CN101093216B - Method for preprocessing gas chromatographic analyzed sample of feeding liquid for tobacco - Google Patents
Method for preprocessing gas chromatographic analyzed sample of feeding liquid for tobacco Download PDFInfo
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Abstract
A method for pre-treating gas-phase chromatograph analysis-sample of feed liquid used for preparing cigarette applies primary balance-extraction operation to extract out compositions required by gas-phase chromatograph analysis and contained in sample of feed liquid used for preparing cigarette.
Description
Technical field
The present invention relates to the science monitoring of cigarette materials liquid product inherent quality, specifically the cigarette gas chromatographic analysis sample pretreating method of feed liquid.
Background technology
In order to carry out science monitoring to cigarette materials liquid product inherent quality, solve cigarette enterprise to cigarette " as can be known, controlled " ability with material liquid component, people have carried out research (the document 1. Chinese tobacco association industry Professional Committee tobacco chemistry group work report of cigarette with the gas chromatographic analysis sample pretreating method of feed liquid, Zhang Hong, 2005.11.30).
The cigarette feed liquid is formulated by multiple monomer essence and flavoring agent and auxiliary material, the distribution of its chemical composition is very extensive, comprise from alcohol, aldehyde, ketone, the ester of volatility, half volatile and wait until non-volatile high boiling sugar, terpenoid etc., therefore volatility and semi-volatility component wherein can not directly carry out gas chromatographic analysis, must carry out pre-service to sample, then the component that extracts is analyzed (document 2. " essence and spices ", Sun Baoguo, Zheng Fuping, Liu Yu flat sennit work, Sinopec publishing house, 2000.11; Document 3. " synthetic perfume technical manual ", Liu Shuwen writes, China Light Industry Press, 2000.7; Document 4. " tobacco industry handbook, Huang Jia chief editor, China Light Industry Press, Guangdong Economic publishing house, 1999.4).
At present do not see that with volatility in the feed liquid and semi-volatility component bibliographical information is arranged with the gas chromatographic analysis cigarette, and flavouring essence for tobacco, the gas chromatographic analysis sample of volatility and semi-volatility component in the spices, the general steam distillation that adopts earlier, organic solvent extraction, the while distillation extraction, static headspace analysis technology, supercritical fluid technique, methods such as solid-phase microextraction are carried out pre-service (document 5.Steinhart H, Stephan A, Bucking M.Advances in flavour research[J] .J.High ResolutChromatogr, 2000,23 (7-8): 489-496. document 6.Chialva F, Gabrig G, Liddle P, et al.Application of the method comparison with the traditionanalysis of essential oils[J] .J.High Resolut Chromatogr, 1982,5 (4): 182-188.), they respectively have the relative merits of oneself.
The steam distillation method is simple to operate, but gained reappearance is relatively poor relatively as a result, be not suitable for quantitative test.
Though the organic solvent extracting access method can be by the repeatedly bigger enrichment of extraction acquisition, trivial operations, error is big, easily pollutes.For containing the cigarette feed liquid that component is many, chemical property difference is big, because the partition factor difference of each component is big, all components that need analyze are difficult to reach simultaneously the purpose of high-recovery, and therefore, cigarette should not adopt the method for general organic solvent extraction with feed liquid.
Static headspace analysis need not solvent extraction, and is little to the chromatographic column injury, but static headspace analysis only is applicable to more lower boiling component analysis, is inappropriate for the cigarette feed liquid that contains a large amount of half volatile components.
Supercritical fluid technique is a technology that has development potentiality, its nontoxic, harmless, noresidue, and operating temperature is low, and hydrolysis, oxidation, esterification or thermal distortion do not take place in extract; But its shortcoming is with high content of technology, and poor operability should not be promoted.
When solid-phase microextraction is used for the essence and flavoring agent constituent analysis, have easy and simple to handle, highly sensitive, qualitative satisfactory for result, do not use advantages such as solvent and sample detection non-destructive, because biphase equilibrium is inaccessible, therefore accurately also having certain problem in the quantitative test.
Generally speaking, cigarette adopts the while distillation extraction can obtain very high enrichment with feed liquid, and water miscible component ethanol, propylene glycol extraction quantity are seldom; But distillation extraction and back step extract is concentrated simultaneously, and not only step is many, consuming time, and the error that operation may cause is big, and the chance of pollution is also many.
