CN105784698A - Rapid saccharin sodium detection kit and detection method thereof - Google Patents
Rapid saccharin sodium detection kit and detection method thereof Download PDFInfo
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- CN105784698A CN105784698A CN201610133497.3A CN201610133497A CN105784698A CN 105784698 A CN105784698 A CN 105784698A CN 201610133497 A CN201610133497 A CN 201610133497A CN 105784698 A CN105784698 A CN 105784698A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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Abstract
The invention provides a rapid saccharin sodium detection kit which is characterized by comprising an extracting agent, an acid solution of methylene blue and accessories such as a reaction bottle, a suction tube and a sampling spoon, wherein the extracting agent is a mixed reagent of trichloromethane and ethanol; the volume percentage of the ethanol in the extracting agent is 1-2%; the concentration of the methylene blue solution in the acid solution of the methylene blue is 4*10<-3>-0.16mol/l; the acid medium in the acid solution of the methylene blue is one of acid solutions such as sulfuric acid and hydrochloric acid; the hydrogen ion concentration of the acid medium is 0.01-4mol/l. A detection method of the rapid saccharin sodium detection kit adopts the mixed reagent of trichloromethane and ethanol as the extracting agent, so that the detection sensitivity is greatly improved, detection values have large developing gradients, whether a detected sample is within a qualification or not can be very accurately judged, and moreover as the stability of the trichloromethane is improved and the volatility is degraded, the rapid saccharin sodium detection kit is relatively easy to preserve and transport.
Description
Technical field
The present invention relates to a kind of saccharin sodium quick detection kit and detection method thereof.
Background technology
Saccharin chemical name is o-benzoic sulfimide, and the commodity saccharin of market sale is really the sodium salt of the o-benzoic sulfimide of ease of solubility, is called for short saccharin sodium.Saccharin sodium is synthetic sweetener conventional in food industry, and uses history the longest, but is also the most controversial synthetic sweetener.Sweet 300-500 times of sweetness ratio sucrose, is not decomposed, kidney excretes.But its toxicity is not strong, play dispute main in its carcinogenicity.
The raw material manufacturing saccharin mainly has toluene, chlorosulfonic acid, ortho-aminotoluene etc., is petrochemicals.Toluene is volatile and burns, and even sets off an explosion, and can cause acute poisoning after a large amount of absorption human bodies, bigger to human health damage；Chlorosulfonic acid easily absorbs water to decompose and produces hydrogen chloride gas, harmful, and explosive；The intermediate materials produced in saccharin production process also has harm to health.Saccharin the most also can serious environment pollution.Additionally, privately flow into the saccharin of vast Small Urban, rural market from part medium and small saccharin factory, also as technique is coarse, the operation reason such as not exclusively and containing foreign material such as heavy metal, ammoniate, arsenic.They retain for a long time in human body, accumulate, and affect the health of human body to some extent.
On the other hand, since two thousand five, saccharin application in food has obvious over range, excess phenomenon.Some manufacturers are in order to reduce cost earning sudden huge profits, at beverage, preserved fruit is even specialized in the food such as the jelly of children market, commonly use harmful unhelpful saccharin to replace sucrose, but on food labelling, do not make any expressing, or titled with " protein sugar ", the fact that good names such as " sweet treasured " covers use saccharin, compromise the healthy of consumer, constituted a serious infringement the right to know of consumer, particularly there is the consumer of minority in the case of not knowing saccharin harm completely, edible a large amount of saccharin in short time, decrease of platelet is caused to cause acute massive hemorrhage, multiple organ damage etc., cause pernicious poisoning, Qi Liao various circles of society and the close attention of consumers in general.
