CN108613969A - The rapid detection method of honey element in a kind of white wine - Google Patents
The rapid detection method of honey element in a kind of white wine Download PDFInfo
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- CN108613969A CN108613969A CN201810963812.4A CN201810963812A CN108613969A CN 108613969 A CN108613969 A CN 108613969A CN 201810963812 A CN201810963812 A CN 201810963812A CN 108613969 A CN108613969 A CN 108613969A
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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Abstract
The present invention provides a kind of rapid detection method of honey element in white wine, more particularly to technical field of food safety detection, the honey element in sample is extracted using liquid-liquid extraction method, after colloidal gold or collargol and prepare liquid are mixed again, agglomerator is added, object testing molecule and colloidal gold or colloidal silver nanometer granule can form " hot spot " under the action of agglomerator, and then by the distinctive Electromagnetic enhancement effect of nano material, exclusive Raman spectrum is generated under the effect of the laser, the spectrogram as obtained by Raman spectrometer analysis, it is final to determine in sample whether contain honey element.The present invention is compared to conventional method and other rapid detection methods, improve the specificity, sensitivity, detection speed that honey element detects in white wine, reduce testing cost and operation difficulty, make the detection method of honey element in white wine more quickly, accurately, convenient for the detection of food safety detection process of supervision, such illegal addition behavior can be effectively hit.
Description
Technical field
The invention belongs to technical field of food safety detection, and in particular to the quick detection side of honey element in a kind of white wine
Method.
Background technology
Honey element is that common additive, honey element are in food production its chemical name is sodium cyclohexylsulfamate
A kind of common sweetener, sugariness are 30~40 times of sucrose.
《GB 2760-2014 national food safety standard food additives use standard》In define the limitation of honey element
Value, the Limited Doses in different food products are 0.65-1.6g/kg (in terms of cyclohexylsulfamic), and above-mentioned addition range does not include
White wine.In white wine, honey element belongs to the sweetener for forbidding addition, but illegal producer adds in violation of rules and regulations in order to improve the taste of white wine
Add honey element.
In existing detection technique, mainly have：
1. chromatography detection technique, advantage is that detection is accurate, high sensitivity；The disadvantage is that testing cost is high, detection cycle is long；
2. photometer technology, advantage is that detection speed is fast, and testing cost is low；The disadvantage is that detection limits too high, poor repeatability, inspection
Surveying result does not have application value.
3. it is inconsistent because interfering for drinks sample, testing result is influenced very big.
《The measurement of GB 5009.97-2016 national food safety standard Cyclamate in Foods》Middle sweetness
The detection of element is limited to 10mg/kg.
Therefore it is badly in need of a kind of rapid detection method of honey element in the white wine that can solve existing issue.
Invention content
The present invention in order to overcome the defect that the testing cost of existing detection technique is high, detection time is long, accuracy in detection is low,
Mating surface enhances Raman spectroscopy and Portable Raman spectrometer, using the characteristic of honey element, provides sweet tea in a kind of white wine
The rapid detection method of sweet element, this method have the advantages such as easy to operate, high sensitivity, detection speed are fast, testing cost is low.
The present invention provides the following technical solutions：
The rapid detection method of honey element, specifically comprises the following steps in a kind of white wine：
A. nanogold or nano silver colloidal sol are prepared：It takes 0.01% gold chloride or silver nitrate aqueous solution in round-bottomed flask, stirs
It mixes, be heated to boiling, according to gold chloride or silver nitrate solution：Citric acid solution=100:1% sodium citrate is added in 0.7 ratio
Solution, is heated with stirring to liquid variation as red or yellow green, room temperature cooling, and gained is nanogold or nano silver colloidal sol, often
Temperature is protected from light storage；Nanogold or nano silver colloidal sol are centrifuged under the conditions of 10000 revs/min, remove supernatant, gained lower layer is
It is protected from light storage for concentration nanogold or nano silver colloidal sol, room temperature；
B. agglomerator is prepared：The saturated solution of sodium chloride is prepared, gained is agglomerator, and room temperature is protected from light storage；
C. prepared by standard sample：Compound concentration is the honey element standard solution of 1000mg/L, and 4 DEG C of refrigerations are spare, will prepare
Standard solution, with white wine (Wine Sample use《Cyclohexyl ammonia in GB 5009.97-2016 national food safety standard food
The measurement of base sodium sulfonate》Method detects, and is confirmed as negative sample, that is, is free of the Wine Sample of honey element) gradient dilution to 100,
10,1,0.5,0mg/L, acquired solution is the standard sample of honey element in white wine；
D. isometric Wine Sample to be detected is measured；Refer to identical with the volume of standard sample；
E., the sample pH of step c and d are adjusted to the solution of ＜ 7；
F. oxidant is added into the solution of step e, is reacted with honey element；
G. target detection thing contained in solvent extraction f acquired solutions is used, gained upper solution is prepare liquid；
H. the nanogold or the agglomerator of nano silver colloidal sol and step b for using step a detect prepare liquid, are then poured into quartz
In cuvette, on Raman spectrometer, instrument parameter is set, scans the Surface enhanced Raman spectroscopy of acquisition system, positive spectrogram
Can 786,844,960 ± 3cm-1There are apparent Raman peaks at place.
