CN102608244A - Detection method for simultaneously determining plurality of flavor substances in cigarette cut tobaccos - Google Patents
Detection method for simultaneously determining plurality of flavor substances in cigarette cut tobaccos Download PDFInfo
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- CN102608244A CN102608244A CN2012100532644A CN201210053264A CN102608244A CN 102608244 A CN102608244 A CN 102608244A CN 2012100532644 A CN2012100532644 A CN 2012100532644A CN 201210053264 A CN201210053264 A CN 201210053264A CN 102608244 A CN102608244 A CN 102608244A
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Abstract
The invention provides a detection method for simultaneously determining a plurality of flavor substances in cigarette cut tobaccos. The flavor substances comprise furanone, isoamyl isovalerate, maltol, tabanone, menthol, ethyl maltol, 5-hydroxymethyl furfural and anethole. The method utilizes a solvent oscillation extraction method and a gas chromatography and mass spectrometry method to simultaneously determine the contents of a plurality of the flavor substances in the cigarette cut tobaccos; and the contents of a plurality of the flavor substances in a detection sample is calculated by the steps of preparing the detection sample, preparing a standard solution of a plurality of the flavor substances, preparing a sample solution and carrying out gas chromatography and mass spectrometry analysis. The method disclosed by the invention can accurately measure the contents of a plurality of the important flavor substances in a cigarette cut tobacco sample and is used for effectively evaluating the flavoring uniformity of the cigarette cut tobaccos, so as to provide the powerful technical support to a cigarette tobacco primary process. The method disclosed by the invention has the advantages of rapidness and convenience, simplicity in operation, good repeatability and high assay determination flexibility; and the recycling rate of a plurality of the important flavor substances can meet the requirements.
Description
Technical field
The present invention relates to tobacco detection technique field.
Background technology
In the cigarette process for making; Technology for making tobacco threds process operation is various, long flow path, job operation complicated, technological requirement is high; And perfuming is one of them important procedure, and its task is exactly that a certain amount of essence is applied on pipe tobacco or the stem by the requirement of producing, fill a prescription accurately, equably.Obviously, the accuracy of perfuming and homogeneity are the key factors that influences the cigarette product quality, and the content of important fragrance matter is the inhomogeneity very important index of evaluating cigarette technology for making tobacco threds perfuming in the cigarette shreds.Therefore; The perfuming uniformity index is monitored; To improve the accuracy and the homogeneity of perfuming in the cigarette technology for making tobacco threds, be to improve the stability of cigarette technology for making tobacco threds processing and the pith of controllability, also be the core technology that improves constantly cigarette product quality level.
Each cigarette enterprise lacks the detection method to important fragrance matter in the cigarette shreds at present, is difficult to the important fragrance matter in the pipe tobacco accurately quantitative.What adopted at present then all is to go to derive, calculate from the angle of theory to perfuming accuracy and inhomogeneity evaluation method basically; Or from the angle of process equipment go the adjustment, the rectification; Fundamentally the homogeneity of perfuming is not carried out quantitative research, be difficult to monitor effectively the perfuming process.Therefore; Set up a kind of check and analysis method and measure the content of important fragrance matter in the cigarette shreds; And then the homogeneity of coming the evaluating cigarette tobacco perfuming with the content of important fragrance matter; To strong technical support be provided to the processing of throwing coil of wire cigarette finished product, significant to the accuracy and the inhomogeneity raising of perfuming in the cigarette processing throwing Wiring technology.
Summary of the invention
The object of the invention is directed against the deficiency of above-mentioned prior art just; And a kind of detection method that is used for measuring simultaneously several kinds of important fragrance matters of cigarette shreds is provided specially; Be intended to through measuring the content of several kinds of important fragrance matters in the pipe tobacco; Realize the inhomogeneity evaluation of cigarette technology for making tobacco threds perfuming, improve the cigarette product quality.
The objective of the invention is to realize through following technical scheme.
