-chemical test in the PBS buffer solution, under identical test condition, write down the pairing peak point current of each concentration and be depicted as typical curve, and then obtain the corresponding linear regression equation;
(3) mensuration of sample
Getting the 2.0mL testing sample solution, is 6 0.1molL at pH
-1Carry out electro-chemical test in the PBS buffer solution, then the peak point current that obtains is updated in the equation of linear regression that step (2) obtains, can obtain the concentration of urotropine in the testing sample.
As to qualification of the present invention; A series of variable concentrations standard solution described in the step (2) prepare according to following method: accurately take by weighing the 0.1402g urotropine in beaker; After the adding deionized water dissolves it fully; Be moved into constant volume in the 100mL volumetric flask, be diluted to variable concentrations 3.0x10 with deionized water then
-5MolL
-1, 5.0x10
-5MolL
-1, 1.0x10
-4MolL
-1, 3.0x10
-4MolL
-1, 5.0x10
-4MolL
-1, 7.0x10
-4MolL
-1, 1.0x10
-3MolL
-1, 2.0x10
-3MolL
-1, 2.5x10
-3MolL
-1, 3.0x10
-3MolL
-1, 4.0x10
-3MolL
-1And 5.0x10
-3MolL
-1Described electrochemical test method is a differential pulse voltammetry, and test condition is: initial potential is 1.3V, and the termination current potential is 1.7V, and the current potential increment is 0.05V, and pulse width is 0.05S, and the recurrence interval is 0.2S, and time of repose is 2S, is 6 0.1molL with pH
-1PBS buffer solution is as supporting electrolyte.
As to further qualification of the present invention, the peak point current described in step (2) and the step (3) is the oxidation peak current value; Described PBS buffer solution prepares by following method:
I: 0.5molL
-1NaH
2PO
4The preparation of solution: take by weighing 19.50g NaH
2PO
42H
2O behind deionized water dissolving, is moved into constant volume in the volumetric flask of 250mL in beaker, shake up for use;
II: 0.5molL
-1Na
2HPO
4Preparation: take by weighing 8.95g Na
2HPO
412H
2O behind deionized water dissolving, is moved into constant volume in the volumetric flask of 50mL in beaker, shake up for use;
The solution that above-mentioned steps (I) and step (II) are obtained promptly gets 0.5molL by volume for 212.5:37.5 mixes
-1PBS solution, but time spent suitable dilution.
As step qualification more of the present invention, the testing sample described in the step (3) is handled by following method: take by weighing sample 4.0g, pulverizing is placed in the 100mL beaker; Add the 10mL ethanolic solution, soak 30min, ultrasonic 30min; Filter then, get supernatant constant volume in the 100mL volumetric flask.
After having adopted above-mentioned technical scheme, with 0.1molL
-1PBS buffer solution is done in the measurement system of supporting electrolyte; With differential pulse voltammetry the urotropine standard solution of a series of variable concentrations is carried out electro-chemical test; One tangible oxidation peak has appearred at scanning voltage 1.47V place; This oxidation peak current corresponding value presents linear relationship well with the concentration of its corresponding urotropine, and the gained typical curve is sectional curve (like Figure of description Fig. 2), when concentration is 3.0x10
-5MolL
-1～7.0x10
-4MolL
-1The time (concentration as corresponding respectively among Figure of description Fig. 2 is 3.0x10
-5MolL
-1, 5.0x10
-5MolL
-1, 1.0x10
-4MolL
-1, 3.0x10
-4MolL
-1, 5.0x10
-4MolL
-1, 7.0x10
-4MolL
-1), i
p=100.2C-1.265, coefficient R
2=0.9903; When concentration is 7.0x10
-4MolL
-1～5.0x10
-3MolL
-1The time (concentration as corresponding respectively among Fig. 2 is 7.0x10
-4MolL
-1, 1.0x10
-3MolL
-1, 2.0x10
-3MolL
-1, 2.5x10
-3MolL
-1, 3.0x10
-3MolL
-1, 4.0x10
-3MolL
-1And 5.0x10
-3MolL
-1), i
p=17.53C+60.21, coefficient R
2=0.9978.Wherein C is the concentration of urotropine in the standard solution, i
pBe oxidation peak current.Replicate determination 1.0x10
-4MolL
-1Urotropine standard solution 6 times, gained relative standard deviation RSD is 2.9%, explains that this electrode has good reappearance.