I. spectrogram is smoothed, after denoising, with 844cm-1Place's peak intensity is ordinate, and a concentration of abscissa of honey element passes through
It can get canonical plotting after linear fit, linear equation is：Y=161.2x+300.7 or approximation coefficient；Then further according to mark
Directrix curve figure calculates the content of the honey element in Wine Sample to be detected.
Preferably, pH adjustings are carried out using hydrochloric acid or nitric acid or sulfuric acid or trichloroacetic acid in step e.
Preferably, the extractant in step g is one kind in n-hexane or methanol or ethyl alcohol or ethyl acetate.
Preferably, the preparation method of the honey element standard solution of 1000mg/L described in step c is：Weigh 0.01g sweetnesses
Plain standard items are settled to 10mL with deionized water.
Preferably, the oxidant being added in step f is potassium permanganate, ferric trichloride, hydrogen peroxide, hypochlorite and high chlorine
One kind in acid.
The beneficial effects of the invention are as follows：The detection method developed based on new detection technique, compared to conventional method and
Other rapid detection methods, this method improve the specificity that honey element detects in white wine, sensitivity, detection speed, reduce
Testing cost and operation difficulty, the detection method for making honey element in white wine more quickly, accurately, are supervised convenient for food safety detection
The detection of process can effectively hit such illegal addition behavior.
Description of the drawings
Attached drawing is used to provide further understanding of the present invention, and a part for constitution instruction, the reality with the present invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings：
Fig. 1 is the Surface enhanced Raman spectroscopy figure of the honey element of the standard sample of the present invention.
Specific implementation mode
The rapid detection method of honey element, specifically comprises the following steps in a kind of white wine：
A. nano gold sol is prepared：It takes 0.01% gold chloride or silver nitrate aqueous solution in round-bottomed flask, stirs, is heated to
Boiling, according to gold chloride or silver nitrate solution：Citric acid solution=100:1% sodium citrate solution, stirring is added in 0.7 ratio
Liquid variation is heated to as red or yellow green, room temperature cooling, gained is nanogold or nano silver colloidal sol, and room temperature is protected from light storage
It deposits；Nanogold or nano silver colloidal sol are centrifuged under the conditions of 10000 revs/min, remove supernatant, gained lower layer is to concentrate nanometer
Gold or nano silver colloidal sol, room temperature are protected from light storage；
B. agglomerator is prepared：The saturated solution of sodium chloride is prepared, gained is agglomerator, and room temperature is protected from light storage；
C. prepared by standard sample：0.01g honey element standard items accurately are weighed, are settled to 10mL with deionized water, this solution
For the honey element standard solution of 1000mg/L, 4 DEG C of refrigerations are spare, and with white wine, (Wine Sample uses《GB 5009.97-2016 foods
The measurement of the safe national standard Cyclamate in Foods of product》Method detects, and is confirmed as negative sample, that is, is free of sweetness
The Wine Sample of element) gradient dilution to 100,10,1,0.5,0mg/L, acquired solution is the sample of honey element in white wine；
D. isometric Wine Sample to be detected is measured；Refer to identical with the volume of standard sample；
E. hydrochloric acid or nitric acid or the solution such as sulfuric acid or trichloroacetic acid are used, the sample pH of step c and d are adjusted to ＜ 7
Solution；
F. oxidant is added into the solution of step e, is reacted with honey element, wherein oxidant is potassium permanganate, tri-chlorination
One kind in iron, hydrogen peroxide, hypochlorite and perchloric acid；
G. target contained in n-hexane or methanol or ethyl alcohol or ethyl acetate equal solvent extraction step f acquired solutions is used
Detectable substance, gained upper solution are prepare liquid；
H. the nanogold or the agglomerator of nano silver colloidal sol and step b for using step a detect prepare liquid, are then poured into quartz
In cuvette, on Raman spectrometer, instrument parameter is set, scans the Surface enhanced Raman spectroscopy of acquisition system, positive spectrogram
Can 786,844,960 ± 3cm-1There are apparent Raman peaks at place.
