CN110907440A - Rapid quantitative detection method for sulfur dioxide - Google Patents
Rapid quantitative detection method for sulfur dioxide Download PDFInfo
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Abstract
The invention relates to a sulfur dioxide rapid quantitative detection method, which effectively solves the problem of rapid, effective and accurate quantitative detection of sulfur dioxide content in food and medicinal materials, and is characterized in that a sample to be detected is made into a sample solution to be detected, a sulfur dioxide quantitative detection card is taken out and inserted into a sulfur dioxide rapid detection reaction bottle cap, and the sample solution to be detected and zinc powder are added into the reaction bottle; wetting a reaction hole on the detection card by using a wetting solution, adding an HCl solution into a reaction bottle, sealing, placing the reaction bottle in a constant-temperature constant-humidity reactor for oscillation reaction, and measuring the content of sulfur dioxide in a sample to be detected by using a handheld sulfur dioxide quantitative analyzer; preparing a gradient sodium sulfite standard solution, and drawing a concentration gray standard curve; the detector compares the measured values of the color spots with different depths obtained by the detection reaction with a standard curve, and rapidly and quantitatively detects the content of sulfur dioxide in the food or the medicinal materials. The measuring method of the invention is scientific, rapid and accurate, is not interfered by the color of the sample, and has great economic and social benefits.
Description
Technical Field
The invention relates to the field of medicine and food safety, in particular to a rapid quantitative detection method for sulfur dioxide.
Background
Sulfur dioxide has bleaching property, is often used for processing food by some manufacturers, and leads the selling phase of the food to be more accordant with the will of consumers; after the medicinal materials are fumigated by sulfur, the sulfur and oxygen are combined to form sulfur dioxide. After consumers use the food or the medicinal materials, the liver and the kidney of the human body are seriously damaged and the food or the medicinal materials have carcinogenic effect.
At present, devices, instruments and methods for detecting sulfur dioxide are various, but due to various reasons, the using effect is unsatisfactory, and especially, the content of sulfur dioxide residues in detected food and medicinal materials cannot be accurately and quickly quantified, so that the quality of the detected food and medicinal materials cannot be accurately evaluated and effectively supervised, and the harm of the sulfur dioxide residues to the health of people cannot be scientifically and effectively prevented, and therefore, how to quickly, effectively and accurately quantitatively detect the content of sulfur dioxide in the food and medicinal materials is a necessary technical problem to be solved.
Disclosure of Invention
In view of the above situation, the present invention aims to provide a method for rapidly and quantitatively detecting sulfur dioxide, which can effectively solve the problem of rapidly, effectively and accurately quantitatively detecting the content of sulfur dioxide in food and medicinal materials.
The invention solves the technical scheme that a sulfur dioxide rapid quantitative detection method uses a set of sulfur dioxide quantitative detection system, which mainly comprises (1) a constant temperature and humidity reactor, (2) a sulfur dioxide rapid detection reaction bottle cap, (3) a sulfur dioxide quantitative detection card, (4) a sulfur dioxide quantitative detection reaction reagent, (5) a sulfur dioxide quantitative detection analysis IC card, and (6) equipment instruments and devices of a sulfur dioxide quantitative analyzer, wherein the detection operation comprises the following steps:
(1) preparing a sample:
the sample is a Chinese medicinal material to be detected, a Chinese patent medicine, a Chinese medicinal decoction piece or various food samples, the sample to be detected is cut or crushed into powder, the solid powder and the extraction liquid are placed in an extraction bottle according to the weight-volume ratio of 1:2 to 1:50, the liquid is shaken to soak the sample, the sample is soaked in water bath at 80 ℃, the water bath lasts for 20-30min, and the supernatant is taken out after standing, filtering or centrifuging, so that the sample liquid to be detected is obtained;
(2) and (3) detection:
