CN107727640A - A kind of method for differentiating essence spice for cigarette using SERS method - Google Patents
A kind of method for differentiating essence spice for cigarette using SERS method Download PDFInfo
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- CN107727640A CN107727640A CN201711296895.8A CN201711296895A CN107727640A CN 107727640 A CN107727640 A CN 107727640A CN 201711296895 A CN201711296895 A CN 201711296895A CN 107727640 A CN107727640 A CN 107727640A
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- sers
- cigarette
- essence spice
- essence
- differentiating
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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
Abstract
The invention discloses a kind of method for differentiating essence spice for cigarette using SERS method, and 40 60nm golden nanometer particle is first prepared for reduction of sodium citrate method, the SERS substrates of individual layer are then prepared using two phase process, are spontaneously dried, standby；The SERS chip activity of preparation is measured using 4-Mercaptopyridine molecule, it is determined that higher Raman signal can be obtained, and substrate has preferable uniformity；SERS chips are placed in essence spice for cigarette sample to be measured 12 hours, it directly detected with Raman spectrometer after removing unnecessary essence and flavoring agent；The Raman spectrum of acquisition is analyzed using PCA principal component analytical methods.The present invention is not required to carry out pre-treatment to sample, is not required to add other internal standard compound, can quickly, efficiently, nondestructively realize to the essence spice for cigarette progress quality discrimination in production, suitable for the fast on-line analyzing of batch samples.
Description
Technical field
It is more particularly to a kind of to utilize SERS method the invention belongs to essence and flavoring agent quality inspection technical field
Differentiate the method for essence spice for cigarette.
Background technology
Essence spice for cigarette is one of most important raw and auxiliary material of production of cigarettes, and cigarette process characteristic is crucial auxiliary
Material.Essence spice for cigarette quality stability is directly connected to the organoleptic quality of cigarette product.The character surveillance of essence spice for cigarette
It is divided into two stages, when commodity perfume base buying storage, second, the essence and flavoring agent in production, i.e., carry out secondary tune by commodity perfume base
Essence and flavoring agent after matching somebody with somebody is in product.At present, industry monitoring is perfume material buying storage link, for the essence and flavoring agent in production
Lack corresponding monitoring means in product, tobacco business.Presently mainly pass through some physical property such as refraction index, relative density
Index and artificial the two fragrant links are smelt to carry out character surveillance to essence spice for cigarette.The former is physical detection, can only be reflected
Go out the part of properties of complicated essence and flavoring agent system；And the latter acceptor sees consciousness, environment, individual difference etc. and had a great influence, both
Method is relatively extensive, can not characterize well in essence and flavoring agent in the minor variations of composition.That has reported at present is used to reflect
The assay method of other essence spice for cigarette is mainly mass spectrography, as reported in patent in CN106404884A and CN106248850A
With mass spectrum combination similarity analysis quality control is carried out to essence spice for cigarette.CN105891367A is also reported in the patent
Using the combination of gas-chromatography and mass spectrography quality control is carried out to it.But these method generally existing complex pretreatments,
The reason such as cumbersome is not suitable for the real-time monitoring of a large amount of samples.
The content of the invention
It is an object of the invention to provide one kind can utilize SERS method, carrys out cigarette in quick discriminating production and uses
The method of essence and flavoring agent quality.
Therefore, the technical scheme is that：It is a kind of to differentiate essence spice for cigarette using SERS method
Method, comprise the following steps：
1）The preparation of SERS chips：
40-60nm golden nanometer particle is first prepared for reduction of sodium citrate method, the SERS of individual layer is then prepared using two phase process
Substrate, spontaneously dry, it is standby；
2）SERS chip determinations of activity：
Using 4-Mercaptopyridine molecule to step 1）The SERS chip activity of preparation is measured, it is determined that higher drawing can be obtained
Graceful signal, and substrate has preferable uniformity；
3）The SERS detection of essence spice for cigarette：
SERS chips are placed in 1-2 hours in essence spice for cigarette sample to be measured, then soaked 3-4 times in ultra-pure water again, with except
The unnecessary essence and flavoring agent for going surface physics to adsorb, is drained with vacuum pump, then it is directly detected with Raman spectrometer；
4）Data process＆analysis：
The Raman spectrum of acquisition is analyzed using PCA principal component analytical methods.
Further, the step 1）The a diameter of 55nm of golden nanometer particle used in middle SERS chips.
Further, the step 3）In the SERS chips that assemble be placed in ultra-pure water and soak 3-4 times, when soaking every time
Between be 3-5min.
Further, the step 3）Middle Raman spectrum testing conditions are：785 nm laser, 1200 T gratings, 1.6 mW
Power, adopt for 10 s every time between time spectrum, accumulation adopts spectrum 3 times to each sample every time, and each sample adopts 10 points.