After adopting technique scheme, the present invention has the following advantages:
(1) working electrode is a carbon paste electrode, and this electrode production process is simple, stable performance, and have good reappearance.
(2) use carbon paste electrode can realize that the Direct Electrochemistry of urotropine detects, realized fast detecting, make the testing process of each sample only need a few minutes to accomplish, and it is low to detect cost.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is further specified.
Fig. 1 is the oxidation peak current curve map of urotropine standard solution on carbon paste electrode of variable concentrations;
Fig. 2 is the oxidation peak current of urotropine standard solution on carbon paste electrode and the canonical plotting of its corresponding concentration of variable concentrations.
Embodiment
In order to be illustrated more clearly in content of the present invention, below in conjunction with concrete embodiment the present invention is further described, but will be appreciated that, these embodiment are merely the usefulness that illustrates, and should not be interpreted as the restriction that the present invention implements.
(1) the employed water of experimentation is deionized water, test used reagent be analyze pure.
(2) employed instrument of present embodiment and reagent:
Electrochemical workstation CHI411A (Shanghai occasion China instrument company) is used for the experiment of differential pulse voltammetry, and the accurate digital display acidometer of pHS-2C type (the healthy and free from worry electrooptical technology in Shanghai company limited) is used for the pH of regulator solution.Three-electrode system: working electrode is carbon paste electrode (dag/paraffin), and contrast electrode is a saturated calomel electrode, is platinum electrode to electrode.
Embodiment 1
According to the urotropine concentration in the following steps working sample:
(1) preparation of working electrode
Accurately take by weighing dag that mass ratio is 97:3 and paraffin wax in beaker; Be heated to the complete fusion of paraffin; With continuous stirring of glass bar both are mixed simultaneously, to be cooled to room temperature, said mixture is inserted in the electrode; After electrode surface compressed and polish, promptly get the working electrode carbon paste electrode after rinsing well with deionized water;
(2) drafting of typical curve
With the working electrode carbon paste electrode in the step (1), contrast electrode saturated calomel electrode with the electrode platinized platinum is inserted pH simultaneously is a series of variable concentrations urotropine standard solution (3.0x10 that contain of 6
-5MolL
-1, 5.0x10
-5MolL
-1, 1.0x10
-4MolL
-1, 3.0x10
-4MolL
-1, 5.0x10
-4MolL
-1, 7.0x10
-4MolL
-1, 1.0x10
-3MolL
-1, 2.0x10
-3MolL
-1, 2.5x10
-3MolL
-1, 3.0x10
-3MolL
-1, 4.0x10
-3MolL
-1And 5.0x10
-3MolL
-1) 0.1molL
-1Carry out electro-chemical test in the PBS buffer solution, under identical test condition, write down the pairing peak point current of each concentration and be depicted as typical curve, and then obtain the corresponding linear regression equation; Two equations of linear regression are arranged: concentration is 3.0x10
-5MolL
-1～7.0x10
-4MolL
-1The time, i
p=100.2C-1.265, coefficient R
2=0.9903; Concentration is 7.0x10
-4MolL
-1～5.0x10
-3MolL
-1The time, i
p=17.53C+60.21, coefficient R
2=0.9978.
(3) mensuration of testing sample
Take by weighing commercially available bean curd stick sample 4.0g, pulverizing is placed in the 100mL beaker, adds the 10mL ethanolic solution, soaks 30min, and ultrasonic 30min filters then, gets supernatant constant volume in the 100mL volumetric flask.
