A kind of sulfur dioxide quick detection reagent pipe and detection method thereof
Technical field
The present invention relates to a kind of detection Reagent Tube, and the detection method of content of sulfur dioxide, specifically, relate to a kind of content of sulfur dioxide quick detection reagent pipe, and the detection method of sulfur dioxide in food.
Background technology
In the process of manufacture of food, its distinctive color and luster is kept for making food, manufacturer often adds the color and luster control groups such as bleaching agent and divides, and the oxidation relying on it to have or reducing power suppress, destroy the variable color factor of food, food is faded or avoids brown stain occurs.In China's food service industry, use more component to be sulfur dioxide and sulphite, this kind of component has certain corrosiveness, and in food, excessive use can affect health.Especially sulfur dioxide, it is effectively bleached and antisepsis food, bleaching agent conventional in food processing and anticorrisive agent, but, Use out of range sulfur dioxide class additive, intestines and stomach will be damaged, cause feeling sick, vomiting, also can affect the absorption of calcium, therefore sulfur dioxide has strict consumption control as food additives, China in " food additives use sanitary standard " (GB2760-2011) to drinks, carbohydrate, native article, preserved fruit, in the food such as starch, the maximum use amount of bleaching agent has made regulation, in sulfur dioxide residue limits for 0.01-0.4g/L (kg) not etc.
Domestic the administration for industry and commerce and quality supervised department once repeatedly found individual traders and pedlars or some the food enterprises of some areas, in order to pursue its product, there is good appearance luster, or extend the packaging for foodstuff time limit, or for covering poor quality food, Misuse or Use out of range sulfur dioxide class additive in food.The poisoned food that retailers' bold production sulfur dioxide why like this exceeds standard, mainly because the detection means too backwardness of law enforcement agency, can not detect the sulfur dioxide composition in food on a large scale, fast.There is complex operation in traditional pararosaniline hydrochloridc colorimetric method, sensitivity is low, color development system is unstable, poor reproducibility, often causes testing result to occur comparatively big error.Therefore, on market, the method and technological means thereof that detect the content of sulfur dioxide in food are fast set up in active demand.
Summary of the invention
The invention discloses a kind of simple and easy to do sulfur dioxide detection method, invent coherent detection reagent and detector tube.
The present invention's reagent used is important component part of the present invention, mainly comprises:
Solution A: the two fluoroform sulfimide salt 0.5-1mL of formaldehyde 10-100mL+1-ethyl-3-methylimidazole, adds water and be settled to 1000mL.
B solution: pararosaniline hydrochloridc 0.1-2g+ hydrochloric acid 100-500mL, adds water and be settled to 1000mL.
The invention provides a kind of integrated, reagent sealing good, be convenient to transport, the steps such as multicomponent reagent pipetting volume, reaction, colorimetric are carried out continuously quick combination simultaneously, safer, easy, detect Reagent Tube accurately and rapidly.This detection Reagent Tube effectively overcomes the limitation that traditional test in laboratory instrument volume is comparatively large, cost is high, analytical method is complicated, can meet the quick detection demand of the units such as supervision law enforcement agency and wholesale market, supermarket, dining room, hotel etc. such as quality supervision, industry and commerce, agricultural, health.
This detection Reagent Tube comprises: reagent cup and reaction cup, reagent cup is connected by plastic tape with reaction cup, wherein reagent cup is divided into two chambeies, fill solution A 500uL in chamber 1, in chamber 2, fill B solution 500uL, by aluminium foil, chamber 1 and chamber 2 are sealed, the size of reagent cup bottom opening is less than or equal to the open-topped size of reaction cup, make the lower end of reagent cup can the inner chamber of intercalation reaction cup, be provided with two root thorn pins in reaction cup, two root thorn pins be corresponding with the chamber 1 of reagent cup and chamber 2 respectively.
The using method detecting Reagent Tube is as follows:
Sample detection and result judge
1) sample is added: get 1g testing sample and join in reaction cup, add 3mL water.