The method measuring saccharin sodium at present has fluorescence spectrophotometry, ultraviolet spectrophotometry, TLC, phenol sulphur titanium colorimetric method, high performance liquid chromatography, water titration (method), liquid membrane electrode method etc., and in the food that national standard (GB/T5009.28-2003) specifies, the assay method of saccharin sodium is high performance liquid chromatography, thin-layered chromatography, ion selecting electrode determining method.High performance liquid chromatography has that separative efficiency is high, sensitivity advantages of higher, uses standard control method, point-device can detect the content of saccharin sodium in sample, but its apparatus expensive, volume is big, it is difficult to realize field quick detection.In addition to methylene blue Extraction-Spectrophotometric Determination method, additive method or because of numerous and diverse sample extraction and separation, or because easily being affected by factors such as food compositions, the requirement of field quick detection all can not be reached.
The saccharin sodium quick detection kit product of other companies on existing market, Cleaning Principle used is methylene blue Extraction-Spectrophotometric Determination method, but extractant used is pure chloroform, the method poor sensitivity, detection gradient is inconspicuous, just can observe color distortion during the value that differs greatly, market user is difficult to accurate interpretation and whether goes out detection value at acceptability limit, and to market, user brings puzzlement.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of saccharin sodium quick detection kit, detected value colour developing gradient is big, it is possible to judge that detection sample, whether at acceptability limit, increases substantially detection sensitivity the most accurately.
The technical solution used in the present invention is as follows: a kind of saccharin sodium quick detection kit, this kit includes the acid solution of extractant, methylene blue；And the accessory such as reaction bulb, suction pipe, sample spoon, described extractant is chloroform (CCL3) and ethanol mix reagent according to a certain ratio；
Volume ratio shared by ethanol in described extractant is 1%～2%；
In the acid solution of described methylene blue, methylene blue solution concentration is 4*10-3Mol/l～0.16mol/l；
Acid medium employed in the acid solution of described methylene blue is the acid solution such as sulfuric acid, hydrochloric acid, and the solution hydrogen ion concentration of described acid medium is 0.01mol/l～4mol/l.
Described extractant is divided in transparent vessel, and the acid solution of described methylene blue is loaded in opaque drop bottle, drips and is reacted, then shake extraction after adding testing sample.
Further object is that the detection method that a kind of above-mentioned quick detection kit is provided:
A kind of saccharin sodium method for quick, the method is that the following several character utilizing this experimental principle and agents useful for same realize:
(1), methylene blue can with saccharin sodium react generation hydrophobic type ionic associate, this associated matter can be by chloroform quantified extract；
(2), chloroform (CCL3) volatile and sterling to photaesthesia, meet light note and gradually decompose and generate the phosgene of severe toxicity, reagent preservation aspect also tends to add the ethanol used as stabilizers of 0.3%～1%, on the other hand, after chloroform and ethanol mixing, its volatility substantially reduces, it is easier to storage and transport.
(3), chloroform is as extractant, ethanol content within the specific limits time color developing effect optimal: in the presence of in whole reaction system without ethanol, poor sensitivity, detection gradient is inconspicuous, just can observe color distortion during the value that differs greatly, market user is difficult to accurate interpretation and whether goes out detection value at acceptability limit；When in reaction system, ethanol content exceedes a certain particular value, during extraction, emulsion is serious, and organic phase colour developing loses gradient, it is impossible to according to its colour developing situation, saccharin sodium content is carried out sxemiquantitative judgement.After colour developing, if there is blueness in lower floor's organic phase, then can tentatively judge that this drink may contain saccharin sodium composition, if chromogenic reaction is unchanged, then illustrate in this drink certainly not add saccharin sodium composition, will may be added with saccharin sodium and the sample beyond national standard carries out the equal finer detection of high-efficient liquid the most again.
Utilizing above-mentioned principle and character, extractant chloroform is changed into chloroform and ethanol by the mix reagent of proportioning by the present invention, and the scope of detected alcoholic beverages is made that specification.The method comprises the following steps:
(1), taking out suction pipe and add chloroform and ethanol test solution 1-10ml in reaction bulb, be subsequently adding testing sample 1～10ml, concussion shakes up；
(2) in reaction bulb, add the acid solution of 0.1-2ml methylene blue, shake energetically and make two-phase mixtures, then stand to clear layering, observing lower floor's solution colour developing situation, after colour developing, there is blueness in lower floor's organic phase, then can tentatively judge that this drink may contain saccharin sodium composition, if chromogenic reaction is unchanged, then illustrate in this drink certainly not add saccharin sodium composition, will may be added with saccharin sodium and the sample beyond national standard carries out the equal finer detection of high-efficient liquid the most again.