Summary of the invention
The object of the present invention is to provide the gas chromatographic analysis sample pretreating method of a kind of simple to operate, cigarette that error is little with feed liquid.
For achieving the above object, the technical solution used in the present invention is:
Cigarette adopts the once balance extracting operation to extract the component that cigarette needs with gas chromatographic analysis in the feed liquid sample with the gas chromatographic analysis sample pretreating method of feed liquid.
Concrete operations can be:
For desolventize with propylene glycol outside, the cigarette feed liquid that volatility and half volatile organic component content are little, the once balance extraction solution that is adopted consists of, dichloromethane solution mL: cigarette feed liquid g: saturated common salt aqueous solution ml=1: 5: 3;
For desolventize with propylene glycol outside, the cigarette feed liquid that volatility and half volatile organic component content are big, the once balance extraction solution that is adopted consists of, dichloromethane solution mL: cigarette feed liquid g: saturated common salt aqueous solution ml=1: 1: 3;
Wherein containing internal standard compound phenylacetate, n-octyl alcohol or n-nonyl alcohol concentration in the dichloromethane solution is 1.0mg/ml; Stir centrifugally, take off layer dichloromethane solution and carry out gas chromatographic analysis.
Can carry out as follows with the definite of feed liquid volatility and half volatile organic component content size for cigarette:
With dichloromethane solution mL: cigarette feed liquid g: saturated common salt aqueous solution ml=1: 1: 3 condition once balance extraction, in analytical conditions for gas chromatography: chromatographic column HP-5 50m * 0.20mm * 0.33 μ m; Injector: 280 ℃; Detecting device: 280 ℃; Pressure: 403kpa before the post; Carrier gas: He; Linear speed: constant current 40cm/s; Sample size: 1 μ L; Split ratio: 15: 1; Column temperature: 80 ℃, 10min-5 ℃/min-250 ℃-10 ℃/min-320 ℃, 25min;
Desolventize outer chromatographic peak area in the extract less than 104pAs; Be defined as the little cigarette feed liquid of volatility and half volatile organic component content; Desolventize outer chromatographic peak area in the extract greater than 104pAs, be defined as the big cigarette feed liquid of volatility and half volatile organic component content.
Described stirring can be vortex or fierce concussion; After centrifugal, because water has a large amount of propylene glycol and ethanol, salt supersaturation is sometimes separated out, so white salt crystal can appear in dichloromethane solution lower floor, should note not taking out crystal during sampling.
The present invention has following advantage:
The present invention has carried out once balance extraction and distillation extraction, the repeatedly comparison of the concentrated three kinds of different preprocess methods of extraction simultaneously to the typical cigarette of several compositions with feed liquid.Comparing result: the gas chromatogram of the sample that three kinds of preprocess methods obtain is basic identical, and therefore, the sample that the once balance extraction is handled can embody the globality and the characteristic of volatility and half volatile chemical composition in the smoke materials liquid substantially.
Because the once balance extracting operation is simple: have only sampling, vortex (or fierce concussion), centrifugal; The error main source only is the error of cigarette with feed liquid, solvent, water and internal standard compound dosage, so error is little, and the chance of pollution is few; These characteristics are analyzed particularly important to cigarette with the microcomponent in the feed liquid.With other several preprocess methods relatively, the once balance extracting operation that cigarette is adopted with the feed liquid pre-service is workable, have extensive applicability and good extendability.
Description of drawings
Fig. 1-1,1-2 are 7
#Cigarette adopts different preprocess method gas chromatographies to separate the spectrogram contrast with feed liquid,
Last figure: repeatedly extraction concentrates, and cocnentration factor is 25 times;
Middle figure: the once balance extraction, cocnentration factor is 5 times;
Figure below: the while distillation extraction, cocnentration factor is 10 times.
Fig. 2-1,2-2 are 3
#Cigarette adopts different preprocess method gas chromatogram contrasts with feed liquid, (mark peak in wherein Figure 15 .3 is divided into)
Last figure: repeatedly extraction concentrates, and cocnentration factor is 25 times;
Middle figure: the while distillation extraction, cocnentration factor is 5 times;
Figure below: the once balance extraction, cocnentration factor is 5 times.