Be used for measuring simultaneously the detection method of several kinds of fragrance matters of cigarette shreds; Said several kinds of fragrance matters comprise furanone, iso-amyl iso-valeriate, maltol, cigarette ketone, menthol, ethyl maltol, 5 hydroxymethyl furfural, anethole; This method is utilized solvent oscillation extraction and combined gas chromatography mass spectrometry; Simultaneously the content of several kinds of fragrance matters in the cigarette shreds is measured, may further comprise the steps:
2. prepare several kinds of fragrance matter standard solution: compound method does; Take by weighing furanone, iso-amyl iso-valeriate, maltol, cigarette ketone, menthol, ethyl maltol, 5 hydroxymethyl furfural, anethole and the mixing of equivalent weight respectively; Use ethanol to be mixed with the mixing storing solution of concentration as 100mg/L; Pipette storing solution 0.1 mL, 0.5 mL, 1 mL, 5 mL, 10 mL, 20 mL, 30 mL, 40 mL and 50 mL more respectively; Place nine volumetric flasks respectively; Obtain the compound solution that concentration is followed successively by 0.1 mg/L, 0.5 mg/L, 1.0 mg/L, 5.0 mg/L, 10.0 mg/L, 20.0 mg/L, 30.0 mg/L, 40.0 mg/L and 50.0 mg/L with ethanol dilution, as the working stamndard solution for standby;
3. prepare sample solution: 1. go on foot ready test sample with above-mentioned the and extract, extract is filtered the back add in the naphthalene mark and concentrate and obtain concentrate, again the concentrate filtration is obtained sample solution with extraction solvent;
4. gaschromatographic mass spectrometric analysis: respectively standard solution and sample solution are carried out check and analysis with gas chromatography mass spectrometer, obtain the quality of several kinds of fragrance matters in the sample;
5. calculate the content m of several kinds of fragrance matters in the test sample, computing formula is:
Wherein, A representes the quality of the fragrance matter that check and analysis obtain, and M representes the quality of test sample.
The present invention when preparing test sample, to every batch of pipe tobacco serial sampling 30 times, each sampling interval time 1min, the 100g that at every turn takes a sample gets a batch of sample every day, gets 5 batches altogether with 5 day time, mixes afterwards as test sample.Said extraction solvent be in methylene chloride, methyl tert-butyl ether, normal hexane, the ethanol any one or more than one.During the preparation sample solution, to each test sample extraction 1～3 time; When extracting 2 times or 3 times, refilter concentrated after the extract that each time obtained merges.Mark concentration is 5g/L in the said naphthalene.The analytical conditions for gas chromatography of gas chromatography mass spectrometer is: chromatographic column adopting be elasticity capillary column HP-5MS, injector temperature is 250 ℃, carrier gas is a He gas; Flow velocity is 1.0 mL/min, and sample size is 1.0 μ L, and split ratio is 20:1; Adopt temperature programme and split sampling mode; Heating schedule is: be warming up to 50 ℃ and keep 1min, rise to 160 ℃ and keep 2min with 8 ℃/min speed by 50 ℃ then, then rise to 280 ℃ and keep 15min with 8 ℃/min speed; The analysis condition of the mass detector of gas chromatography mass spectrometer is: solvent delay is 2min, and ionization voltage is 70ev, and ion source temperature is 230 ℃, and the transmission line temperature is 280 ℃, and the scan ion scope is at 35～450amu; The scanning of the mass spectrum pattern adopts full scan and selects the ion scan dual mode to scan simultaneously.
Outstanding advantage of the present invention is: adopt this method, can detect simultaneously several kinds of important fragrance matters in the cigarette shreds sample effectively, the homogeneity of cigarette technology for making tobacco threds perfuming is estimated.The inventive method pre-treatment is easy, and the sample of preparation can directly be used for extraction and detect, and need not grind into powder.Whole check and analysis method is simple and convenient; Favorable reproducibility, assay determination is highly sensitive, through measuring the content of important fragrance matter in the cigarette shreds; For the accuracy and the homogeneity of perfuming in the evaluating cigarette technology for making tobacco threds provides a kind of new approach, significant to improving the cigarette product quality.