taking out the sulfur dioxide quantitative detection card in the reagent box, inserting the sulfur dioxide quantitative detection card into a sulfur dioxide rapid detection reaction bottle cap, and adding 1mL of a sample to be detected and a certain amount of zinc powder into a reaction bottle; wetting the reaction wells on the test card with a wetting fluid; finally, a certain amount of HCl solution is transferred into a reaction bottle by a suction pipe, a reaction bottle cap inserted with a sulfur dioxide quantitative detection card is quickly covered, the reaction bottle cap is placed in a constant-temperature constant-humidity reactor with the temperature and the humidity controlled at 30 ℃ and 45% respectively and the rotating speed of 200r/min, the sulfur dioxide quantitative detection card is drawn out after oscillation reaction for 20min, and the reaction bottle is kept stand for 6-10 min; opening the hand-held sulfur dioxide quantitative analyzer, taking out the sulfur dioxide quantitative detection analysis IC card carried by the kit according to the operation instruction of the instrument, swiping the card to write a program, then inserting the sulfur dioxide quantitative detection analysis IC card into a card slot of the sulfur dioxide quantitative analyzer, selecting a corresponding program, and obtaining data after measurement, namely the content of sulfur dioxide in the sample to be measured;
when the detected sample makes the color of the detection card dark black, even silver gray crystals appear, the sulfur dioxide content in the sample is beyond the linear range of the measured value of the instrument, the error is increased due to direct measurement, and the sample to be detected needs to be diluted by water and then is detected again according to the step (2);
(3) drawing a standard curve:
when a batch of new detection cards are prepared, the new cards are used for redrawing the standard curve, and the step of drawing the standard curve comprises the following steps:
firstly, preparing a sodium sulfite standard solution: adding double distilled water into sodium sulfite to prepare gradient sodium sulfite standard solutions corresponding to different sulfur dioxide concentrations;
detecting sodium sulfite standard products with different concentration gradients by using the detection method, inserting test strips with different spot gray levels obtained by detection into a handheld sulfur dioxide quantitative analyzer, opening the analyzer, selecting a gray level detection program (GHX 201108080001), measuring gray levels of developed spots with different concentrations, detecting each concentration for 3 times, and averaging the gray levels; in an Excel worksheet, performing linear regression by taking a gray value as a vertical coordinate and a sulfur dioxide concentration value as a horizontal coordinate to obtain a concentration gray standard curve; inputting the parameters of the standard curve into an IC card through an IC card reader, namely a sulfur dioxide quantitative detection analysis card which is synchronous with the kit; when the detection is started, the sulfur dioxide quantitative detection analysis card carried in the reagent box is taken out, the card is placed at the back of the sulfur dioxide quantitative analyzer for reading the card, a detection program is selected, and the detector automatically compares the measured values of the color spots with different depths obtained by the detection reaction with a standard curve, so that the sulfur dioxide content in the food or the medicinal material can be quickly and quantitatively measured.
The measuring method is scientific, rapid and accurate, and can effectively solve the problem of rapid quantitative determination of sulfur dioxide content in food and traditional Chinese medicinal materials. The method can be used for quickly and preliminarily screening samples, provides convenience for detecting sulfur dioxide or sulfur dioxide residues added in foods and medicinal materials, provides a detection means for ensuring the safety of the foods and the medicines, can be widely applied to quickly and quantitatively detecting sulfur dioxide in foods such as vermicelli, biscuits, preserved fruits, dried fruits, chocolate and chocolate products, various dried vegetables and the like, traditional Chinese medicine decoction pieces and Chinese patent medicines, is not interfered by the color of the samples, is beneficial to the health of people, and has huge economic and social benefits.
Drawings
FIG. 1 is a graph of a gray scale level of the present invention.
FIG. 2 is a front view of the structure of the test card of the present invention.
FIG. 3 is a bottom view of the test card of the present invention.
FIG. 4 is a front view of a hand-held sulfur dioxide detector of the present invention.
FIG. 5 is a block diagram of the circuit of the hand-held sulfur dioxide detector of the present invention.
Detailed Description
The following detailed description of the embodiments of the present invention refers to the accompanying drawings.
