CN103076428A - Method for detecting content of saccharin sodium in feed sweetening agent - Google Patents
Method for detecting content of saccharin sodium in feed sweetening agent Download PDFInfo
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- CN103076428A CN103076428A CN2013100403101A CN201310040310A CN103076428A CN 103076428 A CN103076428 A CN 103076428A CN 2013100403101 A CN2013100403101 A CN 2013100403101A CN 201310040310 A CN201310040310 A CN 201310040310A CN 103076428 A CN103076428 A CN 103076428A
- Authority
- CN
- China
- Prior art keywords
- saccharin
- saccharin sodium
- asccharin
- sweetener
- content
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 235000003599 food sweetener Nutrition 0.000 title claims abstract description 40
- 239000003765 sweetening agent Substances 0.000 title claims abstract description 40
- FTLYMKDSHNWQKD-UHFFFAOYSA-N (2,4,5-trichlorophenyl)boronic acid Chemical compound OB(O)C1=CC(Cl)=C(Cl)C=C1Cl FTLYMKDSHNWQKD-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229940085605 saccharin sodium Drugs 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001514 detection method Methods 0.000 claims abstract description 22
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical class C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000012266 salt solution Substances 0.000 claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003513 alkali Substances 0.000 claims abstract description 9
- 239000002274 desiccant Substances 0.000 claims abstract description 9
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 5
- 230000000694 effects Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000013213 extrapolation Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000001838 alkalimetric titration Methods 0.000 claims description 2
- 229940081974 saccharin Drugs 0.000 abstract 3
- 235000019204 saccharin Nutrition 0.000 abstract 3
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 abstract 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract 2
- 239000000969 carrier Substances 0.000 abstract 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 12
- 238000004448 titration Methods 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000010446 mirabilite Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- -1 purity Chemical compound 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses a method for detecting the content of saccharin sodium in feed sweetening agent. The method comprises the following steps that 1, sweetening agent samples are dissolved by saturated saccharin salt solution; 2, excessive hydrochloric acid is added so that the saccharin sodium generates saccharin under the strong acid conditions; 3, after a small amount of hydrofluoric acid is dripped, filter paper is used for filtering, and purified saccharin is obtained; 4, washing is carried out; 5, the purified saccharin is put into a beaker containing hot alcohol for dissolving, phenolphthalein is added, then, alkali is used for dripping until solution generates reddish color, in addition, the color cannot be faded within 30s, and the consumed alkali quantity is recorded; and 6, the content of the saccharin sodium in the feed sweetening agent can be obtained through calculation. The method has the advantages that the influence caused by drying agent and carriers is reduced, the detection of the content of the saccharin sodium in the feed sweetening agent is more precise, and the consumed detection time is about 30 minutes and is greatly shortened.
Description
Technical field
The present invention relates to the improvement of saccharin sodium content detection technology, specifically refer to a kind of method that detects saccharin sodium content in the feed sweetener, belong to saccharin sodium content detection technical field.
Background technology
Prior art mainly contains two kinds of means to the detection of saccharin sodium content: 1. perchloric acid titration method; 2. high performance liquid chromatography.The perchloric acid titration method is that the saccharin sodium sterling detects the method in the GB, and the advantage that the perchloric acid titration method detects is: consuming time short, and high to the sterling accuracy in detection.Shortcoming is: specificity is strong, can only be used for sterling and detect, and is unstable to the product testing result of the saccharin sodium that adds auxiliary material, easily is subjected to the impact of auxiliary material.Because feed sweetener except saccharin sodium, also contains a certain amount of carrier and drying agent, carrier and drying agent detect the perchloric acid titration method disturbing effect, so the perchloric acid titration method is not high to the detection accuracy of saccharin sodium content in the sweetener.Although the high performance liquid chromatography testing result is accurate, there is significantly deficiency, such as length consuming time, detecting probably needs two hours, and the front also has six hours setup time, and chromatographic column is easily polluted; The specificity of pillar is strong, and is also not high to the detection accuracy of saccharin sodium content in the sweetener.