I. spectrogram is smoothed, after denoising, with 844cm-1Place's peak intensity is ordinate, and a concentration of abscissa of honey element passes through
It can get canonical plotting after linear fit, linear equation is：Y=161.2x+300.7 or approximation coefficient；Then further according to mark
Directrix curve figure calculates the content of the honey element in Wine Sample to be detected.
Principle
Liquid-liquid extraction is namely utilized by adjusting pH, extracting target molecule using oxidant reaction, by organic solvent
Method extracts the honey element in sample, then by after colloidal gold or nano silver and prepare liquid mixing, agglomerator is added, object is to be measured
Molecule and colloidal gold or nanometer Nano silver grain can form " hot spot " under the action of agglomerator, and then by nano material
Distinctive Electromagnetic enhancement effect, generates exclusive Raman spectrum under the effect of the laser, is composed as obtained by Raman spectrometer analysis
Figure, it is final to determine in sample whether contain honey element.
In the present embodiment, due to being free from honey element in normal white wine, therefore the sweet tea of standard sample is only tested
The measurement of sweet element, wherein the Surface enhanced Raman spectroscopy figure of the honey element of standard sample as shown in Figure 1, wherein from down to up according to
The secondary spectrogram for the corresponding honey element concentration of a-e, wherein a-e correspond to the white of the honey element of 0,0.5,1,10,100mg/L respectively
Wine.
By gradient test, that is, gradually increased Wine Sample is (happy by adding for selection honey element concentration gradients
Element, white wine is also to use herein《The survey of GB 5009.97-2016 national food safety standard Cyclamate in Foods
It is fixed》Method detects, and is confirmed as negative sample, that is, is free of the Wine Sample of honey element) make known to the honey element of examination criteria sample
The method for detecting honey element in white wine with (Surface enhanced Raman spectroscopy method) of the invention, Monitoring lower-cut is up to 0.5mg/L.
It is worth noting that since honey element is to forbid addition in white wine, whether contain when in a kind of white wine of detection
Have and only need whether the positive to be presented by qualitative detection when honey element, without calculating concrete numerical value, that is to say, that in reality
In detection process, for testing goal, it can selectively decide whether to make standard curve.
It these are only the preferred embodiment of the present invention, be not intended to restrict the invention, although with reference to the foregoing embodiments
Invention is explained in detail, for those skilled in the art, still can be to foregoing embodiments institute
The technical solution of record is modified or equivalent replacement of some of the technical features.It is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (5)
1. the rapid detection method of honey element in a kind of white wine, which is characterized in that specifically comprise the following steps：
A. nanogold or nano silver colloidal sol are prepared：Take 0.01% gold chloride or silver nitrate aqueous solution in round-bottomed flask, stirring adds
Heat is to boiling, according to chlorauric acid solution or silver nitrate solution：Citric acid solution=100:1% sodium citrate is added in 0.7 ratio
Solution, is heated with stirring to liquid variation as red or yellow green, room temperature cooling, and gained is nanogold or nano silver colloidal sol, often
Temperature is protected from light storage；Nanogold or nano silver colloidal sol are centrifuged under the conditions of 10000 revs/min, remove supernatant, gained lower layer is
It is protected from light storage for concentration nanogold or nano silver colloidal sol, room temperature；
B. agglomerator is prepared：The saturated solution of sodium chloride is prepared, gained is agglomerator, and room temperature is protected from light storage；
C. prepared by standard sample：Compound concentration is the honey element standard solution of 1000mg/L, and 4 DEG C of refrigerations are spare, by the mark of preparation
Quasi- solution, with white wine, (Wine Sample uses《Cyclohexylamino sulphur in GB 5009.97-2016 national food safety standard food
The measurement of sour sodium》Method detects, and is confirmed as negative sample, that is, is free of the Wine Sample of honey element) gradient dilution to 100,10,1,
0.5,0mg/L, acquired solution are the standard sample of honey element in white wine；
D. isometric Wine Sample to be detected is measured；
E., the sample pH of step c and d are adjusted to the solution of ＜ 7；
F. oxidant is added into the solution of step e, is reacted with honey element；
G. target determinand contained in solvent extraction f acquired solutions is used, gained upper solution is prepare liquid；
H. the nanogold or the agglomerator of nano silver colloidal sol and step b for using step a detect prepare liquid, are then poured into quartz cuvette
In ware, on Raman spectrometer, instrument parameter is set, scans the Surface enhanced Raman spectroscopy of acquisition system, positive spectrogram can be
786、844、960±3cm-1There are apparent Raman peaks at place.
I. spectrogram is smoothed, after denoising, with 844cm-1Place's peak intensity is ordinate, a concentration of abscissa of honey element, by linear
It can get canonical plotting after fitting, linear equation is：Y=161.2x+300.7 or approximation coefficient；Then further according to standard song
Line chart calculates the content of honey element in Wine Sample to be detected.