Below in conjunction with specific embodiment the present invention is further set forth.
Description of drawings
Several kinds of fragrance matter mixing standard specimen total ion current figure in the pipe tobacco that Fig. 1 will detect for the present invention;
Fig. 2 is the selection ion flow graph of the selected cigarette shreds sample of embodiment.
Among the figure, 1, furanone; 2, iso-amyl iso-valeriate; 3, maltol; 4, cigarette ketone; 5, menthol; 6, naphthalene (interior mark); 7, ethyl maltol; 8,5 hydroxymethyl furfural; 9, anethole.
Embodiment
Embodiment 1
Be used for measuring simultaneously the detection method of several kinds of fragrance matters of cigarette shreds, said several kinds of fragrance matters are meant furanone, iso-amyl iso-valeriate, maltol, cigarette ketone, menthol, ethyl maltol, 5 hydroxymethyl furfural, anethole.The inventive method is utilized solvent oscillation extraction and gaschromatographic mass spectrometric analysis coupling method, simultaneously the content of several kinds of fragrance matters in the cigarette shreds is measured, and may further comprise the steps:
When preparing test sample, to every batch of pipe tobacco serial sampling 30 times, each sampling interval time 1min, the 100g that at every turn takes a sample gets a batch of sample every day, gets 5 batches altogether with 5 day time, mixes afterwards as test sample.
2. prepare several kinds of fragrance matter standard solution: compound method does; Take by weighing furanone, iso-amyl iso-valeriate, maltol, cigarette ketone, menthol, ethyl maltol, 5 hydroxymethyl furfural, anethole and the mixing of equivalent weight respectively; Use ethanol to be mixed with the mixing storing solution of concentration as 100mg/L; Pipette storing solution 0.1 mL, 0.5 mL, 1 mL, 5 mL, 10 mL, 20 mL, 30 mL, 40 mL and 50 mL more respectively; Place nine volumetric flasks respectively; Obtain the compound solution that concentration is followed successively by 0.1 mg/L, 0.5 mg/L, 1.0 mg/L, 5.0 mg/L, 10.0 mg/L, 20.0 mg/L, 30.0 mg/L, 40.0 mg/L and 50.0 mg/L with ethanol dilution, as the working stamndard solution for standby;
3. prepare sample solution: 1. go on foot ready test sample with above-mentioned the and carry out oscillation extraction, extract is filtered the back add in the naphthalene mark and concentrate and obtain concentrate, again the concentrate filtration is obtained sample solution with extraction solvent.In the optional methylene chloride of extraction solvent, methyl tert-butyl ether, normal hexane, the ethanol any one or more than one.Mark concentration is 5.0 g/L in the naphthalene that is added.During the preparation sample solution, can be to each test sample extraction 1～3 time.When extracting 2 times or 3 times, refilter concentrated after the extract that each time obtained merges.
4. gaschromatographic mass spectrometric analysis: respectively standard solution and sample solution are carried out check and analysis with gas chromatography mass spectrometer, obtain the quality of several kinds of fragrance matters in the sample.The analytical conditions for gas chromatography of gas chromatography mass spectrometer is: chromatographic column adopting be elasticity capillary column HP-5MS, injector temperature is 250 ℃, carrier gas is a He gas; Flow velocity is 1.0 mL/min, and sample size is 1.0 μ L, and split ratio is 20:1; Adopt temperature programme and split sampling mode; Heating schedule is: be warming up to 50 ℃ and keep 1min, rise to 160 ℃ and keep 2min with 8 ℃/min speed by 50 ℃ then, then rise to 280 ℃ and keep 15min with 8 ℃/min speed; The analysis condition of the mass detector of gas chromatography mass spectrometer is: solvent delay is 2min, and ionization voltage is 70ev, and ion source temperature is 230 ℃, and the transmission line temperature is 280 ℃, and the scan ion scope is at 35～450amu; The scanning of the mass spectrum pattern adopts full scan and selects the ion scan dual mode to scan simultaneously.