The invention relates to a quantitative detection method of sulfur dioxide, which comprises the following steps:
(1) preparing a sample:
preparing a food sample: sampling food to be detected, cutting into pieces, crushing in a crusher, putting 5g of the powder into an extraction bottle, adding 5mL of NaOH solution with the volume concentration of 0.125%, tightly covering a cover, shaking to soak the sample with liquid, carrying out water bath at 80 ℃ for 20min, standing, filtering or centrifuging, and taking supernatant, namely the food liquid sample to be detected;
preparing a traditional Chinese medicine sample: the traditional Chinese medicine is a traditional Chinese medicine or a traditional Chinese medicine decoction piece, the traditional Chinese medicine is cut into pieces and then crushed in a crusher, the prepared rehmannia root or the medlar is cut into small millet particles by the scissors, 1g of the prepared rehmannia root or the medlar is weighed and placed in an extraction bottle, 5mL of NaOH solution with the volume concentration of 0.125 percent is added, a cover is tightly covered, the liquid is shaken to soak a sample, the mixture is subjected to water bath at the temperature of 80 ℃ for 20min and is kept stand for 40-60min, and the supernatant is taken to obtain a sample of the traditional Chinese medicine liquid to be detected;
(2) and (3) detection:
taking out the sulfur dioxide quantitative detection card, inserting one end with a positioning round hole into a sulfur dioxide rapid detection reaction bottle cap, enabling one end with a yellow adhesive tape to face upwards, sucking 1mL of a sample to be detected by using a suction pipe, placing the sample in a reaction bottle, adding 2 zinc particles, sucking 7 microlitre of wetting liquid by using a micropipettor, wherein the wetting liquid is prepared by Triton X-1001%, Tween-201%, 1% of glycerol and the balance of water, wetting a reaction hole on the sulfur dioxide quantitative detection card, sucking 1mL of HCl with the volume concentration of 20% into the reaction bottle by using the suction pipe, covering the reaction bottle cap on the reaction bottle, plugging, slightly shaking the reaction bottle to uniformly mix the liquid in the bottle, placing the reaction bottle in a constant-temperature and constant-humidity reactor with controllable temperature and humidity, reacting for 10-30min under the conditions of the rotation speed of 200r/min, the temperature of 20-30 ℃ and the humidity of 35-70%, and extracting the sulfur, balancing the room temperature for 6-10min, opening the handheld sulfur dioxide quantitative analyzer, taking out the sulfur dioxide quantitative detection analysis IC card carried by the kit according to the operation instruction of the analyzer, swiping the card for writing the program, then inserting the detection card into a card slot of the sulfur dioxide quantitative analyzer, selecting the corresponding program, and obtaining the data after measurement, namely the content of the sulfur dioxide in the sample to be measured;
(3) and (3) data judgment:
when the detected sample is food, if the color of the detection card is dark black, even silver gray crystals appear, the sulfur dioxide content of the sample is beyond the linear range of the measured value of the instrument, the numerical value detection is inaccurate, and the sample to be detected needs to be diluted by 5 times and then re-detected according to the step (2);
when the detected sample is a traditional Chinese medicine, if the color of the detection card is dark black, even silver gray crystals appear, the sulfur dioxide content of the sample is beyond the linear range of the measured value of the instrument, the numerical value detection is inaccurate, and the sample to be detected needs to be diluted by 5 times and then re-detected according to the step (2);
(4) drawing a standard curve:
when a batch of new detection cards are prepared, the new cards are used for redrawing the standard curve, and the step of drawing the standard curve comprises the following steps:
firstly, preparing a sodium sulfite standard solution: adding double distilled water into sodium sulfite to prepare gradient sodium sulfite standard solutions corresponding to different sulfur dioxide concentrations;
detecting sodium sulfite standard products with different concentration gradients by using the detection method, inserting test strips with different spot gray levels obtained by detection into a handheld sulfur dioxide quantitative analyzer, opening the analyzer, selecting a gray level detection program (GHX 201108080001), measuring gray levels of developed spots with different concentrations, detecting each concentration for 3 times, and averaging the gray levels; in an Excel worksheet, performing linear regression by taking a gray value as a vertical coordinate and a sulfur dioxide concentration value as a horizontal coordinate to obtain a concentration gray standard curve; inputting the parameters of the standard curve into an IC card through an IC card reader, namely a sulfur dioxide quantitative detection analysis card which is synchronous with the kit; when the detection is started, taking out the sulfur dioxide quantitative detection analysis card carried in the reagent box, and placing the card at the back of the sulfur dioxide quantitative analyzer for reading the card; selecting a detection program, and automatically comparing the measured values of the color spots with different depths obtained by the detection reaction with a standard curve by using a detector, so that the content of sulfur dioxide in the food or the medicinal material can be quickly and quantitatively measured.
