CN105675785A - Method for fast gas chromatography identification of quality of tobacco flavors for invitation for bids - Google Patents
Method for fast gas chromatography identification of quality of tobacco flavors for invitation for bids Download PDFInfo
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- CN105675785A CN105675785A CN201610055021.2A CN201610055021A CN105675785A CN 105675785 A CN105675785 A CN 105675785A CN 201610055021 A CN201610055021 A CN 201610055021A CN 105675785 A CN105675785 A CN 105675785A
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Abstract
The invention discloses a method for fast gas chromatography identification of quality of tobacco flavors for invitation for bids and belongs to the technical field of flavor quality control. The method comprises steps as follows: chromatograms of a standard sample and bidding samples on two chromatographic columns are acquired by using a HERACLES II type ultra-fast gas chromatography electronic nose system; linear conversion is performed on primary data vectors with a PCA (principal component analysis) method, and one of the bidding samples, which has the minimum Mahalanobis distance with the standard sample, is judged as a bid sample. The method comprises the simple steps, is convenient to operate and capable of performing fast detection, full scanning and no blind zones are realized in sample detection, the bid sample with the quality closest to that of the standard sample can be accurately identified from the bidding samples, and the method is particularly applicable to social open bidding work for the tobacco flavors.
Description
Technical field
The invention belongs to essence and flavoring agent quality control technical field, be specifically related to a kind of fast gas chromatography for calling for bid and identify essence spice for cigarette quality method.
Background technology
Essence spice for cigarette is cigarette product " soul ", is the secret place of cigarette products style characteristic formation, and therefore, essence spice for cigarette quality control is one of critical support of cigarette product quality.
At present, essence spice for cigarette product control index includes physics class (refraction index, relative density, acid number, miscible degree, volatile material total amount), security classes (heavy metal, limit with Organic substance), cost class (solvent) and true class (property material), sense organ class (fragrance) and finger printing class (gas phase fingerprint, liquid phase fingerprint and near-infrared fingerprint) etc. index, but what these indexs had only lays particular emphasis on a certain characteristic of essence and flavoring agent, it is difficult to embody the quality overall picture of essence spice for cigarette, have with sensory evaluation for foundation, easily by subjective consciousness, environment and individual variation impact, some detection processes are loaded down with trivial details, analytical cycle is longer, it is subject to solvent and form interference. above method is difficult to meet the technical characteristic of essence spice for cigarette socialization competitive bidding work " fast, accurate, complete ", and therefore, tobacco business urgently develops the detection technique with features such as " analytical cycle are short, Identification is accurate, sample covers complete ".
Summary of the invention
Present invention aims to the deficiency of existing essence spice for cigarette product control identification technology, a kind of fast gas chromatography for calling for bid is provided to identify essence spice for cigarette quality method, can quick and precisely identify acceptance of the bid sample immediate with standard sample quality in bid sample by the method, be particularly suited for socialization's competitive bidding work of essence spice for cigarette.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of fast gas chromatography for calling for bid identifies essence spice for cigarette quality method, utilizes HERACLESII type fast gas chromatography electric nasus system that essence spice for cigarette bid sample is differentiated.
Described identifies essence spice for cigarette quality method for the fast gas chromatography called for bid, and comprises the steps:
Step (1), utilize the supper-fast gas chromatogram electric nasus system of HERACLESII type, carrying out the sample introduction of sample initially with the mode of headspace sampling, then gather and obtain standard sample and bid sample chromatogram on two root chromatogram columns, times of collection is at least 3 times;The type of two described root chromatogram columns respectively MXT-5 type chromatographic column and MXT-1701 type chromatographic column;
Step (2), adopts principal component analytical method, the original data vector of the chromatogram that step (1) obtains is carried out linear transformation, and the judgement that between bid sample and standard sample, mahalanobis distance is minimum is middle standard specimen.
It is further preferred that in step (1), described injector temperature is 150-200 DEG C, sampling volume is 10uL-5mL, sample introduction speed 50-250uL/s; The thermal oscillation temperature that adds of headspace sampling bottle is 25-100 DEG C, and heating duration of oscillation is 5-20min.
It is further preferred that in step (1), the testing sample quality in headspace sampling bottle is 0.05-0.5g.
It is further preferred that in step (1), the length of MXT-5 type chromatographic column and MXT-1701 type chromatographic column × interior through being 10m × 0.18mm.