5. calculate the content m of several kinds of fragrance matters in the test sample, computing formula is m=A/M, and wherein, A representes the quality of the fragrance matter that check and analysis obtain, and M representes the quality of test sample.
Embodiment 2
Be used for measuring simultaneously the detection method of cigarette shreds furanone, iso-amyl iso-valeriate, maltol, cigarette ketone, menthol, ethyl maltol, 5 hydroxymethyl furfural, several kinds of fragrance matters of anethole; Assay method is to utilize solvent oscillation extraction and combined gas chromatography mass spectrometry, and several kinds of important fragrance matters in cigarette shreds sample or the used essence of sample are measured.
The inventive method is at first screened the pre-treatment experiment condition, and experiment parameter is optimized.Specifically may further comprise the steps:
1. detect the preparation with sample: sample can be taken from aromatic tobacco in the cigarette throwing Wiring technology, any in aromatic tobacco, the flavouring essence for tobacco not.Present embodiment is selected aromatic tobacco.Tobacco sample can be gathered in a certain fixed position in the sampling location of aromatic tobacco sample behind throwing line perfuming drum outlet; Treat stable back continuous random sampling 30 times in every batch, each sampling interval time 1min, each sampling quality 100g; Get one batch sample every day; Got five batches altogether with five day time, with five batches sample mix, the sample of measuring as several kinds of important fragrance matters.
2. prepare several kinds of fragrance matter standard solution: compound method specifically comprises: these several kinds of standard items of furanone, iso-amyl iso-valeriate, maltol, cigarette ketone, menthol, ethyl maltol, 5 hydroxymethyl furfural and anethole that take by weighing 0.1 g (being accurate to 0.1mg) respectively are formulated as the mixing storing solution of 100mg/L with ethanol dilution in beaker.Mixing storing solution should keep in Dark Place under 4 ℃～8 ℃ conditions, effective in three months.Working stamndard solution gets by mixing the storing solution dilution; Pipette storing solution 0.1 mL, 0.5 mL, 1 mL, 5 mL, 10 mL, 20 mL, 30 mL, 40 mL and 50 mL more respectively; Place nine volumetric flasks respectively; Obtain the compound solution that concentration is followed successively by 0.1 mg/L, 0.5 mg/L, 1.0 mg/L, 5.0 mg/L, 10.0 mg/L, 20.0 mg/L, 30.0 mg/L, 40.0 mg/L and 50.0 mg/L with ethanol dilution; As the working stamndard solution for standby, the working stamndard solution term of validity was generally 7 days, so should dispose weekly.
3. prepare sample solution: take by weighing 1 ~ 20g (being accurate to 0.1mg) tobacco sample and put into the 250mL conical flask; Add 60 ~ 200mL methylene chloride or methyl tert-butyl ether or normal hexane or ethanolic solution; The jog extraction flask; Moistening sample seals the back with 180r/min ~ 200 r/min speed oscillations extraction, 15 ~ 90min.Mark is settled to 1.0mL in the naphthalene that 10 μ L concentration are 5.0g/L with adding after the extract filtering and concentrating, again concentrate is crossed the organic system filter membrane and obtains sample solution.
Sample size, extraction solvent, extraction time, extraction times etc. all will be carried out grouping experiment successively, and the gaschromatographic mass spectrometric analysis of going forward side by side is determined optimized sample pre-treatments condition, sees table 1.