In order to ensure the use effect and convenient use, the reaction temperature of the sulfur dioxide reactor is generally 25 ℃ and the volume humidity is 45 percent;
the detection card structure comprises a bottom plate, a surface protection film, a reaction layer and a double-sided adhesive layer, wherein the double-sided adhesive layer 4 is arranged on the middle part of the bottom plate 1, the integral reaction layer 3 is bonded on the double-sided adhesive layer 4, two ends of the reaction layer 3 are fixed on the bottom plate 1 through symmetrical fixing pressing strips 2, a reaction hole 6 is formed in the middle part of the bottom plate, a positioning hole 5 is formed in one end of the bottom plate, a through hole corresponding to the reaction through hole 6 in the bottom plate is formed in the middle part of the double-sided adhesive layer 4 and is communicated with the reaction layer 3, and the integral surface protection layer covers the bottom plate, the;
the sulfur dioxide quantitative analyzer is a hand-held sulfur dioxide quantitative analyzer and structurally comprises an upper shell 7 and a handle 8 which is connected with the upper shell into a whole, wherein a liquid crystal display screen 10 is arranged at the front part of the upper shell, a detection card insertion hole 9 is formed in the side surface of the upper shell, a keyboard 12 for controlling the working state is arranged at the front part of the handle, the keyboard is composed of a left key 12-3, a lower key 12-4, a right key 12-1, an upper key 12-2, a confirmation key 12-6 and a return key 12-5, anti-skid threads 11 are arranged on the two outer sides of the handle, a microcontroller with the model STM32F103VET6 is arranged in the upper shell, a driving interface 1 of the microcontroller is connected with a liquid crystal driving board control interface 4, a detection interface 2 of the liquid crystal driving board is connected with a photoelectric detector, a liquid crystal screen interface 3 of the liquid crystal driving board is connected with the liquid crystal, the liquid crystal driving board has pin 1 connected to the serial port, pin 2 connected to JTAG interface, pin 3 connected to the motor, pin 4 connected to the photoelectric switch, pin 5 connected to the RF connector, power pin 6 connected to the power source, pin 7 connected to the Micro USB interface, and pin 8 connected to the front keyboard 12. .
When in use, the detection card is inserted into the detection card insertion hole 9 of the hand-held sulfur dioxide detector.
It is to be noted that all other apparatuses not particularly given a structure among the apparatuses are prior arts (commercially available products).
The invention relates to a method for detecting sulfur dioxide residue in food and Chinese medicinal materials by utilizing the reaction of hydrogen sulfide generated by sulfite reduction and lead acetate to generate a lead sulfide black tracer, which has the advantages of simple operation, high sensitivity, good selectivity and the like. The method is characterized in that a special reaction bottle cap made of silica gel is designed, a lead acetate reaction film is prepared into a detection card, and improved measures such as experiment conditions are optimized, so that a sulfur dioxide quantitative rapid detection method which is simple and convenient to operate and stable in result is established, and the reaction principle is as follows:
SO2+2NaOH＝Na2SO3+H2O
8HCl+3Zn+Na2SO3＝3ZnCl2+2NaCl+H2S↑+3H2O
H2S+Pb(Ac)2＝PbS↓+2HAc
however, special attention is paid to the detection process:
1. positive samples should be confirmed using standard methods.
2. The agent is corrosive and should be rinsed immediately with a large amount of water to avoid contact with the skin, if the eye is accidentally touched.
3. The extraction bottle, the reaction bottle and the plastic suction pipe can be reused after being cleaned, and distilled water is required to be self-provided.
4. The optimum temperature of the experiment is 15-35 ℃, and the optimum humidity is 35-70%. When the operation is not in the range, the experimental result is influenced, so that the detection result is inaccurate.