Described testing sample in above-mentioned steps (1) is non-breast class beverage, ice lolly, cold drink, and alcoholic strength is not higher than the alcoholic beverage of 15%, such as Sprite, cola, ice lolly, pre-rectification, beer etc.；
Described ethanol total amount proportion in above-mentioned steps (1) reaches optimum efficiency when 2%；
The solution hydrogen ion concentration of the described acid medium in above-mentioned steps (2) is 0.01mol/l～4mol/l.
The method for quick of the present invention can be used for detecting non-breast class beverage, ice lolly, cold drink and alcoholic strength and is not higher than the alcoholic beverage of 15%, such as Sprite, cola, ice lolly, pre-rectification, beer etc..
Compared with prior art, there is advantages that
1, the method for quick of the present invention is that the mix reagent using chloroform and ethanol is as extractant, detection sensitivity is so greatly improved, detected value colour developing gradient is big, can judge the most accurately whether to detect sample at acceptability limit, and add the stability of chloroform, reduce its volatility, it is easier to storage and transport.
2, the scope of the method for quick specification of present invention detection drink, after in drink, ethanol content is more than 15%, during extraction, emulsion increases the weight of, organic phase colour developing gradient is the most obvious, according to its colour developing situation, saccharin sodium content sxemiquantitative judgement, the scope of specification detection drink cannot be carried out, on-site quick screening target guidance can be made, reduce and false-positive probability occurs, solve the puzzlement of market operation personnel.
3, the compositions such as the added benzoic acid of the method, citric acid, HFCS, white granulated sugar, essence are used all colour developing to be affected the most too much, thus ensure that chromogenic reaction result accuracy rate is higher than 97%, false negative rate is 0, rapidly suspicious specimen can be narrowed down to the least scope, finally have only to these few suspicious specimen are carried out the equal Precision measurement of high-efficient liquid, i.e. can detect that the saccharin sodium content sample beyond national regulation.
Detailed description of the invention
Below the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only a part of embodiment of the present invention, rather than whole embodiments, in the case of not conflicting, embodiment in the application and the feature in embodiment can be mutually combined, and describe the present invention in detail below in conjunction with embodiment.
Embodiment 1: Sprite, specification 500ml；
Saccharin sodium content in Sprite is used for quickly detecting by the present embodiment, and it specifically comprises the following steps that
Taking chloroform and ethanol test solution 1ml in reaction bulb, add 2ml and shaken the Sprite of venting carbon dioxide in the reaction bulb installing extractant, dropping 0.1ml methylene blue solution concentration is 4*10-3Mol/l, hydrogen ion concentration are the sulfuric acid mixed solution of the methylene blue solution of 0.01mol/l, tighten reaction bulb bottle cap, shake energetically about 1 minute, make two-phase mixtures, stand to clear layering and observe lower floor's solution colour developing situation.In blueness, then can determine that there is saccharin sodium composition in the present embodiment Sprite, color is the deepest, and saccharin sodium content is the highest, its color is compareed with standard color comparison card, and gained is saccharin sodium concentration.
Embodiment 2: Coca-Cola, specification 500ml；
Saccharin sodium content in Coca-Cola is used for quickly detecting by the present embodiment, and it specifically comprises the following steps that
Take chloroform and ethanol test solution 3ml in reaction bulb, add 3ml and shake Coca-Cola of venting carbon dioxide in the reaction bulb installing extractant, the sulfuric acid mixed solution of methylene blue solution that dropping 0.5ml methylene blue solution concentration is 0.05mol/l, hydrogen ion concentration is 0.05mol/l, tighten reaction bulb bottle cap, shake about 1 minute energetically, make two-phase mixtures, stand to clear layering and observe lower floor's solution colour developing situation.In blueness, then can determine that there is saccharin sodium composition in the present embodiment Coca-Cola, color is the deepest, and saccharin sodium content is the highest, its color is compareed with standard color comparison card, and gained is saccharin sodium concentration.