Fig. 3-1,3-2 are 10
#Cigarette adopts different preprocess method gas chromatogram contrasts with feed liquid,
Last figure: repeatedly extraction concentrates, and cocnentration factor is 10 times;
Middle figure: the while distillation extraction, cocnentration factor is 5 times;
Figure below: the once balance extraction, cocnentration factor is 1 times.
Fig. 4 is 10
#The test findings of feed liquid retention time repeatability;
Fig. 5 is 10
#The test findings of each concentration of component repeatability of feed liquid;
Fig. 6 is 14
#The test findings of feed liquid retention time repeatability;
Fig. 7 is 14
#The test findings of each concentration of component repeatability of feed liquid;
Fig. 8 is 15
#The test findings of feed liquid retention time repeatability;
Fig. 9 is 15
#The test findings of each concentration of component repeatability of feed liquid.
Embodiment
The present invention recommends to adopt the once balance extraction to cigarette with the feed liquid pre-service.The mechanism of liquid liquid once balance extraction is identical with static headspace analysis, all is under stationary temperature, pressure condition, and component reaches balance in two alternate distribution.Because during balance, the partition factor k value of two phase components only is the function of temperature and pressure volumes such as (, People's Education Publishing House, 1961.8) physical chemistry teaching and research groups of document 7. " physical chemistry " Nanjing University.When cigarette form to be determined with feed liquid, in two alternate distribution with form also and just determine, so the sample that the extraction of liquid liquid once balance is extracted is identical with static headspace analysis as relative quantification, is rational equally.As a kind of preprocess method, key issue is: 1) can the once balance extraction extract the component that needs; 2) whether the component of Ti Quing reaches the detection sensitivity that analytical approach needs, 3) whether the once balance extracting process repeats stablizes, and these several respects can be by the go forward side by side repeated experiment acquisition conclusion of row method of the gas chromatogram of more different preprocess methods.
Cigarette feed liquid gas chromatographic analysis sample, it is as follows to adopt the once balance extraction to carry out pretreated concrete operations:
The preparation of 1-1 inner mark solution
Precision takes by weighing standard specimen (composition according to feed liquid can be selected phenylacetate, n-octyl alcohol or n-nonyl alcohol respectively) 1.0g, is the inner mark solution of 1.0mg/ml with heavily steaming methylene chloride (analyzing pure) compound concentration.
The 1-2 cigarette extracts preprocess method with feed liquid sample once balance
Because it is big that cigarette is formed difference with feed liquid, according to its composition cigarette is divided into two classes with the feed liquid preprocess method:
(1) for desolventize with propylene glycol outside, (natural essence in the feed liquid, flavour content are relatively large with feed liquid for the little cigarette of volatility and half volatile organic component content, compound essence, flavour content are less relatively), adopt methylene chloride (mL): cigarette feed liquid (g): water (ml)=1: 5: 3, concrete operations are as follows:
Precision takes by weighing cigarette feed liquid 15g, put in the 50ml conical centrifuge tube, the 1.0mg/ml inner mark solution and the 9ml saturated common salt aqueous solution (preparation of millipore water) that add 3ml with liquid-transfering gun respectively, vortex (or fierce concussion) 1min, centrifugal 5min (3000r/min) takes off layer dichloromethane solution and carries out gas chromatographic analysis.
(2) for desolventize with propylene glycol outside, (natural essence in the feed liquid, flavour content are relative less with feed liquid for the big cigarette of volatility and half volatile organic component content, compound essence, flavour content are relatively large), adopt methylene chloride (mL): cigarette is with feed liquid (g): water (ml)=1: 1: 3; Concrete operations are as follows:
Precision takes by weighing cigarette feed liquid 5g, put in the 50ml conical centrifuge tube, add the 5ml1.0mg/ml inner mark solution respectively, 15ml saturated common salt aqueous solution (preparation of millipore water) with liquid-transfering gun, centrifugal 5min (3000r/min) behind the vortex 1min takes off layer dichloromethane solution and carries out gas chromatographic analysis.