The method can be effectively used for primarily screening foods and traditional Chinese medicinal materials suspected to contain sulfur dioxide, can quickly detect the sulfur dioxide illegally remained in the foods such as vermicelli, biscuits, preserved fruits, dried fruits, chocolate products, dried vegetables and the like, and the traditional Chinese medicinal materials, Chinese patent medicines and traditional Chinese medicinal decoction pieces, ensures the safety of the foods and the traditional Chinese medicines, and has very good effect through experiments, the method takes the traditional Chinese medicine liquorice as an example, and carries out real test, when in operation, a disposable PE glove is worn, a proper amount of liquorice sampled in the market is taken, the medicinal materials are clamped by tweezers and crushed in a crusher, 1g of powder is weighed in an extraction bottle (or the prepared rehmannia root or the medlar is taken and crushed into the size of millet granules by scissors), 1g of powder is weighed in the balance and placed in the extraction bottle, 5mL of extracting solution (0.125 percent by mass and volume) is added, a NaOH cover is tightly covered, the liquid sample is soaked by shaking, water bath at 80 deg.C for 20min (water bath is conventional in laboratory), shaking, mixing, and filtering with filter paper to obtain supernatant as the solution to be detected.
1mL of the solution to be detected was aspirated by a pipette into a reaction flask, and a certain amount of zinc powder (0.015g) was added to the reaction flask.
A micropipette (commercially available routine) is used for sucking 7 mu L of wetting solution (Triton X-100, 1%; Tween-20, 1%; glycerol, 1%; and the balance water), reaction holes on the detection card are wetted, 1mL of 20% HCl is sucked into the reaction bottle by using a pipette, and the reaction bottle is immediately covered with a bottle stopper inserted with the wetted test strip and then tightly plugged.
Gently shaking, placing into sulfur dioxide reactor (patent equipment ZL201822155929.8) (rotation speed 200rpm, temperature 30 deg.C, humidity 45%) for reaction for 30min, and taking out the detection card and standing for 10 min. Opening the hand-held sulfur dioxide detector, taking out the IC card carried by the kit according to the operation instruction of the instrument, swiping the card to write a program, inserting the detection card into the card slot of the sulfur dioxide detector, selecting the detection program, and clicking the instrument to display the numerical value after measurement. (the test card after the reaction should be measured within 6-15 min) the results are: 94.9 mg/kg.
The detection result is basically consistent with that of 95.2mg/kg by detecting the traditional Chinese medicine decoction pieces according to a third method (ion chromatography) of 'Chinese pharmacopoeia' 2015 edition. The accuracy rate is 99.68%.
Taking vermicelli as an example, performing a real-land test, wearing disposable PE gloves during operation, taking a proper amount of vermicelli sampled from the market, clamping the vermicelli by using forceps, crushing the vermicelli in a crusher, weighing 1g of powder in an extraction bottle by using a balance, adding 5mL of extracting solution (0.125% NaOH solution), covering the extraction bottle tightly, shaking to soak a sample in liquid, carrying out water bath at 80 ℃ for 20min (a water bath pot is a conventional laboratory), shaking uniformly, and filtering to obtain a supernatant, namely the liquid to be tested.
Firstly, inserting one end with a positioning round hole into a chemical gas detection bottle cap (a product in the prior patent, patent No. ZL201620703797.6), enabling one end with a yellow adhesive tape to face upwards, sucking 7 mu L of wetting liquid by using a micropipettor (a product sold in the market), wherein the wetting liquid is prepared from Triton X-1001%, Tween-201%, glycerol 1% and the balance of water, and wetting a reaction membrane on a detection card. Secondly, accurately sucking 1mL of a sample to be detected by a liquid transfer device, placing the sample in a reaction bottle, adding a certain amount of 0.015g of zinc powder, and finally sucking 1mL of HCl with the volume concentration of 20% into the reaction bottle by the liquid transfer device. Thirdly, covering the reaction bottle with a reaction bottle cap, tightly plugging the reaction bottle cap, and slightly shaking the reaction bottle to uniformly mix the liquid in the reaction bottle. Fourthly, placing the sample in a reactor (a product of the prior patent, patent No. ZL201822155929.8) with controllable temperature and humidity, reacting for 30min at the rotation speed of 200rpm, the temperature of 30 ℃ and the humidity of 35 percent, taking out the detection card, and balancing the temperature of the obtained detection card for 10min at room temperature to ensure that the detection card is fully dried. Opening the hand-held sulfur dioxide detector, taking out the IC card carried by the kit according to the instrument operation instruction, swiping the card for writing the program, inserting the balanced detection card into the card slot of the sulfur dioxide detector, selecting the corresponding program, and obtaining the data after measurement, namely the content of sulfur dioxide in the sample to be measured; the instrument displays the value after clicking on the measurement. (the detection card after the reaction should be measured within 6-15 min). The results were: 87.2 mg/kg.