Embodiment 3: Finda, specification 500ml；
Saccharin sodium content in Finda is used for quickly detecting by the present embodiment, and it specifically comprises the following steps that
Take chloroform and ethanol test solution 10ml in reaction bulb, add 10ml and shake the Finda of venting carbon dioxide in the reaction bulb installing extractant, adding 2ml methylene blue solution concentration is 0.16mol/l, hydrogen ion concentration is the sulfuric acid mixed solution of the methylene blue solution of 4mol/l, tighten reaction bulb bottle cap, shake about 1 minute energetically, make two-phase mixtures, stand to clear layering and observe lower floor's solution colour developing situation, in blueness, then can determine that the present embodiment Finda has saccharin sodium composition, color is the deepest, saccharin sodium content is the highest, its color is compareed with standard color comparison card, gained is saccharin sodium concentration.
Enforcement 4: pre-rectification, specification 275ml；
Saccharin sodium content in pre-rectification is used for quickly detecting by the present embodiment, and it specifically comprises the following steps that
Take chloroform and ethanol test solution 10ml in reaction bulb, add 10ml and shake the pre-rectification of venting carbon dioxide in the reaction bulb installing extractant, dropping 2ml methylene blue solution concentration is 0.10mol/l, hydrogen ion concentration is the sulfuric acid mixed solution of the methylene blue solution of 1mol/l, tighten reaction bulb bottle cap, shake about 1 minute energetically, make two-phase mixtures, stand to clear layering and observe lower floor's solution colour developing situation, in blueness, then can determine that in the pre-rectification of the present embodiment have saccharin sodium composition, color is the deepest, saccharin sodium content is the highest, its color is compareed with standard color comparison card, gained is saccharin sodium concentration.
Implement 5 beer, specification 330ml；
Saccharin sodium content in beer is used for quickly detecting by the present embodiment, and it specifically comprises the following steps that
Take chloroform and ethanol test solution 5ml in reaction bulb, add 10ml and shake the beer of venting carbon dioxide in the reaction bulb installing extractant, the sulfuric acid mixed solution of methylene blue solution that dropping 1ml methylene blue solution concentration is 0.10mol/l, hydrogen ion concentration is 1mol/l, tighten reaction bulb bottle cap, shake about 1 minute energetically, make two-phase mixtures, stand to clear layering and observe lower floor's solution colour developing situation.In blueness, then can determine that there is saccharin sodium composition in the present embodiment beer, color is the deepest, and saccharin sodium content is the highest, its color is compareed with standard color comparison card, and gained is saccharin sodium concentration.
The detection situation contrast of embodiment saccharin sodium:
Using detection reagent described above and detection method, carry out contrasting testing result with high performance liquid chromatography, detect 30 batch samples altogether, first with saccharin sodium content in this law detection judgement sample, then compare by high performance liquid chromatography, result is as follows:
Note: "+" represent beyond national standard.
As can be seen from the above table, the identical rate of two kinds of methods is 100%, visible chromogenic reaction result accuracy rate of the present invention is higher, false positive rate is 0, suspicious specimen can be narrowed down to the least scope by the present invention rapidly, finally have only to these few suspicious specimen are carried out the equal Precision measurement of high-efficient liquid, i.e. can detect that the illegal sample containing saccharin sodium.
The method for quick of the present invention is that the mix reagent using chloroform and ethanol is as extractant, detection sensitivity is so greatly improved, detected value colour developing gradient is big, can judge the most accurately whether to detect sample at acceptability limit, and add the stability of chloroform, reduce its volatility, it is easier to storage and transport.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every equivalent structure utilizing description of the invention content to be made or equivalence flow process conversion; or directly or indirectly it is used in other relevant technical fields, the most in like manner it is included in the scope of patent protection of the present invention.
