CN102928356A - Method for measuring essence solvent content rapidly - Google Patents
Method for measuring essence solvent content rapidly Download PDFInfo
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- CN102928356A CN102928356A CN2012104327600A CN201210432760A CN102928356A CN 102928356 A CN102928356 A CN 102928356A CN 2012104327600 A CN2012104327600 A CN 2012104327600A CN 201210432760 A CN201210432760 A CN 201210432760A CN 102928356 A CN102928356 A CN 102928356A
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Abstract
The invention provides a method for measuring essence solvent content rapidly. The method is characterized in that the Fourier transform near-infrared spectrum technology is used for building a prediction model of essence solvent content so as to perform rapid measurement of the solvent content. The method includes the following steps: 1) solvent standard solutions of series concentrations are prepared; 2) the near-infrared transmitted spectrum of the standard solutions is acquired; 3) the actual concentrations of the solvent standard solutions and the transmitted spectrum are fit to form the prediction model of the solvent content; 4) the transmitted spectrum of an essence sample to be tested is obtained according to acquisition parameters of the step 2); and 5) the transmitted spectrum of the essence sample to be tested is compared with the built prediction model to obtain the solvent content of the essence sample. The method for measuring the essence solvent content rapidly has the following advantages: the sample does not need to be diluted and preprocessed, on-line detection can be performed, detection speed is rapid, one sample only needs 1-2 minutes, content of various solvents in the sample can be detected simultaneously, detection sensitivity is high, repeatability is high, instrument operation is simple, and the test method is suitable for popularization.
Description
Technical field
The present invention relates to essence quality testing field, specifically relate to a kind of method of Fast Measurement essence solvent.The method is to utilize Fourier transform-near-infrared spectrum technique to set up the forecast model of essence solvent, thereby carries out the Fast Measurement of solvent.
Background technology
Essence is according to certain ratio and technique with multiple spices and solvent, the spice mixt with certain odor type that obtains through artificial allotment, because form complexity, product is subject to the impact of the many factors such as raw material and processing technology, it is extremely important that it is carried out strict quality control.
The composition of content maximum is various solvents in the essence, so solvent composition is essence product stability and one of qualified important symbol whether.In the existing essence standard, mainly be by the quality after the evaporation of test essence product solvent, calculate quantity of solvent (universal test methods of YC/T 145.9 Volatile Components in Tobacco Flavor total amounts).Yet this method can only be tested the solvent total amount, and can't reflect the composition situation of various solvents in the product.Present karl Fischer method (Li Haiyan, Tang Danyu, Xiao Yan etc. the fast look of karl Fischer method is measured the moisture in the flavouring essence for tobacco. the Agriculture of Anhui science, 2009,37(20): 9332-9333), vapor-phase chromatography (Soviet Union's state year. the improvement of the gas chromatography analysis method of solvent in the flavouring essence for tobacco. tobacco science and technology, 2002(6): 27-31) be used to the direct-detection of variety classes solvent in the essence.But the karl Fischer method is just for the detection of moisture, although and vapor-phase chromatography can detect the various solvents in the essence simultaneously, need to carry out certain dilution or pre-treatment to sample, and having relatively high expectations to the testing staff.
Near infrared spectrum mainly is that the anharmonicity by molecular vibration produces when making molecular vibration from ground state to the high level transition, and mainly by C-H, O-H, S-O, the sum of fundamental frequencies of the groups such as N-H and C=O absorb to absorb with frequency multiplication and form molecule in the absorption in NIR district.Different groups or near infrared absorption wavelength and the intensity of same group in the different chemical environment have significant difference, so near infrared spectrum has abundant structure and composition information, be fit to the Analysis of Complex system, can realize quick, the non-destructive on-line analysis of sample.
Summary of the invention
Purpose of the present invention just is being based on above-mentioned prior art situation and a kind of quick nondestructive that provides is measured the method for essence solvent, thereby realizes real-time control and the on-line analysis of essence production and application.This method utilizes Fourier transform near infrared spectrometry to set up essence solvent forecast model, and sample need not pre-service, and is easy and simple to handle, and weak point consuming time can be predicted multi-solvents content simultaneously, and prediction effect is desirable.