The optimization experiment of table 1 extraction pre-treatment condition
| Optimize content (pre-treatment condition) | The grouping experiment content |
| The selection of tobacco sample amount | 1.0g，2.0g，5.0g，10.0g，15.0g，20.0g |
| The selection of extraction time | 15min，30min，45min，60min，90min |
| The selection of extraction solvent | Methylene chloride, methyl tert-butyl ether, normal hexane, ethanol |
| The selection of extraction times | 1 extraction, 2 extractions, 3 extractions |
For example, get five parts of 1.0g tobacco sample, add the 60mL methylene chloride respectively, difference oscillation extraction 15min, 30min, 45min, 60min, 90min, every duplicate samples extraction 1 time.After extraction is accomplished; Be filtered to extract in the round-bottomed flask of band 1mL tail pipe through quantitative filter paper; Adding 10 μ L concentration is the interior mark of naphthalene of 5.0g/L; Be evaporated to 1.0mL with Rotary Evaporators, again it obtained sample solution through the organic system membrane filtration, sample solution is transferred to treated the sample introduction analysis in the stratographic analysis bottle.Behind gaschromatographic mass spectrometric analysis, selecting chromatographic peak area is greatly several kinds of samples that the fragrance matter recovery is good, is optimized sample pre-treatments condition with its pre-treatment condition (tobacco sample amount, extraction time, extraction solvent, extraction times).And for example, get five parts of 15.0g tobacco sample, add 200 mL ether respectively; Difference oscillation extraction 15min, 30min, 45min; 60min, 90min, every duplicate samples extraction 3 times; Combining extraction liquid and with adding after the extract filtering and concentrating mark is settled to 1.0 mL in the naphthalene that 10 μ L concentration are 5.0g/L, again concentrate is crossed the organic system filter membrane and obtains sample solution.Sample solution is behind gaschromatographic mass spectrometric analysis, and selecting chromatographic peak area is greatly several kinds of samples that the fragrance matter recovery is good, is optimized sample pre-treatments condition with its pre-treatment condition.
4. gaschromatographic mass spectrometric analysis: respectively standard solution and sample solution are carried out check and analysis with gas chromatography mass spectrometer, obtain the quality of several kinds of fragrance matters in the sample.The analytical conditions for gas chromatography of gas chromatography mass spectrometer is: chromatographic column adopting be elasticity capillary column HP-5MS (30m * 0.25mmi.d * 0.25 μ m i.d); Injector temperature is 250 ℃, and carrier gas is a He gas, and flow velocity is 1.0 mL/min; Sample size is 1.0 μ L; Split ratio is 20:1, adopts temperature programme and split sampling mode, and heating schedule is: be warming up to 50 ℃ and keep 1min; Rise to 160 ℃ and keep 2min with 8 ℃/min speed by 50 ℃ then, then rise to 280 ℃ and keep 15min with 8 ℃/min speed; The analysis condition of the mass detector of gas chromatography mass spectrometer is: solvent delay is 2min, and ionization voltage is 70ev, and ion source temperature is 230 ℃, and the transmission line temperature is 280 ℃, and the scan ion scope is at 35～450amu; The scanning of the mass spectrum pattern adopts full scan and selects the ion scan dual mode to scan simultaneously, and wherein selecting the characteristic ion of ion scan is the characteristic ion of several kinds of important fragrance matters, comprises quota ion and qualitative ion.In the mass spectrophotometry of complexion spectrum, target retention time and quota ion are seen table 2 in several kinds of important fragrance matters and the naphthalene.
Table 2 mass detector detects the retention time and the qualitative, quantitative ion of 8 kinds of important fragrance matters
| Sequence number | The fragrance matter title | Retention time (min) | Quota ion (m/z) | Qualitative ion (m/z) |
| 1 | Furanone | 8.34 | 128 | 43 |
| 2 | Iso-amyl iso-valeriate | 9.38 | 85 | 70 |
| 3 | Maltol | 9.56 | 126 | 97 |
| 4 | Cigarette ketone | 10.31 | 154 | 70 |
| 5 | Menthol | 10.79 | 138 | 81 |
| 6 | Naphthalene (interior mark) | 11.04 | 128 | 128 |
| 7 | Ethyl maltol | 11.25 | 140 | 71 |
| 8 | 5 hydroxymethyl furfural | 11.83 | 126 | 97 |
| 9 | Anethole | 12.94 | 148 | 117 |
Several kinds of fragrance matter mixing standard specimen total ion current figure that full scan obtains see Fig. 1; The selection ion flow graph of selecting ion scan to obtain is seen Fig. 2.
