CN103630534A - Quick detection method for sulfur dioxide in food - Google Patents
Quick detection method for sulfur dioxide in food Download PDFInfo
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- CN103630534A CN103630534A CN201310615136.9A CN201310615136A CN103630534A CN 103630534 A CN103630534 A CN 103630534A CN 201310615136 A CN201310615136 A CN 201310615136A CN 103630534 A CN103630534 A CN 103630534A
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Abstract
The invention relates to a quick detection method for sulfur dioxide in food. The quick detection method comprises the steps of firstly, preprocessing a sample to be tested, carrying out ultrasonic extraction by adopting an aqueous alkali; then adding water and an acid solution into a distilling flask, connecting the distilling flask with a condensing device, placing an outlet of a condensing pipe into a starch solution added with a small quantity of titrating solution, and finally heating the distilling flask, wherein because sulfur dioxide contained in the sample to be tested can be released from the distilling flask in a heating process and the starch solution added with a small quantity of titrating solution flows through the condensing pipe, the light blue starch solution fades; continuing to dropwise adding a titrating solution until the light blue of the starch solution does not fade, thus judging a titration end point, so as to calculate the content of the sulfur dioxide in the sample to be tested through calculating the consumption quantity of the titrating solution when the titration end point is reached. The quick detection method is simple, is capable of performing qualitative and quantitative detection on the content of the sulfur dioxide in the sample to be tested, accurate in detection result and free of harmful effects to the environment and the detection personnel; the end point is easily judged.
Description
Technical field
The invention belongs to food safety detection field, be specifically related to a kind of detection method of sulfur dioxide in food.
Background technology
In food, conventional sulphite comprises sodium sulphite, sodium bisulfite, Hydros and sodium pyrosulfite etc., at present, all generally uses sulphite to use in China's food-processing industry
In bleaching, anticorrosion, decolouring and anti-oxidant.Sulphurous acid and and salt can with food in the effects such as sugar, protein, pigment, enzyme, the rope of supporting one's family, aldehyde, ketone, produce sequestered and mating type
Sulphuric dioxide.In recent years, due to the Use out of range of sulphite in foods and the situation of abuse day by day serious, directly cause sulfur dioxide content in food obviously to increase.In addition, also there is the illegal product of part man, in food, directly add a large amount of sulphuric dioxide.
The sulphuric dioxide of the long-term excess intake of people, can cause gastrointestinal reaction, affect Calcium and phosphorous absorption, obviously reduce immunity of organisms, on multiple internal organs such as body brain, liver, stomach, kidneys, all can produce obvious impact, in addition, because sulphuric dioxide is very easily water-soluble, major part can be blocked in people's upper respiratory tract, generates sulphurous acid, sulfuric acid and sulfate on moistening mucous membrane, directly stimulate or infringement respiratory tract, severe patient can be lethal.Therefore the health that the excessive sulphuric dioxide, adding in food directly jeopardizes people is life security even.In China < < food additives use hygienic standard > >, to sulphuric dioxide, the usable range in food and use amount etc. have all been made clear and definite regulation.
At present, the method that sulfur dioxide in food is detected has multiple, traditional detection method mainly comprises hydrochloric para-rosaniline method and the rear iodimetric titration of distillation, these two kinds of detection methods can be carried out accurate quantitative analysis to the content of sulfur dioxide in food, but detection method complex operation, detection time is long, and need professional and technical personnel to complete in corresponding laboratory, in hydrochloric para-rosaniline method testing process wherein, need to use poisonous reagent tetrachloro mercury sodium, testing staff and environment are all brought to significantly serious pollution.Therefore, for the situation of China's food sulphuric dioxide severe overweight, in the urgent need to finding a kind of science, detection method accurately and rapidly.
Summary of the invention
Object of the present invention is exactly for the defect existing in above-mentioned prior art, to provide a kind of can carry out to the content of sulfur dioxide in food the method for fast detecting.
Technical scheme of the present invention is as follows:
A method for quick for sulfur dioxide in food, comprises the following steps:
(1) testing sample is carried out to pre-service, the testing sample of handling well is joined in the triangular flask of tool plug, drip aqueous slkali, ultrasound wave extracts, and filters, and gets filtrate and is added in cucurbit;
(2) in cucurbit, add water and acid solution, install condensing unit, condenser pipe endpiece is inserted in starch solution;
(3) in starch solution, drip a small amount of vs, stir, starch solution is become light blue, cucurbit is heated, as starch solution azury in heating process, the explanation of fading contains sulphuric dioxide in testing sample, proceeds step (4);
(4) when light blue starch solution fades, continue to drip vs, the color that maintains light blue starch solution is constant, until light blue starch solution no longer fades, draws the content of sulphuric dioxide in testing sample by calculating the addition of vs.