Getting the above-mentioned testing sample solution of 2.0mL, is 6 0.1molL at pH
-1In the PBS supporting electrolyte, carry out electro-chemical test,, calculate the concentration of urotropine in institute's test sample article according to the current value and the pairing equation of linear regression of typical curve of scanning gained according to the method and the step of " typical curve drafting " among the embodiment 1.Mensuration result shows that near 1.47V, do not observe oxidation peak current, promptly measured current value is approximately 0 μ A in the sample, does not contain the food additives urotropine of violating a ban thus in the judgement sample.In above-mentioned testing sample solution, add the 1.0x10 of 1.0mL respectively
-2MolL
-1, 3.0x10
-2MolL
-1And 5.0x10
-2MolL
-1The urotropine standard solution, make that the concentration of the urotropine that added in the sample solution is 1.0x10
-4MolL
-1(14.02 μ gmL
-1), 3.0x10
-4MolL
-1(42.05 μ gmL
-1) and 5.0x10
-4MolL
-1(70.09 μ gmL
-1), under the same test condition, detecting, and calculate its recovery of standard addition, its result is as shown in table 1.
Certain brand bean curd stick recovery of standard addition of table 1 is measured result (n=3)
The sample detection method that following examples 2 adopt is identical with embodiment 1, and the accepted standard curve is also identical with embodiment 1 with equation of linear regression.
Embodiment 2
Sample source: bean vermicelli is sold in certain supermarket
Take by weighing commercially available bean vermicelli sample 4.0g, pulverizing is placed in the 100mL beaker, adds the 10mL ethanolic solution, soaks 30min, and ultrasonic 30min filters then, gets supernatant constant volume in the 100mL volumetric flask.
Getting the above-mentioned testing sample solution of 2.0mL, is 6 0.1molL at pH
-1In the PBS supporting electrolyte, carry out electro-chemical test,, calculate the concentration of urotropine in institute's test sample article according to measured current value and the pairing equation of linear regression of typical curve according to the method and the step of " typical curve drafting " among the embodiment 1.Mensuration result shows that near 1.47V, do not observe oxidation peak current, promptly measured current value is approximately 0 μ A in the sample, does not contain the food additives urotropine of violating a ban thus in the judgement sample.In above-mentioned testing sample solution, add the 1.0x10 of 1.0mL respectively
-2MolL
-1, 3.0x10
-2MolL
-1And 5.0x10
-2MolL
-1The urotropine standard solution, make that the concentration of the urotropine that added in the sample solution is 1.0x10
-4MolL
-1(14.02 μ gmL
-1), 3.0x10
-4MolL
-1(42.05 μ gmL
-1) and 5.0x10
-4MolL
-1(70.09 μ gmL
-1), under the same test condition, detecting, and calculate its recovery of standard addition, its result is as shown in table 2.
Certain brand bean vermicelli recovery of standard addition of table 2 is measured result (n=3)
Based on above-mentioned test result, can see that the method for the food interpolation urotropine of violating a ban in the Electrochemical Detection food of the present invention is simple to operate, fast convenient, it is low to detect cost, has realized the electrochemical method to the direct detection of urotropine simultaneously.The foregoing description only is used to explain content of the present invention, but this is not to be limitation of the present invention.
Claims (5)
1. electrochemical method that detects in the food adjuvant urotropine of violating a ban is characterized in that may further comprise the steps:
(1) preparation of working electrode
Accurately take by weighing dag that mass ratio is 97:3 and paraffin wax in beaker; Be heated to the complete fusion of paraffin; With continuous stirring of glass bar both are mixed simultaneously, to be cooled to room temperature, said mixture is inserted in the electrode; After electrode surface compressed and polish, promptly get the working electrode carbon paste electrode after rinsing well with deionized water;
(2) drafting of typical curve
With the working electrode carbon paste electrode in the step (1), contrast electrode saturated calomel electrode with the electrode platinized platinum is inserted pH simultaneously is 6 the 0.1molL that contains a series of variable concentrations urotropine standard solution
-1Carry out electro-chemical test in the PBS buffer solution, under identical test condition, write down the pairing peak point current of each concentration and be depicted as typical curve, and then obtain the corresponding linear regression equation;
(3) mensuration of sample
Getting the 2.0mL testing sample solution, is 6 0.1molL at pH
-1Carry out electro-chemical test in the PBS buffer solution, then the peak point current that obtains is updated in the equation of linear regression that step (2) obtains, can obtain the concentration of urotropine in the testing sample.