After centrifugal, because water has a large amount of propylene glycol and ethanol, salt supersaturation is sometimes separated out, so white salt crystal can appear in dichloromethane solution lower floor, should note not taking out crystal during sampling.
The 1-3 cigarette repeatedly extracts preprocess method with the feed liquid sample
Once balance extraction handled adopt methylene chloride (mL): cigarette is with feed liquid (g): the sample of water (ml)=1: 5: 3, when repeatedly extracting, get the 25g feed liquid and add the 15mL saturated aqueous common salt, use the 5ml dichloromethane extraction more respectively three times, combining extraction liquid, rotary evaporation is concentrated into about 1ml.
Once balance extraction handled adopt methylene chloride (mL): cigarette is with feed liquid (g): the sample of water (ml)=1: 1: 3, when repeatedly extracting, get the 5g feed liquid and add the 15mL saturated aqueous common salt, use the 5ml dichloromethane extraction more respectively three times, combining extraction liquid, rotary evaporation is concentrated into 1～0.5ml.
1-4 cigarette feed liquid sample distillation extraction preprocess method simultaneously
The 5g feed liquid is added in the 400ml milipore water, carried out the while distillation extraction 2 hours, shift extract, be concentrated into 1～0.5ml to rotary evaporator with the 50ml methylene chloride.
The comparison of the different preprocess methods of feed liquid of embodiment 2. several typical cigarettes
The sample analysis condition that different preprocess methods extract is as follows:
Chromatograph: Agilent 6890N gas chromatograph
Data acquisition system (DAS): Hewlett-Packard's chem workstation
Analytical conditions for gas chromatography:
Chromatographic column HP-5 50m * 0.20mm * 0.33 μ m (Agilent Technologies, USA)
Injector: 280 ℃; Detecting device: 280 ℃; Pressure: 403kpa before the post; Carrier gas: He;
Linear speed: 40cm/s (constant current); Sample size: 1 μ L; Split ratio: 15: 1.;
Column temperature: 80 ℃ of (10min)-5 ℃/min-250 ℃-10 ℃/min-320 ℃ (25min);
2-17
#The cigarette comparison of the different preprocess methods of feed liquid
7
#Cigarette is relatively seen accompanying drawing 1 with the sample chromatogram figure that the different preprocess methods of feed liquid extract.
Repeatedly the concentrated active principle area of extraction is 1.15e
5PA.s; Distillation extraction active principle area is 6.46e simultaneously
2PA.s, once balance extraction active principle area are 7.50e
3PA.s.[annotate: the total area-solvent of active principle area=chromatographic peak (methylene chloride, ethanol, propylene glycol) peak area, down together "
2-23
#The cigarette comparison of the different preprocess methods of feed liquid
3
#Cigarette is relatively seen accompanying drawing 2 with the sample chromatogram figure that the different preprocess methods of feed liquid extract.
Repeatedly the concentrated active principle area of extraction is 2.76e
4PA.s, distillation extraction active principle area is 1.72e simultaneously
3PA.s, once balance extraction active principle area is 2.57e
3PA.s.
2-310
#The cigarette comparison of the different preprocess methods of feed liquid
10
#Cigarette is relatively seen accompanying drawing 3 with the sample chromatogram figure that the different preprocess methods of feed liquid extract.
Repeatedly the concentrated active principle area of extraction is 4.78e
5PA.s, distillation extraction active principle area is 1.71e simultaneously
5PA.s, once balance extraction active principle area is 4.43e
4PA.s.
From accompanying drawing 1～3 more as can be seen: at first, repeatedly extraction concentrates, distillation extraction distributes all very similar with the chromatogram of once balance extraction sample simultaneously; Secondly, repeatedly extract the enrichment method maximum, because ethanol soluble in water and propylene glycol repeatedly extract the back by a large amount of enrichments, therefore, other active principles do not reach the enrichment of expection; Simultaneously distillation extraction and once balance extraction phase ratio, natural essence, flavour content low 3
#, 7
#Cigarette extracts not as once balance on the contrary with the enrichment of feed liquid; For compound essence, flavour content big 10
#The cigarette feed liquid, distillation extraction is very similar with the once balance extraction chromatogram that obtains simultaneously, angle from the active principle area that extracted, distillation extraction is better than the once balance extraction simultaneously, but it is 1: 1 o'clock that solid-liquid ratio is adopted in the once balance extraction, and the gas chromatography active principle peak area total amount of extraction sample is greater than 10
4PA.s still is enough for gas chromatographic detection.