The sulfur content of the vermicelli is basically consistent with the result of 86.9mg/kg by detecting the sulfur content of the vermicelli according to a third method (ion chromatography) of 'Chinese pharmacopoeia' 2015 edition. The accuracy rate is 99.65%.
The method of the invention can obtain the same or similar results after repeatedly detecting and comparing different traditional Chinese medicine decoction pieces and foods for many times, and shows that the method is stable and reliable, has high sensitivity, average error of about 0.3 percent, high testing speed, one-time detection of about 40 minutes, at least 3 times shorter than the existing detection method, greatly improves the working efficiency, provides reliable technical guarantee for effectively preventing the food and the medicinal materials from adding sulfur dioxide, and has huge economic and social benefits.
Claims (5)
1. A sulfur dioxide rapid quantitative detection method is characterized in that a set of sulfur dioxide quantitative detection system is used, the system mainly comprises (1) a constant temperature and humidity reactor, (2) a sulfur dioxide rapid detection reaction bottle cap, (3) a sulfur dioxide quantitative detection card, (4) a sulfur dioxide quantitative detection reaction reagent, (5) a sulfur dioxide quantitative detection analysis IC card, and (6) equipment instruments and devices of a sulfur dioxide quantitative analyzer, and the detection operation comprises the following steps:
(1) preparing a sample:
the sample is a Chinese medicinal material to be detected, a Chinese patent medicine, a Chinese medicinal decoction piece or various food samples, the sample to be detected is cut or crushed into powder, the solid powder and the extraction liquid are placed in an extraction bottle according to the weight-volume ratio of 1:2 to 1:50, the liquid is shaken to soak the sample, the sample is soaked in water bath at 80 ℃, the water bath lasts for 20-30min, and the supernatant is taken out after standing, filtering or centrifuging, so that the sample liquid to be detected is obtained;
(2) and (3) detection:
taking out the sulfur dioxide quantitative detection card in the reagent box, inserting the sulfur dioxide quantitative detection card into a sulfur dioxide rapid detection reaction bottle cap, and adding 1mL of a sample to be detected and a certain amount of zinc powder into a reaction bottle; wetting the reaction wells on the test card with a wetting fluid; finally, a certain amount of HCl solution is transferred into a reaction bottle by a suction pipe, a reaction bottle cap inserted with a sulfur dioxide quantitative detection card is quickly covered, the reaction bottle cap is placed in a constant-temperature constant-humidity reactor with the temperature and the humidity controlled at 30 ℃ and 45% respectively and the rotating speed of 200r/min, the sulfur dioxide quantitative detection card is drawn out after oscillation reaction for 20min, and the reaction bottle is kept stand for 6-10 min; opening the hand-held sulfur dioxide quantitative analyzer, taking out the sulfur dioxide quantitative detection analysis IC card carried by the kit according to the operation instruction of the instrument, swiping the card to write a program, then inserting the sulfur dioxide quantitative detection analysis IC card into a card slot of the sulfur dioxide quantitative analyzer, selecting a corresponding program, and obtaining data after measurement, namely the content of sulfur dioxide in the sample to be measured;
when the detected sample makes the color of the detection card dark black, even silver gray crystals appear, the sulfur dioxide content in the sample is beyond the linear range of the measured value of the instrument, the error is increased due to direct measurement, and the sample to be detected needs to be diluted by water and then is detected again according to the step (2);
(3) drawing a standard curve:
when a batch of new detection cards are prepared, the new cards are used for redrawing the standard curve, and the step of drawing the standard curve comprises the following steps:
firstly, preparing a sodium sulfite standard solution: adding double distilled water into sodium sulfite to prepare gradient sodium sulfite standard solutions corresponding to different sulfur dioxide concentrations;
detecting sodium sulfite standard products with different concentration gradients by using the detection method, inserting test strips with different spot gray levels obtained by detection into a handheld sulfur dioxide quantitative analyzer, opening the analyzer, selecting a gray level detection program (GHX 201108080001), measuring gray levels of developed spots with different concentrations, detecting each concentration for 3 times, and averaging the gray levels; in an Excel worksheet, performing linear regression by taking a gray value as a vertical coordinate and a sulfur dioxide concentration value as a horizontal coordinate to obtain a concentration gray standard curve; inputting the parameters of the standard curve into an IC card through an IC card reader, namely a sulfur dioxide quantitative detection analysis card which is synchronous with the kit; when the detection is started, the sulfur dioxide quantitative detection analysis card carried in the reagent box is taken out, the card is placed at the back of the sulfur dioxide quantitative analyzer for reading the card, a detection program is selected, and the detector automatically compares the measured values of the color spots with different depths obtained by the detection reaction with a standard curve, so that the sulfur dioxide content in the food or the medicinal material can be quickly and quantitatively measured.