2. a kind of electrochemical method that detects the adjuvant urotropine of violating a ban in the food as claimed in claim 1 is characterized in that the concentration of the described a series of variable concentrations urotropine standard solution of step (2) is respectively 3.0x10
-5MolL
-1, 5.0x10
-5MolL
-1, 1.0x10
-4MolL
-1, 3.0x10
-4MolL
-1, 5.0x10
-4MolL
-1, 7.0x10
-4MolL
-1, 1.0x10
-3MolL
-1, 2.0x10
-3MolL
-1, 2.5x10
-3MolL
-1, 3.0x10
-3MolL
-1, 4.0x10
-3MolL
-1And 5.0x10
-3MolL
-1
3. a kind of electrochemical method that detects the adjuvant urotropine of violating a ban in the food as claimed in claim 1 is characterized in that the described electrochemical test method of step (2) is a differential pulse voltammetry, and test condition is: initial potential is 1.3V; The termination current potential is 1.7V; The current potential increment is 0.05V, and pulse width is 0.05S, and the recurrence interval is 0.2S; Time of repose is 2S, is 6 0.1molL with pH
-1PBS buffer solution is as supporting electrolyte.
4. a kind of electrochemical method that detects the adjuvant urotropine of violating a ban in the food as claimed in claim 1 is characterized in that the peak point current described in step (2) and the step (3) is the oxidation peak current value.
5. a kind of electrochemical method that detects the adjuvant urotropine of violating a ban in the food as claimed in claim 1; It is characterized in that the described testing sample of step (3) handles by following method: take by weighing sample 4.0g, pulverize and be placed in the beaker, add the 10mL ethanolic solution; Soak 30min; Ultrasonic 30min filters then, gets supernatant constant volume in the 100mL volumetric flask.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104849451A (en) * | 2015-05-08 | 2015-08-19 | 河北大学 | Detection kit of hexamethylene tetramine, detection method and application |
| CN106546582A (en) * | 2016-11-04 | 2017-03-29 | 东莞市食品药品检验所 | The quick detection reagent and method of hexamethylenamine in food |
| CN111458361A (en) * | 2020-01-06 | 2020-07-28 | 中国地质大学（北京） | Portable XRF-based method for measuring content of elements in leech |
| CN113252762A (en) * | 2021-04-13 | 2021-08-13 | 西北农林科技大学 | Method for rapidly detecting special virgin olive oil adulterated olive pomace oil |
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| CN102042977A (en) * | 2010-10-19 | 2011-05-04 | 广西师范大学 | Method for indirectly measuring formaldehyde content of air or water by adopting capillary electrophoresis and Rucbpy electrochemiluminescence |
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| CN102042977A (en) * | 2010-10-19 | 2011-05-04 | 广西师范大学 | Method for indirectly measuring formaldehyde content of air or water by adopting capillary electrophoresis and Rucbpy electrochemiluminescence |
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| M.A.KOUPPARIS等: "kinetic determination of formaldehyde and hexamethylenetetramine with a cyanide-selective electrode", 《ANALYTICA CHIMICA ACTA》 * |
| ZDENKA MARTINKOVÁ等: "Determination of Hexamine in the Dithane DG Fungicide Using Capillary Isotachophoresis", 《SENSING IN ELECTROANALYSIS》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104849451A (en) * | 2015-05-08 | 2015-08-19 | 河北大学 | Detection kit of hexamethylene tetramine, detection method and application |
| CN106546582A (en) * | 2016-11-04 | 2017-03-29 | 东莞市食品药品检验所 | The quick detection reagent and method of hexamethylenamine in food |
| CN111458361A (en) * | 2020-01-06 | 2020-07-28 | 中国地质大学（北京） | Portable XRF-based method for measuring content of elements in leech |
| CN113252762A (en) * | 2021-04-13 | 2021-08-13 | 西北农林科技大学 | Method for rapidly detecting special virgin olive oil adulterated olive pomace oil |
| CN113252762B (en) * | 2021-04-13 | 2022-12-13 | 西北农林科技大学 | Method for rapidly detecting special virgin olive oil adulterated olive pomace oil |
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|---|---|
| CN102735739B (en) | 2014-01-08 |
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Granted publication date: 20140108 Termination date: 20160705 |