Further, the step 4）Analysis concretely comprises the following steps：To step 3）In multiple surface enhanceds of each sample draw
Graceful spectrogram is analyzed, and after removing exceptional value, PCA analyses is carried out to it, and then distinguish different samples.
The present invention carries out quality discrimination using SERS technology to the essence spice for cigarette in production first；
Then two-dimentional substrate is make use of to prepare the SERS substrates of this method；Most spectral technique and stechiometry PCA technology phases at last
With reference to the quality of flavoring essence for tobacco in being produced differentiates.PCA technologies are principal component analysis technology, also known as principal component analysis.
Principal component analysis is also referred to as principal component analysis, it is intended to using the thought of dimensionality reduction, multi objective is converted into a few overall target.
SERS has detection speed fast, and test limit is low, and high sensitivity can even reach unimolecule inspection
The advantages that survey, rapidly applied since its discovery among the multiple fields such as food, medicine, biology, chemistry.The present invention utilizes
SERS technology carries out quality testing discriminating to essence spice for cigarette, from the metal nanoparticle of suitable diameter
It can amplify Raman signal as detection substrate, the essence spice for cigarette in quick, lossless, real-time measure production, realize product
Quality discrimination.The present invention is not required to carry out pre-treatment to sample, is not required to add other internal standard compound, can quickly, efficiently, nondestructively
Realize and quality discrimination is carried out to the essence spice for cigarette in production, suitable for the fast on-line analyzing of batch samples.
Brief description of the drawings
It is described in further detail below in conjunction with accompanying drawing and embodiments of the present invention
The average surface that Fig. 1 is 1# and 1#-1 strengthens Raman spectrogram（a）With PCA classification charts（b）；
The average surface that Fig. 2 is 1# and 1#-2 strengthens Raman spectrogram（a）With PCA classification charts（b）.
The average surface that curve S1 is 1# in figure strengthens Raman spectrogram, and the average surface that curve S2 is 1#-1 strengthens Raman
Spectrogram, the average surface that curve S3 is 1#-2 strengthen Raman spectrogram；Point set P1 is 1# PCA classification charts, and point set P2 is 1#-
1 PCA classification charts, point set P3 are 1#-2 PCA classification charts.
Embodiment
The present invention is further described by specific examples below, but does not limit the present invention.
Embodiment：
1. instrument, reagent and instrument condition of work
1）Instrument
Confocal laser-scanning microscopy instrument（XploRA, 785 nm）
2）Reagent
Gold chloride, sodium citrate, essence and flavoring agent
3）Raman spectrum condition
The parameter of Raman spectrometer is arranged to：The XploRA of HORIBA companies, light source：785 nm；Power：1.6 mW；Scan model
Enclose：600 ~ 1500 cm-1；Grating：1200 T；Each sample adopts spectrum 10, then carries out PCA analyses with matlab softwares.
2. essence spice for cigarette sample
The sample message of essence spice for cigarette is as shown in the table.
The problem of in the simulated production of table 1 essence spice for cigarette sample
| Sequence number | Sample | Raw material A | Raw material B | Raw material C | Raw material D | Solvent propylene glycol | The ethanol of solvent 95% |
| 1 | 1#（Normal sample） | 15.0% | 20.0% | 5.0% | 20.0% | 10.0% | 30.0% |
| 2 | 1#—1（Problem sample） | 14.0% | 20.0% | 5.0% | 20.0% | 10.0% | 31.0% |
| 3 | 1#—2（Problem sample） | 14.5% | 20.0% | 5.0% | 20.0% | 10.0% | 30.5% |
The preparation of 3.SERS chips
1）First, 250 mL round-bottomed flask is taken, the water heating for adding 200 mL is boiled.It is rapidly added 1.5 mL 1% lemon
Acid sodium aqueous solution, continue to boil half an hour after solution changes color, cool down, obtain about 55nm（40-60nm）Golden nanometer particle, from
The heart, it is standby；
2）Take appropriate 1）The golden nanometer particle of middle acquisition, which is diluted with water, to be placed in small beaker, 2 ~ 3 mL hexamethylenes of addition, and formation water/
Oily two-phase interface, ethanol in proper amount is then added, wait golden nanometer particle to separate out, formed the golden film of one layer of individual layer in interface, use
Pipettor removes a large amount of hexamethylenes on golden film upper strata, is then pulled golden film to obtain SERS chips out with gold plaque；
3）The chip of acquisition is dried, it is standby.
4. sample determines
1）The SERS chips prepared are placed directly within first among the flavouring essence for tobacco feed liquid prepared, 1-2 takes out after hour；
2）Chip is placed in immersion 3-5 minutes in ultra-pure water again, repeated 3-4 times, to remove the essence feed liquid of excess surface；
3）The chip cleaned up is drained with vacuum pump, tested with burnt micro-Raman spectroscopy is copolymerized.