Summary of the invention
For the accuracy not high deficiency of prior art to saccharin sodium content detection existence in the feed sweetener, the object of the present invention is to provide a kind of not only accuracy in detection high, and the method that saccharin sodium content in the feed sweetener is detected of short, more convenient operation consuming time.
To achieve these goals, the technical solution used in the present invention is such:
Saccharin sodium detection method of content in a kind of feed sweetener, it is characterized in that: detecting step is as follows:
1) with saturated saccharin salt solution dissolving sweetener sample, the saturated saccharin salt solution that every gram sweetener sample needs is 10-20ml;
2) to the 1st) add excessive hydrochloric acid in the step gained solution, and regulate PH＜1, and make saccharin sodium under the strong acid condition of PH＜1, generate asccharin, leave standstill after the stirring until container bottom is separated out pure asccharin fully;
3) to the 2nd) drip a small amount of hydrofluorite in the step gained solution to reduce the formation of drying agent and Support effect and complex compound in the sweetener, stir to leave standstill after 2-3 minute and use Filter paper filtering, obtain pure asccharin;
4) the pure asccharin that filtration is obtained is used first saturated saccharin salt solution washing 2-3 time, and then washs 2-3 time with distilled water;
5) with the 4th) pure asccharin after the step washing puts into the beaker that fills hot alcohol together with filter paper and dissolves, and adds phenolphthalein, again with alkalimetric titration until blush appears in solution, and colour-fast in 30s, record the amount of the alkali that consumes;
6) calculate the amount of pure asccharin by the titer of alkali, obtained again the amount of saccharin sodium by the amount Extrapolation of pure asccharin, can obtain the content of saccharin sodium in the feed sweetener.
Further, the 3rd) hydrofluorite adds by the amount of every gram sweetener sample 0.2-0.5g in the step.
The 5th) the alcohol temperature is 60-80 ℃ in the step, and the amount of alcohol is the corresponding 30-50ml of every gram sweetener sample.
Compared to existing technology, the present invention has following beneficial effect:
1, the present invention has farthest reduced drying agent and Support effect, and the saccharin sodium content detection is more accurate in the feed sweetener, only differs 0.1%-0.7% with the sample comparative result of known content, and degree of accuracy is higher.
2, this method detects about 30min consuming time, compares with high performance liquid chromatography, detects significantly shortening consuming time, even compare with original perchloric acid titration method, detection also more saves time.
The present invention is except high to the asccharin accuracy in detection of composite carrier, and is equally applicable to the detection of pure asccharin, and easy to operate.
Embodiment
The invention will be further described below in conjunction with embodiment.
Saccharin sodium detection method of content in the feed sweetener of the present invention, detecting step is as follows:
1) with saturated saccharin salt solution dissolving sweetener sample, the saturated saccharin salt solution that every gram sweetener sample needs is 10-20ml; Saturated saccharin salt solution is that asccharin and salt all are saturated in aqueous solution, forms mixed solution;
2) to the 1st) add excessive hydrochloric acid in the step gained solution, and regulate PH＜1, and make saccharin sodium under the strong acid condition of PH＜1, generate asccharin, leave standstill after the stirring until container bottom is separated out pure asccharin fully;
During practical operation, add the amount of 2.0ml hydrochloric acid to the 1st by every gram sweetener sample) splash into hydrochloric acid in the step gained solution, the hydrochloric acid proportioning is 3:1, namely the distilled water of the concentrated hydrochloric acid of 3 parts of volumes and 1 part of volume is formulated; The concentration of commercially available concentrated hydrochloric acid is 37%, and experiment is generally 37.5% with concentrated hydrochloric acid, all can be used for this method; Such hydrochloric acid addition had both guaranteed reacting dose (although saccharin sodium content is uncertain in the sweetener sample, its content approximate range still can be determined), had guaranteed again PH＜1;
3) to the 2nd) drip a small amount of hydrofluorite in the step gained solution to reduce the formation of drying agent and Support effect and complex compound in the sweetener, stir to leave standstill after 2-3 minute and use Filter paper filtering, obtain pure asccharin; Hydrofluorite adds by the amount of every gram sweetener sample 0.2-0.5g, and the effect of hydrofluorite is to make filter velocity faster;
4) the pure asccharin that filtration is obtained is used first saturated saccharin salt solution washing 2-3 time, and then washs 2-3 time with distilled water;
5) with the 4th) pure asccharin after the step washing puts into the beaker that fills hot alcohol together with filter paper and dissolves, add phenolphthalein, use again alkali (KOH or NaOH) titration until blush appears in solution, and colour-fast in 30s, the amount of the record alkali that consumes (KOH or NaOH).Pure asccharin solubleness in hot alcohol is better, and the alcohol temperature is 60-80 ℃, and the amount of alcohol is the corresponding 30-50ml of every gram sweetener sample;
6) calculate the amount of pure asccharin by the titer of alkali, obtained again the amount of saccharin sodium by the amount Extrapolation of pure asccharin, can obtain the content of saccharin sodium in the feed sweetener.
