CN103353450B - The method for quick of saccharin sodium in a kind of wine product - Google Patents
The method for quick of saccharin sodium in a kind of wine product Download PDFInfo
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- CN103353450B CN103353450B CN201310273537.0A CN201310273537A CN103353450B CN 103353450 B CN103353450 B CN 103353450B CN 201310273537 A CN201310273537 A CN 201310273537A CN 103353450 B CN103353450 B CN 103353450B
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Abstract
The invention discloses the method for quick of saccharin sodium in a kind of wine product, it comprises the steps:, and (1) prepares Raman detection nano particle, (2) the saccharin sodium titer of variable concentrations is prepared, (3) Raman detection nano particle mixes with the saccharin sodium standard wine liquid of variable concentrations respectively, Raman spectrometer carries out Raman spectrum detection to it, obtains the saccharin sodium SERS collection of illustrative plates of variable concentrations; (4) calculate the characteristic peak intensity of the saccharin sodium SERS collection of illustrative plates of variable concentrations, obtain the SERS intensity-concentration relationship curve of saccharin sodium; (5) wine liquid to be measured is carried out Raman spectrum detection, by the characteristic peak of SERS collection of illustrative plates that obtains and the curve control of step (4), whether judge in wine liquid to be measured containing saccharin sodium.It is fast that the present invention has detection speed, and testing cost is low, and to testing staff without any professional technique requirement, can realize the advantages such as detection fast.
Description
Technical field
The present invention relates to the method for quick of saccharin sodium in a kind of wine product.
Background technology
Sweetener is the important food additives of a class, and its gives food with sweet taste, improves the quality of food, have heat low, be applicable to the advantages such as diabetes patient.Sweetener can be divided into natural sweetener and artificial synthesis edulcorant by its source.In modern food industry the artificial synthesis edulcorant of widespread use mainly to comprise saccharin sodium, honey element, Aspartame, acesulfame potassium, Sucralose, alitame and knob sweet.Wherein saccharin sodium is the most ancient sweetener.Asccharin was found in 1878 by American scientist, was accepted soon by food industry circle and consumer.Asccharin chemical name is o-benzoic sulfimide, and the commodity asccharin of market sale is actual is the sodium salt of the o-benzoic sulfimide of ease of solubility, is called for short saccharin sodium.The sugariness of saccharin sodium is about 450 ~ 550 times of sucrose, thus its 100,000/ aqueous solution and pleasantly sweet sense.Saccharin sodium is organic chemical industry's sintetics, is food additives instead of food, except cause sweet sensation in the sense of taste except, to human body without any nutritive value.On the contrary, when edible more asccharin, the normal secretions of gastrointestinal disturbances enzyme can be affected, reduce the receptivity of small intestine, make anorexia.
White wine is the distinctive national tradition product of China, has the history of more than one thousand years, due to its unique style, deeply likes by consumers in general, also enjoys high reputation in the world, be called as " national treasure ".For protection China national tradition product, do not allow in its production run of clear stipulaties in national standard to add sweetener.But indivedual manufacturing enterprises are the bitterness hiding wine, keep wine soma ice-cold, mellow, soft, still wine production and to blend in process in violation of rules and regulations with the addition of the sweeteners such as saccharin sodium, especially white wine.
At present, the detection method of adding sweetener in wine is mainly contained: high performance liquid chromatography, HPLC-MS technology, ultra-performance liquid chromatography-mass spectrometric hyphenated technique (as disclosed the method for six kinds of micro-sweeteners in a kind of ultrahigh pressure liquid phase chromatogram-flight time mass spectrum Simultaneously test white wine in CN200910184787.0), chromatography of ions, colourimetry, thin layer chromatography etc.These detection methods all need to carry out complicated pre-treatment to wine product, and operate lengthy and jumbled consuming time, and there are certain requirements testing staff's professional skill, testing cost is also higher, and detection time is long, is unfavorable for popularizing in a line supervision department.
Summary of the invention
The object of the present invention is to provide the method for quick of saccharin sodium in a kind of wine product, to solve the above-mentioned problems in the prior art.