Claims (7)
1. a saccharin sodium quick detection kit, it is characterised in that: described kit includes extractant, secondary
The acid solution of methyl blue；And the accessory such as reaction bulb, suction pipe, sample spoon, described extractant is chloroform
Mix reagent with ethanol；
Volume ratio shared by ethanol in described extractant is 1%～2%；
In the acid solution of described methylene blue, methylene blue solution concentration is 4*10-3Mol/l～0.16mol/l；
Acid medium employed in the acid solution of described methylene blue is in the acid solution such as sulfuric acid, hydrochloric acid
Kind, the solution hydrogen ion concentration of described acid medium is 0.01mol/l～4mol/l.
Saccharin sodium quick detection kit the most according to claim 1, it is characterised in that: described extraction
Agent is divided in transparent vessel, and the acid solution of described methylene blue is loaded in opaque drop bottle.
3. the saccharin sodium method for quick as described in claim 1 or 2 any one, it is characterised in that:
Comprise the following steps:
(1), take out suction pipe and add extractant chloroform and ethanol test solution 1-10ml in reaction bulb, then
Adding testing sample 1～10ml, concussion shakes up 1 minute；
(2), in reaction bulb add 0.1-2ml methylene blue acid solution, shake energetically and make two-phase mixtures,
Then standing to clear layering, observe lower floor's solution colour developing situation, after colour developing, there is blueness in lower floor's organic phase,
Then can tentatively judge that this drink may contain saccharin sodium composition, if chromogenic reaction is unchanged, then this drink is described
Product do not add saccharin sodium composition certainly.
Saccharin sodium method for quick the most according to claim 3, it is characterised in that: described step (1)
In described testing sample be non-breast class beverage, ice lolly, cold drink, and alcoholic strength be not higher than 15% alcohol drink
Material, such as Sprite, cola, ice lolly, pre-rectification, beer etc..
Saccharin sodium method for quick the most according to claim 3, it is characterised in that: described step (1)
Volume ratio shared by ethanol in described extractant is 1%～2%.
Saccharin sodium method for quick the most according to claim 3, it is characterised in that: described step (1)
Volume ratio shared by ethanol in described extractant is preferably 2%.
Saccharin sodium method for quick the most according to claim 3, it is characterised in that: step (2)
In the solution hydrogen ion concentration of described acid medium be 0.01mol/l～4mol/l.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106932525A (en) * | 2017-03-02 | 2017-07-07 | 广州安诺食品科学技术有限公司 | Auramine O quick detection kit, detection method and the application of medicinal material in the detection |
| CN107907397A (en) * | 2017-11-23 | 2018-04-13 | 苏州泽科生物科技有限公司 | Collagenous fibres horse pine trichrome stain kit and preparation method thereof and colouring method |
| CN110031455A (en) * | 2019-04-12 | 2019-07-19 | 宜宾学院 | A kind of quick detection natural aromatic oil mixes the method and kit of puppet |
| CN113758884A (en) * | 2021-08-20 | 2021-12-07 | 西安科技大学 | Method capable of dynamically monitoring content of saccharin sodium in electrolytic copper foil plating solution |
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| CN1122336A (en) * | 1995-04-29 | 1996-05-15 | 张卫民 | Saccharin zinc and its producing process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106932525A (en) * | 2017-03-02 | 2017-07-07 | 广州安诺食品科学技术有限公司 | Auramine O quick detection kit, detection method and the application of medicinal material in the detection |
| CN106932525B (en) * | 2017-03-02 | 2018-12-21 | 广州安诺科技股份有限公司 | Auramine O quick detection kit, detection method and the application of medicinal material in the detection |
| CN107907397A (en) * | 2017-11-23 | 2018-04-13 | 苏州泽科生物科技有限公司 | Collagenous fibres horse pine trichrome stain kit and preparation method thereof and colouring method |
| CN110031455A (en) * | 2019-04-12 | 2019-07-19 | 宜宾学院 | A kind of quick detection natural aromatic oil mixes the method and kit of puppet |
| CN113758884A (en) * | 2021-08-20 | 2021-12-07 | 西安科技大学 | Method capable of dynamically monitoring content of saccharin sodium in electrolytic copper foil plating solution |
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