The whole detection principle of this method is, saccharin sodium can generate asccharin under the strong acid condition of PH＜1, and asccharin do not dissolve in saturated saccharin salt solution, draws the content of saccharin sodium in the sample by conversion.Reaction equation is:
C
7H
4NNaO
3S +HCL
C
7H
5O
3NS+NaCL
Although the 1st) step and the 4th) step has been used saturated saccharin salt solution, namely added asccharin, but because the asccharin in the saturated saccharin salt solution has been dissolved in the salt solusion, the state with solid does not present, and this method the 2nd) asccharin of step reaction generation is again because saccharin salt solution is saturated, can not be dissolved in the saturated saccharin salt solution, stay with the solids of sedimentation form fully in washing process, therefore the asccharin in the saturated saccharin salt solution can not cause interference to final content detection.All can not exert an influence to measurement result after drying agent, carrier and the HCL reaction yet.
The 6th) in the step " being obtained the amount of saccharin sodium by the amount Extrapolation of pure asccharin ", carry out Extrapolation by above-mentioned reaction equation exactly.
The feasibility of this method is verified in comparative study by the following examples.
Get six clean triangular flasks, number respectively 1-6 number, in each triangular flask, add respectively the 2g saccharin sodium, and then in the 1-6 triangular flask, add respectively the 0.15g drying agent, add respectively 2.85g glauber salt (carrier a kind of) in the most backward 1-3 triangular flask, add respectively 2.85g dry powder (carrier a kind of) in the 4-6 triangular flask, all weighing accurate countings, just configure like this 5g feed sweetener sample in each triangular flask, can directly calculate saccharin sodium content=m in this feed sweetener by layoutprocedure
Sugar/ m
Always* ω (ω is the effective content coefficient of saccharin sodium, i.e. purity, the present embodiment is 98.2%) namely obtains standard value.Then detect operation according to the method for the invention, the record result calculates actual value, and calculates error.
The present invention is to the testing result of 6 groups of samples following (wherein actual value is the value of actual measurement gained, the prescription value of standard value for adding).Can find out from following result, press the detected result of this method and standard value error about 0.5%;
Carrier is glauber salt: the standard value actual value
No. 1 39.28% 39.22%
No. 2 39.28% 39.16%
No. 3 39.28% 39.40%
Carrier is dry powder: the standard value actual value
No. 4 39.28% 39.34%
No. 5 39.28% 39.14%
No. 6 39.28% 39.26%
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although with reference to preferred embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not breaking away from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (3)
1. saccharin sodium detection method of content in the feed sweetener, it is characterized in that: detecting step is as follows:
1) with saturated saccharin salt solution dissolving sweetener sample, the saturated saccharin salt solution that every gram sweetener sample needs is 10-20ml;
2) to the 1st) add excessive hydrochloric acid in the step gained solution, and regulate PH＜1, and make saccharin sodium under the strong acid condition of PH＜1, generate pure asccharin, leave standstill after the stirring until container bottom is separated out pure asccharin fully;
3) to the 2nd) drip a small amount of hydrofluorite in the step gained solution to reduce the formation of drying agent and Support effect and complex compound in the sweetener, stir to leave standstill after 2-3 minute and use Filter paper filtering, obtain pure asccharin;
4) the pure asccharin that filtration is obtained is used first saturated saccharin salt solution washing 2-3 time, and then washs 2-3 time with distilled water;
5) with the 4th) pure asccharin after the step washing puts into the beaker that fills hot alcohol together with filter paper and dissolves, and adds phenolphthalein, again with alkalimetric titration until blush appears in solution, and colour-fast in 30s, record the amount of the alkali that consumes;
6) calculate the amount of pure asccharin by the titer of alkali, obtained again the amount of saccharin sodium by the amount Extrapolation of pure asccharin, can obtain the content of saccharin sodium in the feed sweetener.