Technical scheme provided by the invention is as follows:
In wine product, a method for quick for saccharin sodium, comprises the steps:
(1) Raman detection nano particle is prepared,
(2) the saccharin sodium titer of variable concentrations is prepared,
(3) Raman detection nano particle mixes with the saccharin sodium titer of variable concentrations respectively, and Raman spectrometer carries out Raman spectrum detection to it, obtains the saccharin sodium SERS collection of illustrative plates of variable concentrations;
(4) calculate the characteristic peak intensity of the saccharin sodium SERS collection of illustrative plates of variable concentrations, obtain the SERS intensity-concentration relationship curve of saccharin sodium;
(5) wine liquid to be measured is carried out Raman spectrum detection, by the characteristic peak of SERS collection of illustrative plates that obtains and the spectral contrast of step (3), whether judge in wine liquid to be measured containing saccharin sodium.
Separately can also according to the Raman spectrum curve of wine liquid to be measured, and the curve control of step (4), obtain the concentration of saccharin sodium.
Raman detection nano particle of the present invention comprises Au, Ag or copper nano-particle.These nano particles and preparation method thereof are prior art.
In the preferred embodiment, described Raman detection nano particle is 50-300nm.
Wine of the present invention comprises white wine, red wine or rice wine.
In the preferred embodiment, the operation of step (2) is as follows:
A, get 0.1000g saccharin sodium, dissolve, constant volume is in 100ml volumetric flask, and this is 1000ppm saccharin sodium standard solution;
B, again according to step a preparation standard solution, preparation 100ppm, 50ppm, 10ppm, 1ppm, 100ppb saccharin sodium titer.
In the preferred embodiment, the operation of step (3) is as follows:
The centrifugal concentrating of a, nano particle: by ultrasonic for nano particle 5min, mixing, gets 1.5ml colloidal sol in the plastic centrifuge tube of 1.5ml, centrifugal 8000rmp/min, 5min; Removing supernatant, retains the colloidal sol of 10ul;
B, Raman detection: portable Raman spectrometer, optical maser wavelength 785nm, power 280mW; Extract 200ul liquid to be measured and 10ul nano particle with the liquid-transfering gun of 200ul to mix and be placed in removable ELISA Plate.Laser spot is focused in the surface of determinand, then start to adopt spectrum, adopt spectrum time 1s, average time 1, cumulative frequency 1.
Seen from the above description, the invention provides the method for quick of saccharin sodium in a kind of wine product, in conjunction with high-sensitive Surface enhanced raman spectroscopy technology, realize the quick detection to saccharin sodium in wine product, have detection speed fast (T.T. is about 30s), detect and be limited to 1ppm, testing cost is low, and to testing staff without professional technique requirement, quick detection can be realized.
Accompanying drawing explanation
Fig. 1 is the testing result figure of the embodiment of the present invention 2.
Curve is from the bottom to top respectively: 100ppb, 1ppm, 10ppm, 50ppm, 100ppm and blank.
Fig. 2 is the testing result figure of the embodiment of the present invention 3;
Fig. 3 is the testing result figure of the embodiment of the present invention 4;
Fig. 4 is the testing result figure of the embodiment of the present invention 5.
Embodiment
The preparation of embodiment 155nmAu
Getting 200mL massfraction is that the aqueous solution of chloraurate of 0.01% is in 250mL round-bottomed flask, reflux heating is to boiling under magnetic stirring, then the sodium citrate aqueous solution that 1.4mL massfraction is 1% is added rapidly, solution becomes black within half a minute, continue reflux heating 40min, solution gradually becomes brownish red by faint yellow, naturally cools to room temperature after making its complete reaction, can obtain the golden nanometer particle colloidal sol that diameter is about 55 ± 10nm.
Embodiment 2
The preparation of saccharin sodium titer:
Get 0.1000g saccharin sodium (producer, purity), dissolve, constant volume is in 100ml volumetric flask.This is 1000ppm saccharin sodium standard solution.
The preparation of saccharin sodium titer: according to the saccharin sodium standard solution of the 1000ppm prepared, then prepare 100ppm, 50ppm above, 10ppm, 1ppm, 100ppb saccharin sodium titer.