Natural essence, flavour content high 3
#, 7
#Emulsion was very serious when cigarette extracted with feed liquid, and layering is difficulty very, had therefore only extracted three times.
Table 1 is 18 kinds of cigarettes adopt the laggard promoting the circulation of qi analysis of hplc of once balance pre-service with feed liquid result.
18 kinds of cigarettes of table 1 result of feed liquid gas chromatographic analysis
In the table 1: solvent: feed liquid: water=solvent (mL): feed liquid (g): water (mL);
A
Ethanol=ethanol peak area;
A
Propylene glycol=propylene glycol peak area;
A
EffectThe total area-the A of chromatographic peak in the=spectrogram
Ethanol-A
Propylene glycol-A
Methylene chloride
Various cigarettes in the table 1 are all provided by producer with feed liquid, and wherein 3
#, 7
#, 10
#Concrete composition see Table 2～4.
As can be seen from Table 1: all feed liquids can reach 10 by effective peak area of once balance extraction back stratographic analysis
3More than the pA.s, this is enough for gas chromatography is quantitative, illustrates that the once balance extraction has extensive applicability as cigarette with the feed liquid preprocess method.
Test condition: with embodiment 1
Get cigarette feed liquid 14 respectively
#(is interior mark with n-octyl alcohol), 10
#(is interior mark with phenylacetate), 15
#(is interior mark with phenylacetate), the repeatability that method is carried out in once balance extraction pre-service investigates that (every group of sample desolventizes outside the peak, extract 20～35 chromatographic peaks by area size): the repeatability of carrying out retention time and concentration of component is investigated, and experimental result sees Table 5～7, accompanying drawing 4～9.From experimental result and accompanying drawing as can be seen: the RSD value of each component retention time is 0.02～0.10%; When mark carried out repeatability investigation to each concentration of component in adopting, the RSD value of each concentration of component value was all less than 5%, and only 10
#6.66 minutes chromatographic peak RSD value of feed liquid big (6.12%).With 14
#Internal standard compound n-octyl alcohol meter in the feed liquid, minimum detectable concentration are 0.33 μ g/g (in n-octyl alcohol, signal to noise ratio (S/N ratio) is 5).
The invention effect is summed up: the present invention adopts the extraction of liquid liquid once balance that cigarette is carried out pre-service with feed liquid, but what of extracted component in forming with feed liquid according to cigarette, cigarette is divided into two classes with feed liquid, can adopts different solid-liquid ratios to carry out pre-service respectively, to reach the requirement of gas chromatographic detection.Different with traditional liquid-liquid extraction method in this patent is to adopt the once balance extraction to extract sample; Utilize vortex (or fierce concussion), the auxiliary once balance extraction of centrifugation method.Vortex or fierce concussion can guarantee that extraction results is in equilibrium state really; Centrifugally operated can be avoided the appearance of emulsion, and the cigarette that some liquid-liquid extraction methods can't be handled obtains good treatment with feed liquid, and this is especially favourable with feed liquid for the higher cigarette of medicinal extract content.Adopt this method handle complicated cigarette with feed liquid with distillation extraction simultaneously, repeatedly extraction concentrates contrast, as can be seen: the sample that the once balance extraction extracts can embody the globality and the characteristic of volatility and half volatile chemical composition in the smoke materials liquid equally.Because the once balance extracting operation is simple, have only sampling, vortex (or fierce concussion), centrifugal, error is mainly derived from the error of cigarette with feed liquid, solvent, water and internal standard compound dosage, so error is little, the chance of polluting is also little, and these analyze particularly important to cigarette with the microcomponent in the feed liquid.Method repeated experiment result is: the RSD value of each component retention time is 0.02～0.10%; In adopting during scalar quantity, the RSD value of each concentration of component is all less than 5%, and only 10
#6.66 minutes chromatographic peak RSD value of feed liquid is big; Minimum detectable concentration is 0.33 μ g/g (in n-octyl alcohol, signal to noise ratio (S/N ratio) is 5).