Described in step (2), to testing sample the concrete grammar processed, be:
When testing sample is solid, take 1-3g testing sample, adopt polishing or comminutor to pulverize; Or when testing sample is liquid, adopt graduated cylinder amount directly to measure 5-10ml testing sample.
Preferably, described aqueous slkali is selected from a kind of in sodium hydroxide solution or potassium hydroxide solution.
Preferably, the concentration of described aqueous slkali is 0.1-0.3 mol/L.
Preferably, the addition of described aqueous slkali is 10-15ml.
Add aqueous slkali can with food samples in sulphuric dioxide react, generate sulfate or sulphite;
Preferably, the time that described ultrasound wave extracts is 15-30min.
Preferably, described acid solution is selected from a kind of in phosphoric acid solution or hydrochloric acid solution.
Preferably, the concentration of described acid solution is 5-15mol/L.
Preferably, the addition of described acid solution is 5-10ml.
Add acid solution heating can make the sulfate or the sulphite that generate discharge sulfur dioxide gas.
Preferably, in described cucurbit, adding the amount of water is 300-400ml.
Preferably, the aqueous solution that described starch solution is starch, concentration is 1-3g/L, the addition of starch solution is 100-150ml.
Preferably, vs is iodine standard solution or bromine standard solution.
The concentration of described vs is 0.005-0.03mol/L, preferably 0.01 mol/L.
Preferably, the temperature of described heating is 50-80 ℃.
Compared to the prior art, beneficial effect of the present invention is as follows:
This group invention mainly according to sulphuric dioxide easily oxidized principle design, first adopt aqueous slkali to extract sulphuric dioxide, adopt again acid solution acidifying, cucurbit is heated simultaneously, be beneficial to sulphuric dioxide discharges from cucurbit, again the sulphuric dioxide discharging is joined and in the starch solution that contains vs, carry out redox reaction, observe the variation of starch solution color, judgement titration end-point, according to the volumescope of the vs consuming, calculate the amount of sulphuric dioxide, whole experimental technique is simple, detection method science, and result is accurate.
2. while adopting traditional hydrochloric para-rosaniline method to detect the sulphuric dioxide in food, use tetrachloro mercury sodium to make the absorption liquid of sulphuric dioxide, use zinc acetate and potassium ferrocyanide as clarificant, to testing staff, can damage, to environment, can pollute, the reagent safety of using in this group invention is nontoxic, on testing staff's health and environment all without affecting.
3. the invention of this group first adopts aqueous slkali to extract to testing sample, avoided the impact of other components on testing result in testing sample, also avoid other coloured component judgements to titration end-point in testing process in testing sample, improved the accuracy of testing result.
4. GB/T5009.34 sulphite in foods the second method is in the way of distillation, need receive to 200ml with lead acetate solution, with concentrated hydrochloric acid, discharge again, complex steps, and for some special samples, while adopting lead acetate solution to absorb, can make absorption liquid color change, make titration end-point difficult judgment, affect testing result.In the invention of this group, first with aqueous slkali, sulphuric dioxide is extracted, while adopting acid solution acidifying, adopt hydrochloric acid and phosphoric acid, avoided above-mentioned defect.
Embodiment
The present invention, by the present invention of following specific embodiment more detailed description, can make those skilled in the art more fully understand the present invention, but not limit the present invention in any way.
Embodiment 1
(1) take 1g testing sample (mushroom), adopt polishing to pulverize, the testing sample crushing (mushroom) is joined in the triangular flask of tool plug, dripping 10ml concentration is the sodium hydroxide solution of 0.1 mol/L, ultrasound wave extracts 15min, filters, and gets filtrate and is added in cucurbit;
(2) in cucurbit, add the phosphoric acid solution of 300ml water and 5ml concentration 5mol/L, install condensing unit, it is in 1g/L and starch solution that condenser pipe endpiece is inserted 100ml concentration;
(3) in starch solution, drip a small amount of 0.03mol/L iodine standard solution liquid, stir, starch solution is become light blue, cucurbit is heated, be heated to 50 ℃, as starch solution azury in heating process fades in explanation testing sample (mushroom), contain sulphuric dioxide, proceed step (4);
(4) when fading, continues light blue starch solution to drip iodine standard solution, the color that maintains light blue starch solution is constant, until light blue starch solution no longer fades, by calculating the addition of iodine standard solution, draw the content of sulphuric dioxide in testing sample (mushroom).
By titration calculating, show that in tremella, content of sulfur dioxide is 0.01%.