The centrifugal concentrating of 55nmAu (Citratesodium):
By ultrasonic for 55nmAu 5min, mixing, gets 1.5ml colloidal sol in the plastic centrifuge tube of 1.5ml, centrifugal (8000rmp/min, 5min).Removing supernatant, retains the colloidal sol of about 10ul.
In embodiment 3 white wine, saccharin sodium detects
Certain brand white wine commercial, detects not containing saccharin sodium through other method
One control group (blank) is set
One saccharin sodium group (add saccharin sodium solution in the wine liquid of blank, make it contain the saccharin sodium of 1ppm)
1, instrument: the portable Raman spectrometer in Tyke must be answered, optical maser wavelength 785nm, power 280mW.
2,200ul liquid to be measured is extracted with the liquid-transfering gun (producer) of 200ul and 10ul55nmAu mixes (blackening of colloidal sol color) and is placed in removable ELISA Plate.Laser spot is focused in the surface of determinand, then start to adopt spectrum, adopt spectrum time 1s, average time 1, cumulative frequency 1.(note: this process is wanted fast).
Note: the above whole room temperature that operates in is carried out.
Testing result is shown in Fig. 2
In embodiment 4 grape wine, saccharin sodium detects
Certain brand grape wine commercial, detects not containing saccharin sodium through other method
One control group (blank) is set
One saccharin sodium group (add saccharin sodium solution in the wine liquid of blank, make it contain the saccharin sodium of 1ppm)
1, instrument: the portable Raman spectrometer in Tyke must be answered, optical maser wavelength 785nm, power 280mW.
2,200ul liquid to be measured is extracted with the liquid-transfering gun (producer) of 200ul and 10ul55nmAu mixes (blackening of colloidal sol color) and is placed in removable ELISA Plate.Laser spot is focused in the surface of determinand, then start to adopt spectrum, adopt spectrum time 1s, average time 1, cumulative frequency 1.(note: this process is wanted fast).
Note: the above whole room temperature that operates in is carried out.
Testing result is shown in Fig. 3
In embodiment 3 rice wine, saccharin sodium detects
Certain brand rice wine commercial, detects not containing saccharin sodium through other method
One control group (blank) is set
One saccharin sodium group (add saccharin sodium solution in the wine liquid of blank, make it contain the saccharin sodium of 1ppm)
1, instrument: the portable Raman spectrometer in Tyke must be answered, optical maser wavelength 785nm, power 280mW.
2,200ul liquid to be measured is extracted with the liquid-transfering gun (producer) of 200ul and 10ul55nmAu mixes (blackening of colloidal sol color) and is placed in removable ELISA Plate.Laser spot is focused in the surface of determinand, then start to adopt spectrum, adopt spectrum time 1s, average time 1, cumulative frequency 1.(note: this process is wanted fast).
Note: the above whole room temperature that operates in is carried out.
Testing result is shown in Fig. 4
Claims (5)
1. the method for quick of saccharin sodium in wine product, comprises the steps:
(1) Raman detection nano particle is prepared,
(2) the saccharin sodium titer of variable concentrations is prepared,
(3) Raman detection nano particle mixes with the saccharin sodium titer of variable concentrations respectively, and Raman spectrometer carries out Raman spectrum detection to it, obtains the saccharin sodium SERS collection of illustrative plates of variable concentrations; The operation of step (3) is as follows:
The centrifugal concentrating of a, nano particle: by ultrasonic for nano particle 5min, mixing, gets 1.5ml colloidal sol in the plastic centrifuge tube of 1.5ml, centrifugal 8000rmp/min, 5min; Removing supernatant, retains the colloidal sol of 10 μ l;
B, Raman detection: portable Raman spectrometer; Extract 200 μ l liquid to be measured and 10 μ l nano particles with the liquid-transfering gun of 200 μ l to mix and be placed in removable ELISA Plate; Laser spot is focused in the surface of determinand, then start to adopt spectrum, adopt spectrum time 1s, average time 1, cumulative frequency 1;
(4) calculate the characteristic peak intensity of the saccharin sodium SERS collection of illustrative plates of variable concentrations, obtain the SERS intensity-concentration relationship curve of saccharin sodium;
(5) wine liquid to be measured is carried out Raman spectrum detection, by the characteristic peak of SERS collection of illustrative plates that obtains and the spectral contrast of step (3), whether judge in wine liquid to be measured containing saccharin sodium; And/or
According to the Raman spectrum curve of wine liquid to be measured, and the curve control of step (4), obtain the concentration of saccharin sodium.