5. data process＆analysis
Analyze obtaining 10 SERS figures, after removing exceptional value, PCA is carried out to it with matlab softwares
Analysis, it is found that different samples can perfectly make a distinction.
As shown in Figure 1 and Figure 2, the average surface that curve S1 is 1# strengthens Raman spectrogram, and curve S2 is 1#-1 average table
Face strengthens Raman spectrogram, and the average surface that curve S3 is 1#-2 strengthens Raman spectrogram；Point set P1 is 1# PCA classification charts,
Point set P2 is 1#-1 PCA classification charts, and point set P3 is 1#-2 PCA classification charts.Thus can understand to 1#（Normal sample）、1#—1
（Problem sample）、1#—2（Problem sample）Make a distinction.
Claims (5)
- A kind of 1. method for differentiating essence spice for cigarette using SERS method, it is characterised in that：Including following step Suddenly：1）The preparation of SERS chips：40-60nm golden nanometer particle is first prepared for reduction of sodium citrate method, the SERS of individual layer is then prepared using two phase process Substrate, spontaneously dry, it is standby；2）SERS chip determinations of activity：Using 4-Mercaptopyridine molecule to step 1）The SERS chip activity of preparation is measured, it is determined that higher drawing can be obtained Graceful signal, and substrate has preferable uniformity；3）The SERS detection of essence spice for cigarette：SERS chips are placed in 1-2 hours in essence spice for cigarette sample to be measured, then soaked 3-4 times in ultra-pure water again, with except The unnecessary essence and flavoring agent for going surface physics to adsorb, is drained with vacuum pump, then it is directly detected with Raman spectrometer；4）Data process＆analysis：The Raman spectrum of acquisition is analyzed using PCA principal component analytical methods.
- 2. a kind of method for differentiating essence spice for cigarette using SERS method as claimed in claim 1, it is special Sign is：The step 1）The a diameter of 55nm of golden nanometer particle used in middle SERS chips.
- 3. a kind of method for differentiating essence spice for cigarette using SERS method as claimed in claim 1, it is special Sign is：The step 3）In the SERS chips that assemble be placed in ultra-pure water and soak 3-4 times, each soak time is 3- 5min。
- 4. a kind of method for differentiating essence spice for cigarette using SERS method as claimed in claim 1, it is special Sign is：The step 3）Middle Raman spectrum testing conditions are：785 nm laser, 1200 T gratings, 1.6 mW power, adopt time spectrum Between for 10 s every time, accumulation adopts spectrum 3 times to each sample every time, and each sample adopts 10 points.
- 5. a kind of method for differentiating essence spice for cigarette using SERS method as claimed in claim 1, it is special Sign is：The step 4）Analysis concretely comprises the following steps：To step 3）In multiple SERS figures of each sample enter Row analysis, after removing exceptional value, PCA analyses are carried out to it, and then distinguish different samples.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110146484A (en) * | 2019-05-22 | 2019-08-20 | 江苏大学 | One kind being based on Cu2The pesticide qualitative discrimination method of O/Ag SERS sensor |
| CN110161011A (en) * | 2019-06-12 | 2019-08-23 | 浙江中烟工业有限责任公司 | Rapid detection method of the Semblance to the essence spice for cigarette of the amounts of mixing different in production |
| CN110646404A (en) * | 2019-10-25 | 2020-01-03 | 陕西中烟工业有限责任公司 | Method for measuring solvent index of tobacco essence |
| CN111189815A (en) * | 2020-01-10 | 2020-05-22 | 西南交通大学 | Sewage tracing method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104730062A (en) * | 2015-04-16 | 2015-06-24 | 苏州大学 | Transparent flexible surface-enhanced Roman spectroscopy substrate (SERS) and preparation method and application thereof |
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2017
- 2017-12-08 CN CN201711296895.8A patent/CN107727640A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104730062A (en) * | 2015-04-16 | 2015-06-24 | 苏州大学 | Transparent flexible surface-enhanced Roman spectroscopy substrate (SERS) and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 夏洪坤等: "Ag/MoS2复合纳米材料对香精分子的SERS效应", 《人工晶体学报》 * |
| 翁士状等: "基于SERS与PCA-SLR实现乙基对氧磷定量检测", 《光谱学与光谱分析》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110146484A (en) * | 2019-05-22 | 2019-08-20 | 江苏大学 | One kind being based on Cu2The pesticide qualitative discrimination method of O/Ag SERS sensor |
| CN110161011A (en) * | 2019-06-12 | 2019-08-23 | 浙江中烟工业有限责任公司 | Rapid detection method of the Semblance to the essence spice for cigarette of the amounts of mixing different in production |
| CN110646404A (en) * | 2019-10-25 | 2020-01-03 | 陕西中烟工业有限责任公司 | Method for measuring solvent index of tobacco essence |
| CN111189815A (en) * | 2020-01-10 | 2020-05-22 | 西南交通大学 | Sewage tracing method |
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Application publication date: 20180223 |