5. calculate the content m of several kinds of fragrance matters in the test sample, computing formula is following:
In the formula:
The content of important fragrance matter in m-every gram cigarette shreds sample (μ g/g);
The quality of important fragrance matter (g) in A-sample;
The quality of M-sample (g).
The cubage of several kinds of important fragrance matters; At first should carry out regretional analysis to its respective concentration, obtain typical curve with the detected object chromatographic peak area of nine groups of standard solution that concentration is followed successively by 0.1 mg/L, 0.5 mg/L, 1.0 mg/L, 5.0 mg/L, 10.0 mg/L, 20.0 mg/L, 30.0 mg/L, 40.0 mg/L and 50.0 mg/L; The object chromatographic peak area that then sample solution is detected, the substitution typical curve promptly obtains the quality of several kinds of fragrance matters in the sample, can calculate the content of fragrance matter in the pipe tobacco thus.The method that obtains of several kinds of fragrance matter quality described herein is an art methods, is with the direct check and analysis of gas chromatography mass spectrometer to obtain.
Embodiment 3
Prepare the chromatographically pure solvent: methylene chloride, absolute ethyl alcohol, methyl tert-butyl ether, normal hexane; Standard items: furanone (CAS:3658-77-3), iso-amyl iso-valeriate (CAS:659-70-1), maltol (CAS:118-71-8), cigarette ketone (CAS:4883-60-7), menthol (CAS:89-78-1), ethyl maltol (CAS:4940-11-8), 5 hydroxymethyl furfural (CAS:67-47-0), anethole (CAS:104-46-1); Naphthalene (CAS:91-20-3), purity is not less than 99%.Certain brand cigarette is aromatic tobacco not.
Preparation machine instrument: electronic balance, supersonic wave cleaning machine, oscillator, Rotary Evaporators, 7890-5975C GC-MS, capillary chromatographic column (elasticity capillary column HP-5MS post, specification are 30m * 0.25mmi.d * 0.25 μ m i.d).These equipment and instruments all can adopt the prior art equipment and instrument.
Working stamndard solution preparation: furanone, iso-amyl iso-valeriate, maltol, cigarette ketone, menthol, ethyl maltol, 5 hydroxymethyl furfural, these several kinds of standard items of anethole are mixed, use ethanol to be mixed with the mixing storing solution of concentration as 100mg/L.Pipette storing solution 0.1 mL, 0.5 mL, 1 mL, 5 mL, 10 mL, 20 mL, 30 mL, 40 mL and 50 mL respectively; Place nine volumetric flasks respectively; Obtain the compound solution that concentration is followed successively by 0.1 mg/L, 0.5 mg/L, 1.0 mg/L, 5.0 mg/L, 10.0 mg/L, 20.0 mg/L, 30.0 mg/L, 40.0 mg/L and 50.0 mg/L with ethanol dilution, as the working stamndard solution for standby.
The not aromatic tobacco sample of selected brand cigarette is accurately taken by weighing 1 ~ 20g (being accurate to 0.1mg); Put into the 250mL conical flask, add 60 ~ 200ml methyl tertbutyl ethereal solution, the jog extraction flask; Moistening sample seals the back with 180r/min ~ 200 r/min speed oscillations extraction, 15 ~ 90min; After extraction is accomplished; Be filtered to extract in the round-bottomed flask of band 1mL tail pipe through quantitative filter paper; Obtain filtrating; Add 10 μ L concentration again as marking in the naphthalene of 5.0g/L and being settled to 1.0mL after using the Rotary Evaporators concentrating under reduced pressure, again concentrate is obtained sample solution through the organic system membrane filtration, sample solution is transferred to treated the sample introduction analysis in the stratographic analysis bottle.