2. The method for rapidly and quantitatively detecting the sulfur dioxide as claimed in claim 1, which is characterized by comprising the following steps of:
(1) preparing a sample:
preparing a food sample: sampling food to be detected, cutting into pieces, crushing in a crusher, putting 5g of the powder into an extraction bottle, adding 5mL of NaOH solution with the volume concentration of 0.125%, tightly covering a cover, shaking to soak the sample with liquid, carrying out water bath at 80 ℃ for 20min, standing, filtering or centrifuging, and taking supernatant, namely the food liquid sample to be detected;
preparing a traditional Chinese medicine sample: the traditional Chinese medicine is a traditional Chinese medicine or a traditional Chinese medicine decoction piece, the traditional Chinese medicine is cut into pieces and then crushed in a crusher, the prepared rehmannia root or the medlar is cut into small millet particles by the scissors, 1g of the prepared rehmannia root or the medlar is weighed and placed in an extraction bottle, 5mL of NaOH solution with the volume concentration of 0.125 percent is added, a cover is tightly covered, the liquid is shaken to soak a sample, the mixture is subjected to water bath at the temperature of 80 ℃ for 20min and is kept stand for 40-60min, and the supernatant is taken to obtain a sample of the traditional Chinese medicine liquid to be detected;
(2) and (3) detection:
taking out the sulfur dioxide quantitative detection card, inserting one end with a positioning round hole into a sulfur dioxide rapid detection reaction bottle cap, enabling one end with a yellow adhesive tape to face upwards, sucking 1mL of a sample to be detected by using a suction pipe, placing the sample in a reaction bottle, adding 2 zinc particles, sucking 7 muL of wetting liquid by using a micropipettor, wherein the wetting liquid is prepared from Triton X-1001%, Tween-201%, 1% of glycerol and the balance of water, wetting a reaction hole on the sulfur dioxide quantitative detection card, sucking 1mL of HCl with the volume concentration of 20% into the reaction bottle by using the suction pipe, covering the reaction bottle cap on the reaction bottle, plugging, slightly shaking the reaction bottle to uniformly mix the liquid in the bottle, placing the reaction bottle in a constant-temperature and constant-humidity reactor with controllable temperature and humidity, reacting for 10-30min under the conditions of the rotating speed of 200r/min, the temperature of 20-30 ℃ and the humidity of 35-70, drawing out the sulfur dioxide quantitative detection card, balancing the room temperature for 6-10min, opening the handheld sulfur dioxide quantitative analyzer, taking out the sulfur dioxide quantitative detection analysis IC card carried by the kit according to the operation instruction of the analyzer, swiping the card to write a program, then inserting the detection card into a card slot of the sulfur dioxide quantitative analyzer, selecting a corresponding program, and obtaining data after measurement, namely the content of sulfur dioxide in the sample to be measured;
(3) and (3) data judgment:
when the detected sample is food, if the color of the detection card is dark black, even silver gray crystals appear, the sulfur dioxide content of the sample is beyond the linear range of the measured value of the instrument, the numerical value detection is inaccurate, and the sample to be detected needs to be diluted by 5 times and then re-detected according to the step (2);
when the detected sample is a traditional Chinese medicine, if the color of the detection card is dark black, even silver gray crystals appear, the sulfur dioxide content of the sample is beyond the linear range of the measured value of the instrument, the numerical value detection is inaccurate, and the sample to be detected needs to be diluted by 5 times and then re-detected according to the step (2);
(4) drawing a standard curve:
when a batch of new detection cards are prepared, the new cards are used for redrawing the standard curve, and the step of drawing the standard curve comprises the following steps:
firstly, preparing a sodium sulfite standard solution: adding double distilled water into sodium sulfite to prepare gradient sodium sulfite standard solutions corresponding to different sulfur dioxide concentrations;