Embodiment 2
(1) take 3g testing sample (tremella), adopt polishing to pulverize, the testing sample crushing (tremella) is joined in the triangular flask of tool plug, drip the sodium hydroxide solution that 15ml concentration is 0.3mol/L, ultrasound wave extracts 30min, filters, and gets filtrate and is added in cucurbit;
(2) in cucurbit, add the phosphoric acid solution of 400ml water and 10ml concentration 8mol/L, install condensing unit, it is in 3g/L and starch solution that condenser pipe endpiece is inserted 150ml concentration;
(3) in starch solution, drip the iodine standard solution that a small amount of concentration is 0.005 mol/L, stir, starch solution is become light blue, cucurbit is heated, be heated to 80 ℃, as starch solution azury in heating process fades in explanation testing sample (tremella), contain sulphuric dioxide, proceed step (4);
(4) when fading, continues light blue starch solution to drip iodine standard solution, the color that maintains light blue starch solution is constant, until light blue starch solution no longer fades, by calculating the addition of iodine standard solution, draw the content of sulphuric dioxide in testing sample (tremella).
By titration calculating, show that in tremella, content of sulfur dioxide is 0.02%.
Embodiment 3
(1) take 2g testing sample (tremella), adopt polishing to pulverize, the testing sample crushing (tremella) is joined in the triangular flask of tool plug, drip the sodium hydroxide solution that 12ml concentration is 0.2mol/L, ultrasound wave extracts 20min, filters, and gets filtrate and is added in cucurbit;
(2) in cucurbit, add the phosphoric acid solution of 300ml water and 10ml concentration 10mol/L, install condensing unit, it is in 2g/L and starch solution that condenser pipe endpiece is inserted 120ml concentration;
(3) in starch solution, dripping a small amount of concentration is 0.01mol/L iodine standard solution, stir, starch solution is become light blue, cucurbit is heated, be heated to 65 ℃, as starch solution azury in heating process fades in explanation testing sample (tremella), contain sulphuric dioxide, proceed step (4);
(4) when fading, continues light blue starch solution to drip iodine standard solution, the color that maintains light blue starch solution is constant, until light blue starch solution no longer fades, by calculating the addition of iodine standard solution, draw the content of sulphuric dioxide in testing sample (tremella).
By titration calculating, show that in tremella, content of sulfur dioxide is 0.05%.
Embodiment 4
(1) take 3g testing sample (tremella), adopt polishing to pulverize, the testing sample crushing (tremella) is joined in the triangular flask of tool plug, drip the potassium hydroxide solution that 15ml concentration is 0.3mol/L, ultrasound wave extracts 30min, filters, and gets filtrate and is added in cucurbit;
(2) in cucurbit, add the hydrochloric acid solution of 400ml water and 10ml concentration 15mol/L, install condensing unit, it is in 3g/L and starch solution that condenser pipe endpiece is inserted 150ml concentration;
(3) in starch solution, drip the bromine standard solution that a small amount of concentration is 0.01mol/L, stir, starch solution is become light blue, cucurbit is heated, be heated to 80 ℃, as starch solution azury in heating process fades in explanation testing sample (tremella), contain sulphuric dioxide, proceed step (4);
(4) when fading, continues light blue starch solution to drip bromine standard solution, the color that maintains light blue starch solution is constant, until light blue starch solution no longer fades, by calculating the addition of bromine standard solution, draw the content of sulphuric dioxide in testing sample (tremella).
By titration calculating, show that in tremella, content of sulfur dioxide is 0.02%.
The above embodiment is preferred embodiments of the present invention, is not to limit the scope of the present invention, and the equivalence of doing according to structure, feature and principle described in the present patent application the scope of the claims therefore all changes or modifies, and all should comprise in patent claim of the present invention.
Claims (10)
1. a method for quick for sulfur dioxide in food, is characterized in that, comprises the following steps:
(1) testing sample is carried out to pre-service, the testing sample of handling well is joined in the triangular flask of tool plug, drip aqueous slkali, ultrasound wave extracts, and filters, and gets filtrate and is added in cucurbit;
(2) in cucurbit, add water and acid solution, install condensing unit, condenser pipe endpiece is inserted in starch solution;
(3) in starch solution, drip a small amount of vs, stir, starch solution is become light blue, cucurbit is heated, as starch solution azury in heating process, the explanation of fading contains sulphuric dioxide in testing sample, proceeds step (4);
(4) when light blue starch solution fades, continue to drip vs, the color that maintains light blue starch solution is constant, until light blue starch solution no longer fades, draws the content of sulphuric dioxide in testing sample by calculating the addition of vs.
2. the method for quick of a kind of sulfur dioxide in food according to claim 1, it is characterized in that, in described step (1) to testing sample and carry out pretreated concrete grammar and be: when testing sample is solid, take 1-3g testing sample, adopt polishing or comminutor to pulverize; Or when testing sample is liquid, adopt graduated cylinder amount directly to measure 5-10ml testing sample.