The gained sample solution is analyzed with gas chromatography mass spectrometer, obtained the quality A. of furanone, iso-amyl iso-valeriate, maltol, cigarette ketone, menthol, ethyl maltol, 5 hydroxymethyl furfural, several kinds of fragrance matters of anethole.Analytical conditions for gas chromatography is: chromatographic column adopting elasticity capillary column HP-5MS (30m * 0.25mm i.d * 0.25 μ m i.d), and 250 ℃ of injector temperatures, carrier gas He1.0 mL/min, sample size 1.0 μ L, split ratio is 20:1; The temperature programme process is: 50 ℃ (keeping 1min), rise to 160 ℃ (keeping 2min) with 8 ℃/min speed by 50 ℃, then rise to 280 ℃ (keeping 15min) by 160 ℃ with 8 ℃/min speed.The Mass Spectrometer Method analysis condition is: solvent delay 2min, and ionization voltage 70ev, 230 ℃ of ion source temperatures, 280 ℃ of transmission line temperature, scan ion scope 35～450amu, the scanning of the mass spectrum mode adopts SCAN and SIM to scan simultaneously.
Calculate the content m of several kinds of important fragrance matters in the tobacco sample:, wherein, A is the quality (g) of important fragrance matter in the sample; M is the quality (g) of the tobacco sample that takes by weighing.
Detection effect to the inventive method is analyzed:
(1) typical curve and detectability
Nine groups of standard solution that concentration are followed successively by 0.1 mg/L, 0.5 mg/L, 1.0 mg/L, 5.0 mg/L, 10.0 mg/L, 20.0 mg/L, 30.0 mg/L, 40.0 mg/L and 50.0 mg/L carry out the gas chromatography mass spectrometer analysis respectively; And be y with the area ratio of target quota ion chromatographic peak in the area of each standard solution quota ion chromatographic peak and the naphthalene; Mark concentration ratio is x in concentration of standard solution and the naphthalene; Carry out the correlation regression analysis, obtain regression equation and linear dependence parameter thereof.With the i.e. standard solution replicate determination 5 times of 0.5 mg/L of least concentration, gained is measured 3 times of detectabilities that are assay method of result standard deviation, and gained is measured 10 times of quantitative limit that are assay method of result standard deviation, and testing result is seen table 3.
The range of linearity of table 3 analytical approach and detectability
| Compound | Concentration range (μ g/mL) | Regression equation | Linearly dependent coefficient R | Detectability (ng/g) | Quantitative limit (ng/g) |
| Furanone | 0.1-50.0 | y = 0.1304x -0.005 | 0.9996 | 42.5 | 142 |
| Iso-amyl iso-valeriate | 0.1-50.0 | y = 0.3271x -0.0015 | 0.9993 | 46.3 | 154 |
| Maltol | 0.5-50.0 | y = 0.2065x -0.0081 | 0.9994 | 59.5 | 198 |
| Cigarette ketone | 0.5-50.0 | y = 0.1317x - 0.0014 | 0.9992 | 40.7 | 136 |
| Menthol | 0.1-50.0 | y = 0.1859x - 0.0016 | 0.9989 | 41.9 | 140 |
| Ethyl maltol | 0.5-50.0 | y = 0.1939x - 0.0121 | 0.9988 | 74.6 | 249 |
| 5 hydroxymethyl furfural | 0.5-50.0 | y = 0.1363x - 0.0067 | 0.9987 | 45.9 | 153 |
| Anethole | 0.1-50.0 | y = 0.3697x - 0.0042 | 0.9992 | 14.7 | 48.9 |
The scope that calculates the typical curve linearly dependent coefficient is between 0.9987 ~ 0.9996, and detectability is between 14.7ng/g ~ 74.6ng/g, and quantitative limit is between 48.9ng/g ~ 249ng/g.Show that the inventive method is all higher to stability, reliability, accuracy and the sensitivity of several kinds of important fragrance matter detections in the pipe tobacco, can satisfy the production demand fully.