Purpose of the present invention can realize by following technique measures: utilize Fourier transform-near-infrared spectrum technique to set up the forecast model of essence solvent, thereby carry out the Fast Measurement of solvent, concrete steps are as follows:
(1) the solvent standard solution of preparation series concentration;
(2) utilize Fourier transform-near infrared spectrometer to gather the near-infrared transmission spectrum of solvent standard solution;
(3) transmitted spectrum and its actual concentrations with the solvent standard solution carries out match, forms the near infrared forecast model of solvent;
(4) obtain the transmitted spectrum of essence sample to be measured according to the acquisition parameter of step (2);
(5) transmitted spectrum of essence sample to be measured is compared with the forecast model of having set up, obtain the solvent of essence sample.
The standard solution of solvent described in the step of the present invention (1) be the essence solvents such as water, ethanol and propylene glycol in one or more potpourri.
Spectra collection described in the step of the present invention (2) (3) (4) (5), spectral manipulation, data fitting, content prediction adopt near infrared spectrometer and its corresponding analysis software to carry out.
The acquisition parameter of standard solution transmitted spectrum is described in the step of the present invention (2): gather wave-number range 10000～4000cm
-1, fixing light path, take the built-in background of instrument as reference, sample and reference all use 16～64 scanning, resolution 2～10cm
-1
Transmitted spectrum described in the step of the present invention (3) is original spectrum or spectrum after pretreatment, and preprocessing procedures is respectively the combination of one or more methods in first order derivative, second derivative, Savitzk-Golay filtering, the filtering of Norris derivative, the baseline correction.
Approximating method described in the step of the present invention (3) is a kind of in partial least squares regression, multiple linear regression, the principal component analysis (PCA).
The present invention compares with existing solvent detection method and has the following advantages: sample need not dilution, need not pre-service, can detect online; Detection speed is fast, and a sample only needs 1～2 minute; The content of multi-solvents in the test sample simultaneously; Detection sensitivity is high, good reproducibility; Instrumentation is simple, and method of testing is fit to popularize and promote.
Description of drawings
Figure
: the correlogram of forecast model solvent predicted value and actual value (A-water, B-ethanol, C-propylene glycol)
Embodiment
The present invention is described in further detail below with reference to embodiment, but does not limit the present invention.
The water-ethanol of preparation different quality concentration-propylene glycol standard mixed solution, the mass concentration of each component is as shown in table 1 in the solution.Gather its near infrared spectrum, gather wave-number range 10000～4000cm
-1, fixing light path, take the built-in background of instrument as reference, sample and reference all use 32 scanning, resolution 4cm
-1Spectrum is carried out baseline correction and second derivative process, actual concentrations and the spectroscopic data of each component carried out the partial least squares regression match, set up the solvent forecast model.
Table
The composition of water-ethanol-propylene glycol standard mixed solution (quality/%)
| Numbering | Water | Ethanol | Propylene glycol | Numbering | Water | Ethanol | Propylene glycol | |
| 1 | 0 | 0 | 100 | 9 | 25 | 75 | 0 | |
| 2 | 0 | 25 | 75 | 10 | 50 | 0 | 50 | |
| 3 | 0 | 50 | 50 | 11 | 50 | 25 | 25 | |
| 4 | 0 | 75 | 25 | 12 | 50 | 50 | 0 | |
| 5 | 0 | 100 | 0 | 13 | 75 | 0 | 25 | |
| 6 | 25 | 0 | 75 | 14 | 75 | 25 | 0 | |
| 7 | 25 | 25 | 50 | 15 | 100 | 0 | 0 | |
| 8 | 25 | 50 | 25 |
As shown in Figure 1, build that predicted value and actual value have good correlativity in the solvent model.
Optional six kinds of essence samples adopt the parameter identical with modeling sample to scan, and gather near infrared spectrum, utilize the solvent forecast model of having set up that its solvent is predicted, simultaneously the actual content of each sample solvent are detected and are contrasted.As shown in table 2, model has good prediction effect.
Utilize the solvent forecast model set up that a kind of essence sample is wherein taken multiple measurements respectively, investigate near-infrared method prediction repeatability.As shown in table 3, model has good prediction repeatability.