In a word, cigarette extracts not only workable with the sample of feed liquid gas chromatographic analysis, the once balance that pre-service is adopted, and has extensive applicability and good extendability.
Table 23
#Cigarette materials formula of liquid list
| Sequence number | Material name | Specification | The place of production | Consumption (%) |
| 1 | The |
4 | ||
| 2 | The plum extract | 7 | ||
| 3 | The |
3 | ||
| 4 | |
6 | ||
| 5 | |
8 |
| Sequence number | Material name | Specification | The place of production | Consumption (%) |
| 6 | |
4 | ||
| 7 | Angelica |
3 | ||
| 8 | |
30 | ||
| 9 | |
15 | ||
| 10 | |
20 |
Table 37
#Cigarette materials formula of liquid list
Table 4 10
#Cigarette materials formula of liquid list
| Material name | Specification | Consumption | Remarks |
| The cloud and mist absolute oil | 10H0801 | 0.5 | |
| Damascenone 939697 | 10B0601 | 0.2 | |
| Damascenone 937459 | 10B4601 | 0.1 | |
| Dihydroactinidiolide | 10A15901 | 0.5 | |
| Angelica lactone (import) | 10A2602 | 0.5 | |
| Acetophenone | 10B1401 | 0.05 | |
| Geranyl acetone | 10B0701 | 0.2 |
| Material name | Specification | Consumption | Remarks |
| First position irisone | 10B3401 | 0.05 | |
| Isophorone | 10B0301 | 0.2 | |
| Furanone (golden aster) | 10B4901 | 0.6 | |
| 3, the 4-acetyl butyryl | 10B2002 | 0.1 | |
| Eugenol | 10K0301 | 0.2 | |
| Nerolidol | 10F1301 | 0.1 | |
| Menthol | 10P1201 | 2.0 | |
| Geranyl acetate | 10A0401 | 1.0 | |
| Root of Dahurain angelica tincture | 10C1401 | 1.7 | |
| |
30 | ||
| EA | 62 |
Table 5 once balance extraction preprocess method repeated experiment result (10
#N=7)
t(min) C(mg/g)
Mean value mean value
sd RSD(％) sd RSD(％)
(min) (mg/g)
6.2349 0.0066 0.11 1.4408 0.0133 0.92
6.6674 0.0064 0.096 0.1054 0.0064 6.11
8.8158 0.0103 0.12 0.7512 0.0058 0.77
11.4586 0.0117 0.10 0.3260 0.0020 0.60
14.3314 0.0104 0.073 0.2705 0.0017 0.62
14.9997 0.0105 0.070 1.2642 0.0033 0.26
15.3069 0.0103 0.068 0.7371 0.0081 1.09
17.7445 0.0097 0.054 2.4440 0.0206 0.84
19.4360 0.0096 0.050 0.0966 0.0006 0.63
20.0017 0.0111 0.055 25.650 40.2177 0.85
20.7081 0.0095 0.046 1.3029 0.0102 0.78
21.5324 0.0087 0.040 0.1122 0.0029 2.58
21.6017 0.0087 0.040 0.1021 0.0016 1.59
22.4672 0.0086 0.038 1.0676 0.0094 0.88
23.7760 0.0087 0.037 0.1165 0.0005 0.46
25.7735 0.0085 0.033 0.5675 0.0056 0.99
26.1700 0.0090 0.035 0.2095 0.0017 0.79
26.4313 0.0092 0.035 8.4839 0.0740 0.87
26.6123 0.0093 0.035 1.2414 0.0119 0.95
26.6832 0.0091 0.034 0.1139 0.0044 3.84
27.4737 0.0092 0.034 2.4947 0.0222 0.89
27.7927 0.0088 0.032 0.9919 0.0093 0.93
28.3004 0.0090 0.032 1.3018 0.0123 0.94
29.1871 0.0091 0.031 0.4263 0.0028 0.66
30.4175 0.0094 0.031 0.2411 0.0016 0.68
30.8682 0.0103 0.033 5.6565 0.0551 0.97
31.1399 0.0087 0.028 0.3319 0.0032 0.97
37.2183 0.0086 0.023 0.1395 0.0014 1.02
39.6035 0.0086 0.022 0.1307 0.0007 0.55
43.0616 0.0084 0.019 0.1293 0.0060 4.63
Table 6 once balance extraction preprocess method repeated experiment result (14
#N=4)
t(min) C(mg/g)
Mean value mean value
sd RSD(％) sd RSD(％)
(min) (mg/g)
2.3911 0.0011 0.044 1.4812 0.0368 2.48
2.5141 0.0015 0.059 216.7428 6.2653 2.89
3.7114 0.0021 0.055 1.1924 0.0411 3.45
4.5765 0.0030 0.066 0.5583 0.0092 1.64