2) reagent adding: enter in reaction cup by reagent cup back-off, firmly press down, reagent is sealed aluminium foil and punctures by pricker, and reagent flows in reaction cup.
3) react: pressure-vaccum mixes, and room temperature leaves standstill 1min-10min.
4) result interpretation: with the content of sulfur dioxide in standard color comparison card colorimetric determination sample: reactant liquor is not containing sulfur dioxide in faint yellow interpret sample, in blue or bluish violet interpret sample containing sulfur dioxide, color is darker, and content of sulfur dioxide is higher.
The making of sulfur dioxide examination criteria colorimetric card:
Get the detection Reagent Tube that 12 embodiments 1 are obtained, respectively to adding 0.0 in reaction cup, 0.1,0.2,0.5,1.0,2.0,4.0,8.0,12.0,16.0,20.0,32.0mg/kg sulfur dioxide standard liquid 3.0mL.Enter in reaction cup by mentioned reagent cup back-off, firmly press down, reagent is sealed aluminium foil and punctures by pricker, and reagent flows in reaction cup.Pressure-vaccum mixes, and room temperature leaves standstill 5min, makes sulfur dioxide examination criteria colorimetric card.
The advantage that the present invention has and good effect are: adopt prefabricated integrated reagent, without the need to extemporaneous preparation, improve operating efficiency; Operating personnel are avoided directly to contact chemicals, safe and reliable; Without the need to using any instrument and auxiliary equipment, consume low; Highly sensitive, meet national examination criteria requirement; Naked eyes contrast color judges testing result, simple and clear; Detector tube deft design is unique, good looking appearance.Adopt the two fluoroform sulfimide salt of 1-ethyl-3-methylimidazole as SO
2absorbent, on the one hand effectively can absorb SO
2, make SO as stabilizing agent on the other hand
2stablize with the chromogenic reaction of pararosaniline hydrochloridc and formaldehyde, color clear, can not pass in time and change, and without the need to adding stabilizing agent in addition again, the detection limit of sulfur dioxide can be reduced to 0.3mg/kg, sensitiveer, favorable reproducibility, and testing result is stablized.
The invention belongs to technical field of food safety detection, be mainly used in the quick detection of content of sulfur dioxide in food samples.The applying unit mainly national law enforcement of checkout gear of the present invention, as the administration for industry and commerce, hygiene department, quality supervision department, commodity inspection and epidemic prevention department etc., food processing enterprises also have wilderness demand to this technology and product in control of product quality.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Fig. 2 is the use procedure schematic diagram that the present invention detects Reagent Tube.
In figure:
1-reagent cup 2-reaction cup 3-chamber 1
4-chamber 2 5-pricker
Detailed description of the invention
Embodiment 1
The compound method of solution is as follows:
Solution A: the two fluoroform sulfimide salt 0.5mL of formaldehyde 40mL+1-ethyl-3-methylimidazole, adds water and be settled to 1000mL.
B solution: pararosaniline hydrochloridc 0.5g+ hydrochloric acid 100mL, adds water and be settled to 1000mL.
As shown in Figure 1, a kind of Reagent Tube that detects comprises: reagent cup and reaction cup, reagent cup is connected by plastic tape with reaction cup, wherein reagent cup is divided into two chambeies, solution A 500uL is filled in chamber 1, B solution 500uL is filled in chamber 2, by aluminium foil, chamber 1 and chamber 2 are sealed, the size of reagent cup bottom opening is less than or equal to the open-topped size of reaction cup, make the lower end of reagent cup can the inner chamber of intercalation reaction cup, making reagent encapsulate cup lower end can the inner chamber of intercalation reaction cuvette, two root thorn pins are provided with in reaction cup, two root thorn pins are corresponding with the chamber 1 of reagent cup and chamber 2 respectively.