2. the rapid detection method of honey element in white wine according to claim 1, which is characterized in that use salt in step e
Acid or nitric acid or sulfuric acid or trichloroacetic acid carry out pH adjustings.
3. the rapid detection method of honey element in white wine according to claim 1, which is characterized in that the extraction in step g
Solvent is one kind in n-hexane or methanol or ethyl alcohol or ethyl acetate.
4. the rapid detection method of honey element in white wine according to claim 1, which is characterized in that described in step c
The preparation method of the honey element standard solution of 1000mg/L is：0.01g honey element standard items are weighed, are settled to deionized water
10mL。
5. the rapid detection method of honey element in white wine according to claim 1, which is characterized in that be added in step f
Oxidant is potassium permanganate or ferric trichloride or hydrogen peroxide or hypochlorite or perchloric acid.
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Cited By (9)
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| CN110333216A (en) * | 2018-12-29 | 2019-10-15 | 厦门市普识纳米科技有限公司 | The detection method of xacin-series antibiotic in a kind of animal foodstuff |
| CN110501323A (en) * | 2019-09-03 | 2019-11-26 | 绍兴谱分科技有限公司 | A kind of dioxin pollution object rapid detection method based on enhancing Raman spectroscopy |
| CN110791655A (en) * | 2019-11-24 | 2020-02-14 | 长春黄金研究院烟台贵金属材料研究所有限公司 | Method for recycling and reusing nano gold |
| CN110987899A (en) * | 2019-12-09 | 2020-04-10 | 西安电子科技大学 | Method for measuring content of total acid total esters in white spirit and identifying quality grade of white spirit |
| CN111912929A (en) * | 2020-06-01 | 2020-11-10 | 厦门大学 | Aflatoxin B1Extraction method and application of |
| CN112098387A (en) * | 2020-08-18 | 2020-12-18 | 普拉瑞思科学仪器（苏州）有限公司 | Surface enhanced Raman detection method for detecting whether quinizarine dye is doped in diesel oil |
| CN112213294A (en) * | 2020-09-22 | 2021-01-12 | 立穹(上海)光电科技有限公司 | Method for rapidly detecting sildenafil in health-care product |
| CN112577940A (en) * | 2019-09-30 | 2021-03-30 | 厦门大学 | Method for rapidly and quantitatively detecting concentration of creatinine in urine at low cost |
| CN116297389A (en) * | 2023-02-15 | 2023-06-23 | 中国人民解放军空军特色医学中心 | Drug detection method capable of causing driving operation disability in biological sample at accident site |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110333216A (en) * | 2018-12-29 | 2019-10-15 | 厦门市普识纳米科技有限公司 | The detection method of xacin-series antibiotic in a kind of animal foodstuff |
| CN110501323A (en) * | 2019-09-03 | 2019-11-26 | 绍兴谱分科技有限公司 | A kind of dioxin pollution object rapid detection method based on enhancing Raman spectroscopy |
| CN110501323B (en) * | 2019-09-03 | 2021-12-31 | 绍兴谱分科技有限公司 | Rapid detection method for dioxin pollutants based on enhanced Raman spectroscopy |
| CN112577940A (en) * | 2019-09-30 | 2021-03-30 | 厦门大学 | Method for rapidly and quantitatively detecting concentration of creatinine in urine at low cost |
| CN110791655A (en) * | 2019-11-24 | 2020-02-14 | 长春黄金研究院烟台贵金属材料研究所有限公司 | Method for recycling and reusing nano gold |
| CN110987899A (en) * | 2019-12-09 | 2020-04-10 | 西安电子科技大学 | Method for measuring content of total acid total esters in white spirit and identifying quality grade of white spirit |
| CN111912929A (en) * | 2020-06-01 | 2020-11-10 | 厦门大学 | Aflatoxin B1Extraction method and application of |
| CN112098387A (en) * | 2020-08-18 | 2020-12-18 | 普拉瑞思科学仪器（苏州）有限公司 | Surface enhanced Raman detection method for detecting whether quinizarine dye is doped in diesel oil |
| CN112213294A (en) * | 2020-09-22 | 2021-01-12 | 立穹(上海)光电科技有限公司 | Method for rapidly detecting sildenafil in health-care product |
| CN116297389A (en) * | 2023-02-15 | 2023-06-23 | 中国人民解放军空军特色医学中心 | Drug detection method capable of causing driving operation disability in biological sample at accident site |
| CN116297389B (en) * | 2023-02-15 | 2023-12-26 | 中国人民解放军空军特色医学中心 | Drug detection method capable of causing driving operation disability in biological sample at accident site |
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Application publication date: 20181002 |