3. the method for quick of a kind of sulfur dioxide in food according to claim 1, is characterized in that, described aqueous slkali is selected from a kind of in sodium hydroxide solution or potassium hydroxide solution.
4. the method for quick of a kind of sulfur dioxide in food according to claim 1, is characterized in that, the concentration of described aqueous slkali is 0.1-0.3 mol/L; The addition of described aqueous slkali is 10-15ml.
5. the method for quick of a kind of sulfur dioxide in food according to claim 1, is characterized in that, the time that described ultrasound wave extracts is 15-30min.
6. the method for quick of a kind of sulfur dioxide in food according to claim 1, is characterized in that, described acid solution is selected from a kind of in phosphoric acid solution or hydrochloric acid solution.
7. the method for quick of a kind of sulfur dioxide in food according to claim 1, is characterized in that, the concentration of described acid solution is 5-15mol/L; The addition of described acid solution is 5-10ml, and the addition of water is 300-400ml.
8. the method for quick of a kind of sulfur dioxide in food according to claim 1, is characterized in that, the aqueous solution that described starch solution is starch, and concentration is 1-3g/L, the addition of starch solution is 100-150ml.
9. the method for quick of a kind of sulfur dioxide in food according to claim 1, is characterized in that, vs is iodine standard solution or bromine standard solution; The concentration of described vs is 0.005-0.03mol/L, preferably 0.01mol/L.
10. the method for quick of a kind of sulfur dioxide in food according to claim 1, is characterized in that, the temperature of described heating is 50-80 ℃.
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| CN201310615136.9A CN103630534A (en) | 2013-11-28 | 2013-11-28 | Quick detection method for sulfur dioxide in food |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104155293A (en) * | 2014-08-15 | 2014-11-19 | 广州衡创测试技术服务有限公司 | Improved detection method for sulfur dioxide |
| CN104198485A (en) * | 2014-08-16 | 2014-12-10 | 中山鼎晟生物科技有限公司 | Rapid detection method of sulfur dioxide in Lycium barbarum fruits |
| CN104297243A (en) * | 2014-10-18 | 2015-01-21 | 中山鼎晟生物科技有限公司 | Method applied to rapid detection of sulfur dioxide in wine products |
| CN104865245A (en) * | 2015-04-29 | 2015-08-26 | 四川省中药饮片有限责任公司 | Method for determining sulfur dioxide in amygdalin contained traditional Chinese medicine and slices thereof |
| CN105929106A (en) * | 2016-04-14 | 2016-09-07 | 梧州市产品质量检验所 | Method for measuring residual sulfur dioxide content of tortoise jelly powder |
| CN109060747A (en) * | 2018-08-21 | 2018-12-21 | 广西科技大学 | The rapid detection method of sulfur dioxide in white granulated sugar |
| CN111257502A (en) * | 2020-03-05 | 2020-06-09 | 江苏权正检验检测有限公司 | Method for measuring sulfur dioxide in dried mushrooms |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104155293A (en) * | 2014-08-15 | 2014-11-19 | 广州衡创测试技术服务有限公司 | Improved detection method for sulfur dioxide |
| CN104198485A (en) * | 2014-08-16 | 2014-12-10 | 中山鼎晟生物科技有限公司 | Rapid detection method of sulfur dioxide in Lycium barbarum fruits |
| CN104297243A (en) * | 2014-10-18 | 2015-01-21 | 中山鼎晟生物科技有限公司 | Method applied to rapid detection of sulfur dioxide in wine products |
| CN104865245A (en) * | 2015-04-29 | 2015-08-26 | 四川省中药饮片有限责任公司 | Method for determining sulfur dioxide in amygdalin contained traditional Chinese medicine and slices thereof |
| CN104865245B (en) * | 2015-04-29 | 2018-09-18 | 四川省中药饮片有限责任公司 | A method of measuring sulfur dioxide in Chinese medicine and its medicine materical crude slice containing amarogentin |
| CN105929106A (en) * | 2016-04-14 | 2016-09-07 | 梧州市产品质量检验所 | Method for measuring residual sulfur dioxide content of tortoise jelly powder |
| CN109060747A (en) * | 2018-08-21 | 2018-12-21 | 广西科技大学 | The rapid detection method of sulfur dioxide in white granulated sugar |
| CN109060747B (en) * | 2018-08-21 | 2021-08-06 | 广西科技大学 | Method for rapidly detecting sulfur dioxide in white granulated sugar |
| CN111257502A (en) * | 2020-03-05 | 2020-06-09 | 江苏权正检验检测有限公司 | Method for measuring sulfur dioxide in dried mushrooms |
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Application publication date: 20140312 |