4.8589 0.0032 0.066 0.4963 0.0070 1.41
6.3385 0.0059 0.094 0.4804 0.0069 1.45
6.4137 0.0062 0.097 0.1599 0.0022 1.40
11.9406 0.0113 0.095 0.7071 0.0090 1.27
13.5071 0.0128 0.095 0.4258 0.0070 1.63
14.3362 0.0112 0.078 0.0800 0.0010 1.30
15.4919 0.0098 0.063 1.9820 0.0361 1.82
16.7580 0.0108 0.065 0.2237 0.0028 1.25
16.9794 0.0099 0.058 0.7923 0.0097 1.23
17.0849 0.0101 0.059 0.2346 0.0029 1.22
17.4249 0.0107 0.061 0.3894 0.0061 1.56
19.0955 0.0107 0.056 0.2060 0.0026 1.26
19.8278 0.0091 0.046 1.3498 0.0179 1.33
20.9338 0.0062 0.029 4.1788 0.0620 1.48
22.2426 0.0100 0.045 0.0927 0.0016 1.72
22.5259 0.0096 0.045 0.0944 0.0013 1.39
24.9798 0.0098 0.039 0.5902 0.0080 1.35
25.1745 0.0100 0.040 0.1134 0.0013 1.18
25.5924 0.0098 0.038 0.0929 0.0012 1.31
26.7044 0.0087 0.032 2.0205 0.0285 1.41
27.0523 0.0093 0.034 0.3280 0.0054 1.65
27.6047 0.0088 0.032 0.0768 0.0015 1.91
34.0895 0.0102 0.030 0.0888 0.0010 1.10
34.2126 0.0100 0.029 0.0713 0.0007 0.98
36.0990 0.0093 0.026 0.8059 0.0126 1.57
36.3116 0.0089 0.024 0.4395 0.0063 1.43
42.5921 0.0104 0.024 0.0717 0.0013 1.81
43.5400 0.0092 0.021 0.0815 0.0016 1.98
45.9046 0.0091 0.020 0.1286 0.0021 1.63
Table 7 once balance extraction preprocess method repeated experiment result (15
#N=7)
t(min) c(mg/g)
Mean value mean value
sd RSD(％) sd RSD(％)
(min) (mg/g)
3.2436 0.0011 0.033 0.3105 0.0046 1.49
3.3248 0.0011 0.034 0.1413 0.0021 1.49
5.0691 0.0033 0.065 0.2113 0.0035 1.65
12.0582 0.0100 0.083 0.7605 0.0126 1.65
13.0326 0.0097 0.075 0.3078 0.0057 1.84
13.6446 0.0093 0.068 0.2772 0.0047 1.68
14.9812 0.0094 0.063 1.5194 0.0308 2.03
15.0701 0.0089 0.059 0.2548 0.0038 1.49
20.9941 0.0126 0.060 11.7964 0.1906 1.61
21.5105 0.0070 0.032 0.1954 0.0057 2.92
22.1373 0.0075 0.034 0.0889 0.0016 1.82
27.6464 0.0067 0.024 0.2315 0.0046 1.97
35.9554 0.0081 0.022 0.1581 0.0024 1.54
39.5607 0.0073 0.018 0.0457 0.0010 2.14
40.2594 0.0075 0.019 0.0949 0.0015 10.2
43.3533 0.0085 0.019 0.0432 0.0005 1.27
43.4583 0.0077 0.017 0.1118 0.0017 1.50
43.5953 0.0081 0.019 0.1526 0.0026 1.73
46.4286 0.0068 0.015 0.0806 0.0012 1.47
46.6707 0.0074 0.016 0.1527 0.0025 1.61
46.9559 0.0074 0.016 0.2600 0.0038 1.47
47.0589 0.0075 0.016 0.1160 0.0017 1.48
Claims (3)
1. cigarette is characterized in that: adopt the once balance extracting operation to extract the component of cigarette with gas chromatographic analysis needs in the feed liquid sample with the gas chromatographic analysis sample pretreating method of feed liquid;
For except that ethanol and propylene glycol, the cigarette feed liquid that volatility and half volatile organic component content are little, the once balance extraction solution that is adopted consists of, dichloromethane solution mL: cigarette feed liquid g: saturated common salt aqueous solution ml=1: 5: 3;
For except that ethanol and propylene glycol, the cigarette feed liquid that volatility and half volatile organic component content are big, the once balance extraction solution that is adopted consists of, dichloromethane solution mL: cigarette feed liquid g: saturated common salt aqueous solution ml=1: 1: 3;
Wherein containing internal standard compound phenylacetate, n-octyl alcohol or n-nonyl alcohol concentration in the dichloromethane solution is 1.0mg/ml;