2. the method for quick of saccharin sodium in a kind of wine product as claimed in claim 1, is characterized in that: described Raman detection nano particle comprises Au, Ag or copper nano-particle.
3. the method for quick of saccharin sodium in a kind of wine product as claimed in claim 2, is characterized in that: described Raman detection nano particle is 50-300nm.
4. the method for quick of saccharin sodium in a kind of wine product as claimed in claim 1, is characterized in that: wine comprises white wine, red wine or rice wine.
5. the method for quick of saccharin sodium in a kind of wine product as claimed in claim 1, it is characterized in that, the operation of step (2) is as follows:
A, get 0.1000g saccharin sodium, dissolve, constant volume is in 100ml volumetric flask, and this is 1000ppm saccharin sodium standard solution;
B, again according to step a preparation standard solution, preparation 100ppm, 50ppm, 10ppm, 1ppm, 100ppb saccharin sodium titer.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104568902B (en) * | 2014-12-31 | 2017-02-22 | 苏州优谱德精密仪器科技有限公司 | Wine liquid detection device |
| CN105606584A (en) * | 2015-12-15 | 2016-05-25 | 厦门出入境检验检疫局检验检疫技术中心 | Method and system for identifying consistency of articles by using Raman spectroscopy |
| CN106770162A (en) * | 2016-12-18 | 2017-05-31 | 江苏师范大学 | A kind of substrate of SERS for detecting sweetener and its preparation method and application |
| CN108613969A (en) * | 2018-08-23 | 2018-10-02 | 普拉瑞思科学仪器（苏州）有限公司 | The rapid detection method of honey element in a kind of white wine |
| CN110186901A (en) * | 2019-06-14 | 2019-08-30 | 绍兴谱分科技有限公司 | Quickly detection has the method for the alcoholic strength of color wine |
| CN112033948A (en) * | 2020-08-21 | 2020-12-04 | 江苏师范大学 | Surface-enhanced Raman test paper and preparation method and application thereof |
| CN113155806A (en) * | 2021-03-23 | 2021-07-23 | 浙江大学山东工业技术研究院 | Method for determining content of saccharin sodium in beverage based on surface enhanced Raman spectroscopy |
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| CN101629906A (en) * | 2008-07-20 | 2010-01-20 | 欧普图垂斯科技有限公司 | Method and system for detecting special chemical substance in the detected object |
| CN102072894A (en) * | 2009-11-25 | 2011-05-25 | 欧普图斯(苏州)光学纳米科技有限公司 | Nano-structure-based spectrum detecting method for detecting chemical and biochemical impurities |
| CN102109467A (en) * | 2010-12-08 | 2011-06-29 | 中国科学院半导体研究所 | Method for quantitatively detecting trace rhodamine 6G |
| CN102127542A (en) * | 2010-12-27 | 2011-07-20 | 江南大学 | Preparation method of self-assembly material having surface-enhanced Raman activity |
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| CN101629906A (en) * | 2008-07-20 | 2010-01-20 | 欧普图垂斯科技有限公司 | Method and system for detecting special chemical substance in the detected object |
| CN102072894A (en) * | 2009-11-25 | 2011-05-25 | 欧普图斯(苏州)光学纳米科技有限公司 | Nano-structure-based spectrum detecting method for detecting chemical and biochemical impurities |
| CN102109467A (en) * | 2010-12-08 | 2011-06-29 | 中国科学院半导体研究所 | Method for quantitatively detecting trace rhodamine 6G |
| CN102127542A (en) * | 2010-12-27 | 2011-07-20 | 江南大学 | Preparation method of self-assembly material having surface-enhanced Raman activity |
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