2. saccharin sodium detection method of content in the feed sweetener according to claim 1 is characterized in that: the amount interpolation that the 3rd) hydrofluorite is pressed every gram sweetener sample 0.2-0.5g in the step.
3. saccharin sodium detection method of content in the feed sweetener according to claim 1 is characterized in that: the 5th) the alcohol temperature is 60-80 ℃ in the step, and the amount of alcohol is the corresponding 30-50ml of every gram sweetener sample.
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| CN201310040310.1A CN103076428B (en) | 2013-02-01 | 2013-02-01 | Method for detecting content of saccharin sodium in feed sweetening agent |
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| CN201310040310.1A CN103076428B (en) | 2013-02-01 | 2013-02-01 | Method for detecting content of saccharin sodium in feed sweetening agent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103743856A (en) * | 2013-12-21 | 2014-04-23 | 广西科技大学 | Method for detecting saccharin sodium salt serving as sweetening agent |
| CN105572289A (en) * | 2016-02-26 | 2016-05-11 | 重庆民泰香料化工有限责任公司 | Method for detecting content of NHDC (Neohesperidin Dihydrochalcone) in mixed type feed additive |
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| CN101634648A (en) * | 2009-08-21 | 2010-01-27 | 江南大学 | Method for detecting six trace sweetening agents in white spirit by ultra-high pressure liquid chromatography and time-of-flight mass spectrometry |
| US7763431B1 (en) * | 2001-03-07 | 2010-07-27 | Senomyx, Inc. | Binding assays that use the T1R2/T1R3 (sweet) taste receptor to identify compounds that elicit or modulate sweet taste |
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2013
- 2013-02-01 CN CN201310040310.1A patent/CN103076428B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7763431B1 (en) * | 2001-03-07 | 2010-07-27 | Senomyx, Inc. | Binding assays that use the T1R2/T1R3 (sweet) taste receptor to identify compounds that elicit or modulate sweet taste |
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| CN101634648A (en) * | 2009-08-21 | 2010-01-27 | 江南大学 | Method for detecting six trace sweetening agents in white spirit by ultra-high pressure liquid chromatography and time-of-flight mass spectrometry |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103743856A (en) * | 2013-12-21 | 2014-04-23 | 广西科技大学 | Method for detecting saccharin sodium salt serving as sweetening agent |
| CN105572289A (en) * | 2016-02-26 | 2016-05-11 | 重庆民泰香料化工有限责任公司 | Method for detecting content of NHDC (Neohesperidin Dihydrochalcone) in mixed type feed additive |
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| CN103076428B (en) | 2014-09-10 |
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Denomination of invention: A method for determination of saccharin sodium content in feed sweetener Effective date of registration: 20210219 Granted publication date: 20140910 Pledgee: Chongqing Branch of China Everbright Bank Co.,Ltd. Pledgor: CHONGQING MINTAI NEW AGROTECH DEVELOPMENT GROUP Co.,Ltd. Registration number: Y2021500000005 |
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Denomination of invention: A method for detecting sodium saccharin content in a feed sweetener Granted publication date: 20140910 Pledgee: Chongqing Branch of China Everbright Bank Co.,Ltd. Pledgor: CHONGQING MINTAI NEW AGROTECH DEVELOPMENT GROUP Co.,Ltd. Registration number: Y2024500000032 |