Embodiment 2
The making of sulfur dioxide examination criteria colorimetric card:
Get the detection Reagent Tube that 12 embodiments 1 are obtained, respectively to adding 0.0 in reaction cup, 0.1,0.2,0.5,1.0,2.0,4.0,8.0,12.0,16.0,20.0,32.0mg/kg sulfur dioxide standard liquid 3.0mL.Enter in reaction cup by reagent cup back-off, firmly press down, reagent is sealed aluminium foil and punctures by pricker, and reagent flows in reaction cup.Pressure-vaccum mixes, and room temperature leaves standstill 5min, makes sulfur dioxide examination criteria colorimetric card.
Embodiment 3
Application examples: the white granulated sugar sample choosing 10 manufacturer production, measures its content of sulfur dioxide by this law and National Standard Method respectively.
Add sample: get 1g testing sample and join in reaction cup, add 3mL distilled water.
Reagent adding: enter in reaction cup by the reagent cup back-off of embodiment 1, firmly press down, reagent is sealed aluminium foil and punctures by pricker, reagent flows in reaction cup.
Reaction: pressure-vaccum mixes, and room temperature leaves standstill 5min.
Testing result sees table 1, and this law can detect the content range of sulfur dioxide substantially, and its detection limit can reach 0.3mg/kg, can detect the content of sulfur dioxide fast, as needed accurately to detect, can use absorption photometric instrument auxiliary detection.
Sample |
This law (mg/kg) |
National Standard Method (mg/kg) |
1 |
24-32 |
29.80 |
2 |
12-24 |
22.03 |
3 |
12-24 |
18.93 |
4 |
12-24 |
19.08 |
5 |
24-32 |
30.96 |
6 |
32-60 |
33.85 |
7 |
24-32 |
26.74 |
8 |
3-6 |
5.08 |
9 |
6-12 |
10.63 |
10 |
12-24 |
13.95 |
Embodiment 4
The compound method of solution is as follows:
Solution A: the two fluoroform sulfimide salt 2mL of formaldehyde 50mL+1-ethyl-3-methylimidazole, adds water and be settled to 1000mL.
B solution: pararosaniline hydrochloridc 2g+ hydrochloric acid 200mL, adds water and be settled to 1000mL.
Detect in the chamber 1 of Reagent Tube and fill solution A 500uL, fill B solution 500uL in chamber 2 and obtain detecting Reagent Tube.
Embodiment 5
The making of sulfur dioxide examination criteria colorimetric card:
Get the detection Reagent Tube that 12 embodiments 4 are obtained, respectively to adding 0.0 in reaction cup, 0.1,0.2,0.5,1.0,2.0,4.0,8.0,12.0,16.0,20.0,32.0mg/kg sulfur dioxide standard liquid 3.0mL.Enter in reaction cup by reagent cup back-off, firmly press down, reagent is sealed aluminium foil and punctures by pricker, and reagent flows in reaction cup.Pressure-vaccum mixes, and room temperature leaves standstill 5min, makes sulfur dioxide examination criteria colorimetric card.
Embodiment 6
Application examples: detect bean vermicelli and bamboo shoots containing amount of sulfur dioxide
Add sample: get 1g testing sample and join in reaction cup, add 3mL distilled water.
Reagent adding: enter in reaction cup by the reagent cup back-off of embodiment 4, firmly press down, reagent is sealed aluminium foil and punctures by pricker, reagent flows in reaction cup.
Reaction: pressure-vaccum mixes, and room temperature leaves standstill 5min.
Detect that containing amount of sulfur dioxide in bean vermicelli is 6-12mg/kg, containing amount of sulfur dioxide in bamboo shoots is 24-32mg/kg.
Embodiment 7
Replica test is tested
Get the sulfur dioxide standard liquid 3.0mL of 5 parts of 4.0mg/kg in the reaction cup of embodiment 1, enter in reaction cup by reagent cup back-off, firmly press down, reagent is sealed aluminium foil and punctures by pricker, and reagent flows in reaction cup.Pressure-vaccum mixes, and room temperature leaves standstill 5min.
Colour developing result indifference, solid colour, can draw thus and adopt method of the present invention to detect sulfur dioxide, color development system is stablized, favorable reproducibility.