It is further preferred that in step (1), chromatograph heating schedule is: initial temperature 35-50 DEG C keeps 1-5s, be warming up to 200-280 DEG C with 2-10 DEG C/s, keeps 10-30s, and detector temperature is 250-280 DEG C, split ratio 1:5-1:50.
Further, preferably, in step (2), the judgement of middle standard specimen: the two-dimensional gas chromatography stacking chart obtained in step (1) is carried out principal component analysis by AlphasoftV14.2 software automatically that adopt HERACLESII type supper-fast gas chromatogram electric nasus system subsidiary, then the mahalanobis distance between bid sample and standard sample is calculated, mahalanobis distance reckling is judged to acceptance of the bid sample, is sample best in quality in bid sample.
Compared with prior art, it has the beneficial effect that the present invention
(1) present invention provides a kind of fast gas chromatography towards bid first and identifies essence spice for cigarette quality method, because adopting the double; two fid detector of double; two chromatographic column, repeatedly verify through great many of experiments, obtain the combination of optimum detection parameter, when adopting the analytical parameters within the scope of this, composition separating effect is better, discrimination index high (>=88), rate of accuracy reached, to 100%, can accurately identify acceptance of the bid sample immediate with standard sample quality in bid sample.
(2) the inventive method compares with the tradition way of invitation for bid such as infrared, conventional gas phase and liquid phase fingerprint: adopt headspace sampling, it is not necessary to the pre-treatment steps such as solvent dissolving, filtration and transfer, simple to operation; Adopt the capillary chromatographic column of metal material, essence and flavoring agent sample suitable in various solvents, various viscosity, overcoming infrared method to moisture, solvent more than 98% with the sample blind area of synthetic perfume, sample detection has accomplished " full scan, non-blind area "; Adopting short and thin double; two chromatographic columns (length × interior through being 10m × 0.18mm), analytical cycle is reduced within 3min from the 60min of conventional chromatogram technology, is particularly suited for the competitive bidding work of essence spice for cigarette socialization.
Accompanying drawing explanation
Fig. 1 is 4# sample two-dimensional gas chromatography stacking chart in MXT-5 type chromatographic column;
Fig. 2 is 4# sample two-dimensional gas chromatography stacking chart in MXT-1701 type chromatographic column;
Fig. 3 is 7# sample two-dimensional gas chromatography stacking chart in MXT-5 type chromatographic column;
Fig. 4 is 7# sample two-dimensional gas chromatography stacking chart in MXT-1701 type chromatographic column;
Fig. 5 is the principal component analysis scatterplot of 4# sample;
Fig. 6 is the principal component analysis scatterplot of 7# sample;
Fig. 7 is the principal component analysis scatterplot of 10# sample;
Fig. 8 is the principal component analysis scatterplot of 28# sample;
Fig. 9 is the principal component analysis scatterplot of 49# sample;
Figure 10 is the principal component analysis scatterplot of 70# sample;
Figure 11 is the principal component analysis scatterplot of 81# sample;
Figure 12 is the principal component analysis scatterplot of 83# sample;
Figure 13 is the principal component analysis scatterplot of 1975# sample;
Figure 14 is the principal component analysis scatterplot of 9527# sample.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention. Unreceipted concrete technology or condition person in embodiment, technology or condition described by the document in this area or carry out according to product description. Agents useful for same or the unreceipted production firm person of instrument, be and can pass through to buy the conventional products obtained.
Material required for the present invention and instrument:
HERACLESII fast gas chromatography Electronic Nose (ALPHAMOS company of France, the double; two chromatographic column of MXT-5 and MXT-1701, length and interior through being 10m × 0.18mm; Electronic balance (prunus mume (sieb.) sieb.et zucc. Teller-Tuo benefit, ME204); Headspace sampling bottle (10mL).
Embodiment 1
A kind of fast gas chromatography for calling for bid identifies essence spice for cigarette quality method, comprises the steps:
Step (1), utilize the supper-fast gas chromatogram electric nasus system of HERACLESII type, with standard sample and bid sample for testing sample, adopt headspace gas input mode to carry out sample introduction, gather respectively and obtain standard sample, bid sample chromatogram on two root chromatogram columns; The type of two described root chromatogram columns respectively MXT-5 type chromatographic column and MXT-1701 type chromatographic column;
Wherein, injector temperature is 150 DEG C, and sampling volume is 5mL, sample introduction speed 50uL/s; The thermal oscillation temperature that adds of headspace sampling bottle is 25 DEG C, and heating duration of oscillation is 20min. Testing sample quality in headspace sampling bottle is 0.5g.