Table 3 model is to the prediction repeatability of essence sample solvent content
| The prediction number of times | Water | Ethanol | Propylene glycol |
| 1 | 52.99 | 2.44 | 24.28 |
| 2 | 51.61 | 2.15 | 24.93 |
| 3 | 52.21 | 2.11 | 24.71 |
| 4 | 49.89 | 2.23 | 23.54 |
| 5 | 52.94 | 2.20 | 23.74 |
| Mean value | 51.93 | 2.23 | 24.24 |
| Standard deviation | 1.27 | 0.13 | 0.60 |
| RSD/% | 2.45 | 5.66 | 2.47 |
Claims (6)
1. the method for a Fast Measurement essence solvent, it is characterized in that: the method is to utilize Fourier transform-near-infrared spectrum technique to set up the forecast model of essence solvent, thereby carries out the Fast Measurement of solvent, and concrete steps are as follows:
(1) the solvent standard solution of preparation series concentration;
(2) utilize Fourier transform-near infrared spectrometer to gather the near-infrared transmission spectrum of solvent standard solution;
(3) transmitted spectrum and its actual concentrations with the solvent standard solution carries out match, forms the near infrared forecast model of solvent;
(4) obtain the transmitted spectrum of essence sample to be measured according to the acquisition parameter of step (2);
(5) transmitted spectrum of essence sample to be measured is compared with the forecast model of having set up, obtain the solvent of essence sample.
2. the method for Fast Measurement essence solvent according to claim 1 is characterized in that: the standard solution of solvent described in the step (1) be the essence solvents such as water, ethanol and propylene glycol in one or more potpourri.
3. the method for Fast Measurement essence solvent according to claim 1 is characterized in that: spectra collection described in the step (2) (3) (4) (5), spectral manipulation, data fitting, content prediction adopt near infrared spectrometer and its corresponding analysis software to carry out.
4. the method for Fast Measurement essence solvent according to claim 1, it is characterized in that: the acquisition parameter of standard solution transmitted spectrum is described in the step (2): gather wave-number range 10000～4000cm
-1, fixing light path, take the built-in background of instrument as reference, sample and reference all use 16～64 scanning, resolution 2～10cm
-1
5. the method for Fast Measurement essence solvent according to claim 1, it is characterized in that: transmitted spectrum described in the step (3) is original spectrum or spectrum after pretreatment, and preprocessing procedures is respectively the combination of one or more methods in first order derivative, second derivative, Savitzk-Golay filtering, the filtering of Norris derivative, the baseline correction.
6. the method for Fast Measurement essence solvent according to claim 1 is characterized in that: the approximating method described in the step (3) is a kind of in partial least squares regression, multiple linear regression, the principal component analysis (PCA).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103698281A (en) * | 2013-12-31 | 2014-04-02 | 四川新绿色药业科技发展股份有限公司 | Fructus psoraleae and near-infrared diffuse reflection measurement method of fructus psoraleae derivative |
| CN108387548A (en) * | 2018-05-24 | 2018-08-10 | 东北农业大学 | A method of sweetener is quickly detected based on infrared spectrum technology |
| CN110646324A (en) * | 2019-10-25 | 2020-01-03 | 陕西中烟工业有限责任公司 | Method for measuring relative density of tobacco essence and flavor |
| CN111272696A (en) * | 2020-03-24 | 2020-06-12 | 山东大学 | Method for rapidly detecting essence doped in Pu' er tea |
| CN112345486A (en) * | 2019-08-08 | 2021-02-09 | 湖南中烟工业有限责任公司 | Method for judging solvent used by monomer perfume raw material solution based on near infrared spectrum technology |
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| CN103698281A (en) * | 2013-12-31 | 2014-04-02 | 四川新绿色药业科技发展股份有限公司 | Fructus psoraleae and near-infrared diffuse reflection measurement method of fructus psoraleae derivative |
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| CN112345486A (en) * | 2019-08-08 | 2021-02-09 | 湖南中烟工业有限责任公司 | Method for judging solvent used by monomer perfume raw material solution based on near infrared spectrum technology |
| CN112345486B (en) * | 2019-08-08 | 2022-06-14 | 湖南中烟工业有限责任公司 | Method for judging solvent used by monomer perfume raw material solution based on near infrared spectrum technology |
| CN110646324A (en) * | 2019-10-25 | 2020-01-03 | 陕西中烟工业有限责任公司 | Method for measuring relative density of tobacco essence and flavor |
| CN111272696A (en) * | 2020-03-24 | 2020-06-12 | 山东大学 | Method for rapidly detecting essence doped in Pu' er tea |
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Application publication date: 20130213 |