detecting sodium sulfite standard products with different concentration gradients by using the detection method, inserting test strips with different spot gray levels obtained by detection into a handheld sulfur dioxide quantitative analyzer, opening the analyzer, selecting a gray level detection program (GHX 201108080001), measuring gray levels of developed spots with different concentrations, detecting each concentration for 3 times, and averaging the gray levels; in an Excel worksheet, performing linear regression by taking a gray value as a vertical coordinate and a sulfur dioxide concentration value as a horizontal coordinate to obtain a concentration gray standard curve; inputting the parameters of the standard curve into an IC card through an IC card reader, namely a sulfur dioxide quantitative detection analysis card which is synchronous with the kit; when the detection is started, taking out the sulfur dioxide quantitative detection analysis card carried in the reagent box, and placing the card at the back of the sulfur dioxide quantitative analyzer for reading the card; selecting a detection program, and automatically comparing the measured values of the color spots with different depths obtained by the detection reaction with a standard curve by using a detector, so that the content of sulfur dioxide in the food or the medicinal material can be quickly and quantitatively measured.
3. The method for rapidly and quantitatively detecting the sulfur dioxide as claimed in claim 1, wherein the reaction temperature of the sulfur dioxide reactor is 25 ℃ and the volume humidity is 45%.
4. The rapid quantitative detection method for sulfur dioxide according to claim 1, characterized in that the detection card structure comprises a bottom plate, a surface protection film, a reaction layer and a double-sided adhesive layer, wherein the double-sided adhesive layer (4) is arranged on the middle part of the bottom plate (1), the integrated reaction layer (3) is adhered on the double-sided adhesive layer (4), two ends of the reaction layer (3) are fixed on the bottom plate (1) through symmetrical fixing pressing strips (2), a reaction hole (6) is arranged in the middle part of the bottom plate, one end of the bottom plate is provided with a positioning hole (5), the middle part of the double-sided adhesive layer (4) is provided with a through hole corresponding to the reaction through hole (6) on the bottom plate and communicated with the reaction layer (3), and the bottom plate, the fixing pressing strips and the reaction.
5. The rapid quantitative detection method for sulfur dioxide according to claim 1, characterized in that the quantitative analyzer for sulfur dioxide is a hand-held quantitative analyzer for sulfur dioxide, and the structure thereof is that the analyzer comprises an upper shell (7) and a handle (8) connected with the upper shell into a whole, the front part of the upper shell is provided with a liquid crystal display screen (10), the side surface is provided with a detection card insertion hole (9), the front part of the handle is provided with a keyboard (12) for controlling the working state, the keyboard is composed of a left key (12-3), a lower key (12-4), a right key (12-1), an upper key (12-2), a confirmation key (12-6) and a return key (12-5), the outer two sides of the handle are provided with anti-skid grains (11), the upper shell is internally provided with a microcontroller with the model of STM32F103VET6, a driving interface 1 of the microcontroller is connected with a control interface 4 of a liquid crystal driving board, and a, liquid crystal screen interface 3 of liquid crystal drive board connects liquid crystal display (10) on the casing front portion, liquid crystal display (10) are the LCD liquid crystal screen, 1 foot of liquid crystal drive board connects the serial ports, 2 joint JTAG interfaces of foot of microcontroller, 3 feet of microcontroller connect the motor, 4 feet of microcontroller connect photoelectric switch, 5 feet of microcontroller connect radio frequency connector, 6 power connection of microcontroller's power pin, microcontroller is equipped with the Micro USB interface through 7 feet, microcontroller connects anterior keyboard (12) of handle through 8 feet.
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