Chromatograph heating schedule is: initial temperature 50 DEG C keeps 3s, is warming up to 280 DEG C with 5 DEG C/s, keeps 18s, and detector temperature is 260 DEG C, split ratio 1:5.
Step (2), adopts principal component analysis (PCA) method, the original data vector of the chromatogram that step (1) obtains is carried out linear transformation, and the judgement that between bid sample and standard sample, mahalanobis distance is minimum is middle standard specimen.
Embodiment 2
A kind of fast gas chromatography for calling for bid identifies essence spice for cigarette quality method, comprises the steps:
Step (1), utilize the supper-fast gas chromatogram electric nasus system of HERACLESII type, with standard sample and bid sample for testing sample, adopt headspace gas input mode to carry out sample introduction, gather respectively and obtain standard sample, bid sample chromatogram on two root chromatogram columns; The type of two described root chromatogram columns respectively MXT-5 type chromatographic column and MXT-1701 type chromatographic column;
Wherein, injector temperature is 180 DEG C, and sampling volume is 10uL, sample introduction speed 250uL/s; The thermal oscillation temperature that adds to headspace sampling bottle is 100 DEG C, and heating duration of oscillation is 5min. Testing sample quality in headspace sampling bottle is 0.05g.
Chromatograph heating schedule is: initial temperature 50 DEG C keeps 1s, is warming up to 200 DEG C with 10 DEG C/s, keeps 10s, and detector temperature is 250 DEG C, split ratio 1:50.
Step (2), adopts principal component analysis (PCA) method, the original data vector of the chromatogram that step (1) obtains is carried out linear transformation, and the judgement that between bid sample and standard sample, mahalanobis distance is minimum is middle standard specimen.
Embodiment 3
A kind of fast gas chromatography for calling for bid identifies essence spice for cigarette quality method, comprises the steps:
Step (1), the collection of chromatogram: for the good essence spice for cigarette bid sample of clarification and volatility (such as 4#, 10#, 49#, 70#, 83#, 1975# and 9527# etc.), accurately weigh (being accurate to arithmetic point the 4th) 0.1 gram with electronic balance and join 10mL headspace sampling bottle, seal, put into automatic headspace sampling dish, heating duration of oscillation is 10min, adding thermal oscillation temperature is 40 DEG C, sampling volume 500uL, sample introduction speed 125uL/s, injector temperature 200 DEG C, detector temperature 280 DEG C, initial temperature 40 DEG C keeps 5s, it is warming up to 260 DEG C with 2 DEG C/s, keep 30s, split ratio 1:10, utilize this head space and chromatograph intensification parameter, gather standard sample and bid sample chromatogram on two root chromatogram columns, as 4 sample one-time detection such as standard that Fig. 1 and Fig. 2 is 4# sample and bid obtain two-dimensional gas chromatography stacking chart, at least repeat 3 times, and for bad essence spice for cigarette bid sample (such as 7#, 28# and 81#) of thickness or solid kind and volatility, except heating duration of oscillation becomes 15min, add thermal oscillation temperature 70 C, sampling volume 5000uL, outside sample introduction speed 500uL/s, all the other conditions remain unchanged, same collection standard and bid sample chromatogram on two root chromatogram columns, such as the two-dimensional gas chromatography stacking chart that 4 sample one-time detection such as standard that Fig. 3 and Fig. 4 is 7# sample and bid obtain, at least repeat 3 times.
10 kinds of essence spice for cigarette bid sample messages are shown in Table 1.
Step (2), the judgement of middle standard specimen: the chromatogram that obtains in step (1) is carried out principal component analysis (PCA) by AlphasoftV14.2 software automatically that adopt this instrument subsidiary, its scatterplot is shown in Fig. 5-Figure 14, then the mahalanobis distance between bid sample and standard sample is calculated, it is shown in Table 2, often in group sample, mahalanobis distance reckling is judged to acceptance of the bid sample, discrimination index high (>=88), rate of accuracy reached is to 100%, identification effect is very good, and it is suitable for the essence spice for cigarette of all kinds (solvent and mode of appearance etc.), sample detection has accomplished " full scan, non-blind area ", analysis time completes within 3min, this is the advantage that other quick analytical technology cannot possess at present, it is particularly suited for socialization's competitive bidding work of essence spice for cigarette.