Stir Centrifugical extraction solution, take off layer dichloromethane solution and carry out gas chromatographic analysis;
Carry out as follows with the definite of feed liquid volatility and half volatile organic component content size for cigarette,
With dichloromethane solution mL: cigarette feed liquid g: saturated common salt aqueous solution ml=1: 1: 3 condition once balance extraction, at analytical conditions for gas chromatography: chromatographic column HP-550m * 0.20mm * 0.33 μ m; Injector: 280 ℃; Detecting device: 280 ℃; Pressure: 403kpa before the post; Carrier gas: He; Linear speed: constant current 40cm/s; Sample size: 1 μ L; Split ratio: 15: 1; Column temperature: behind 80 ℃ of insulation 10min, be warming up to 250 ℃, be warming up to 320 ℃ of insulation 25min with 10 ℃/min again with 5 ℃/min;
The chromatographic peak total area in the extract except that methylene chloride and propylene glycol and ethanol is less than 10
4PAs is defined as the little cigarette feed liquid of volatility and half volatile organic component content; The chromatographic peak total area in the extract except that methylene chloride and propylene glycol and ethanol is greater than 10
4PAs is defined as the big cigarette feed liquid of volatility and half volatile organic component content.
2. according to the gas chromatographic analysis sample pretreating method of the described cigarette of claim 1, it is characterized in that with feed liquid:
After centrifugal, because water has a large amount of propylene glycol and ethanol, salt supersaturation is sometimes separated out, so white salt crystal can appear in dichloromethane solution lower floor, does not take out crystal during sampling.
3. according to the gas chromatographic analysis sample pretreating method of the described cigarette of claim 1 with feed liquid, it is characterized in that: described stirring is vortex or fierce concussion.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101571520B (en) * | 2008-04-28 | 2011-12-28 | 湖北中烟工业有限责任公司 | Gas chromatography multi-standard quantitative analysis method for tobacco essence |
| CN102072940B (en) * | 2010-11-11 | 2012-11-28 | 中国烟草总公司湖北省公司 | Method for measuring contents of coumarin and safrole in flavor and fragrance for cigarette |
| CN102318893A (en) * | 2011-08-26 | 2012-01-18 | 武汉黄鹤楼香精香料有限公司 | Sweet smoke plate essence |
| CN104122358B (en) * | 2014-07-26 | 2015-10-28 | 云南中烟工业有限责任公司 | A kind of assay method of electronic cigarette aroma volatile |
| CN105353069B (en) * | 2015-12-09 | 2017-11-07 | 中山大学惠州研究院 | A kind of detection method of natural perfume material |
| CN105823839B (en) * | 2016-03-15 | 2018-07-03 | 江苏中烟工业有限责任公司 | Piece cigarette absorbs the evaluation method of feed liquid effect during a kind of leaves storage |
| CN109283268A (en) * | 2018-09-27 | 2019-01-29 | 甘肃出入境检验检疫局检验检疫综合技术中心 | The analysis method of fragrance component in a kind of brackish water rose water |
| CN113295813B (en) * | 2021-05-20 | 2024-04-19 | 贵州中烟工业有限责任公司 | Detection method for material liquid application uniformity |
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