Table 1 essence spice for cigarette sample message table
The acceptance of the bid sample critical table of table 2 essence spice for cigarette
The ultimate principle of the present invention, principal character and advantages of the present invention have more than been shown and described. Skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; described in above-described embodiment and description is that principles of the invention is described; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements both fall within the claimed scope of the invention. Claimed scope is defined by appending claims and equivalent thereof.
Claims (7)
1. identify essence spice for cigarette quality method for the fast gas chromatography called for bid for one kind, it is characterised in that: utilize HERACLESII type fast gas chromatography electric nasus system that essence spice for cigarette bid sample is differentiated.
2. the fast gas chromatography for calling for bid as claimed in claim 1 identifies essence spice for cigarette quality method, it is characterised in that comprise the steps:
Step (1), utilize the supper-fast gas chromatogram electric nasus system of HERACLESII type, carrying out the sample introduction of sample initially with the mode of headspace sampling, then gather and obtain standard sample and bid sample chromatogram on two root chromatogram columns, times of collection is at least 3 times;The type of two described root chromatogram columns respectively MXT-5 type chromatographic column and MXT-1701 type chromatographic column;
Step (2), adopts principal component analytical method, the original data vector of the chromatogram that step (1) obtains is carried out linear transformation, and the judgement that between bid sample and standard sample, mahalanobis distance is minimum is middle standard specimen.
3. the fast gas chromatography for calling for bid according to claim 2 identifies essence spice for cigarette quality method, it is characterised in that: in step (1), described injector temperature is 150-200 DEG C, and sampling volume is 10uL-5mL, sample introduction speed 50-250uL/s; The thermal oscillation temperature that adds of headspace sampling bottle is 25-100 DEG C, and heating duration of oscillation is 5-20min.
4. the fast gas chromatography for calling for bid according to claim 2 identifies essence spice for cigarette quality method, it is characterised in that: in step (1), the testing sample quality in headspace sampling bottle is 0.05-0.5g.
5. the fast gas chromatography for calling for bid according to claim 2 identifies essence spice for cigarette quality method, it is characterised in that: in step (1), the length of MXT-5 type chromatographic column and MXT-1701 type chromatographic column × interior through being 10m × 0.18mm.
6. the fast gas chromatography for calling for bid according to claim 2 identifies essence spice for cigarette quality method, it is characterized in that: in step (1), chromatograph heating schedule is: initial temperature 35-50 DEG C keeps 1-5s, it is warming up to 200-280 DEG C with 2-10 DEG C/s, keep 10-30s, detector temperature is 250-280 DEG C, split ratio 1:5-1:50.
7. the fast gas chromatography for calling for bid according to claim 2 identifies essence spice for cigarette quality method, it is characterized in that: in step (2), the judgement of middle standard specimen: the two-dimensional gas chromatography stacking chart obtained in step (1) is carried out principal component analysis by AlphasoftV14.2 software automatically that adopt HERACLESII type supper-fast gas chromatogram electric nasus system subsidiary, then the mahalanobis distance between bid sample and standard sample is calculated, mahalanobis distance reckling is judged to acceptance of the bid sample, is sample best in quality in bid sample.
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| CN106404884A (en) * | 2016-11-22 | 2017-02-15 | 云南中烟工业有限责任公司 | Method for quickly evaluating quality consistency of flavors and fragrances of volatile cigarettes by HS-IMR-MS |
| CN109655530A (en) * | 2017-10-12 | 2019-04-19 | 贵州中烟工业有限责任公司 | A method of identifying flavors and fragrances quality difference |
| CN110659700A (en) * | 2019-10-10 | 2020-01-07 | 西南石油大学 | KNN-based image sample generation method |
| CN112345654A (en) * | 2019-08-06 | 2021-02-09 | 红塔烟草(集团)有限责任公司 | Method for identifying oil stain smoke pollution source based on chromatographic fingerprint spectrum |
| CN113049436A (en) * | 2021-02-08 | 2021-06-29 | 广东中烟工业有限责任公司 | Method for rapidly analyzing consistency of tobacco flavor and fragrance and application thereof |
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| CN110659700A (en) * | 2019-10-10 | 2020-01-07 | 西南石油大学 | KNN-based image sample generation method |
| CN113049436A (en) * | 2021-02-08 | 2021-06-29 | 广东中烟工业有限责任公司 | Method for rapidly analyzing consistency of tobacco flavor and fragrance and application thereof |
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Application publication date: 20160615 |