(3) recovery of standard addition and repeatability
Adopt the test of sample recovery of standard addition; With the standard solution of several kinds of characteristic fragrance matters,, join in certain used brand cigarette pipe tobacco of embodiment 3 according to high, medium and low (50.0,10.0,0.5 μ g/ mL) three concentration gradients; Adopt the inventive method to carry out the gas chromatography mass spectrometer analysis; Each sample is measured respectively 6 times, calculates recovery of standard addition and the relative standard deviation that the inventive method detects several kinds of important fragrance matters that obtain according to analysis result, and the result sees table 4.
Table 4 recovery and repeatability (n=6 time) %
Can know by table 4; On basic, normal, high three mark-on concentration levels; The average recovery rate that utilizes several kinds of characteristic fragrance matters in the cigarette shreds that the inventive method detects is between 85.8% ~ 95.6%; The recovery meets the demands, and sample test result's relative standard deviation RSD is 4.1% ~ 7.1%, and repeatability better.
Claims (6)
1. be used for measuring simultaneously the detection method of several kinds of fragrance matters of cigarette shreds; Said several kinds of fragrance matters comprise furanone, iso-amyl iso-valeriate, maltol, cigarette ketone, menthol, ethyl maltol, 5 hydroxymethyl furfural, anethole; It is characterized in that; This method is utilized solvent oscillation extraction and combined gas chromatography mass spectrometry, simultaneously the content of several kinds of fragrance matters in the cigarette shreds is measured, and may further comprise the steps:
prepares test sample: sample is taken from aromatic tobacco or not aromatic tobacco or the flavouring essence for tobacco in the cigarette technology for making tobacco threds;
2. prepare several kinds of fragrance matter standard solution: compound method does; Take by weighing furanone, iso-amyl iso-valeriate, maltol, cigarette ketone, menthol, ethyl maltol, 5 hydroxymethyl furfural, anethole and the mixing of equal quality respectively; Use ethanol to be mixed with the mixing storing solution of concentration as 100mg/L; Pipette storing solution 0.1 mL, 0.5 mL, 1 mL, 5 mL, 10 mL, 20 mL, 30 mL, 40 mL and 50 mL more respectively; Place nine volumetric flasks respectively; Obtain the compound solution that concentration is followed successively by 0.1 mg/L, 0.5 mg/L, 1.0 mg/L, 5.0 mg/L, 10.0 mg/L, 20.0 mg/L, 30.0 mg/L, 40.0 mg/L and 50.0 mg/L with ethanol dilution, as the working stamndard solution for standby;
3. prepare sample solution: 1. go on foot ready test sample with above-mentioned the and extract, extract is filtered the back add in the naphthalene mark and concentrate and obtain concentrate, again the concentrate filtration is obtained sample solution with extraction solvent;
4. gaschromatographic mass spectrometric analysis: respectively standard solution and sample solution are carried out check and analysis with gas chromatography mass spectrometer, obtain the quality of several kinds of fragrance matters in the sample;
5. calculate the content m of several kinds of fragrance matters in the test sample; Computing formula is
; Wherein, A representes the quality of the fragrance matter that check and analysis obtain, and M representes the quality of test sample.
2. according to the said detection method that is used for measuring simultaneously several kinds of fragrance matters of cigarette shreds of claim 1, it is characterized in that, when preparing test sample; To every batch of pipe tobacco serial sampling 30 times; Each sampling interval time 1min, the 100g that at every turn takes a sample gets a batch of sample every day; Got 5 batches altogether with 5 day time, mix the back as test sample.
3. according to the said detection method that is used for measuring simultaneously several kinds of fragrance matters of cigarette shreds of claim 1, it is characterized in that, above-mentioned 3. go on foot said extraction solvent be in methylene chloride, methyl tert-butyl ether, normal hexane, the ethanol any one or more than one.
4. according to the said detection method that is used for measuring simultaneously several kinds of fragrance matters of cigarette shreds of claim 1, it is characterized in that, during the preparation sample solution, each test sample extraction 1～3 time; When extracting 2 times or 3 times, refilter concentrated after the extract that each time obtained merges.
5. according to the said detection method that is used for measuring simultaneously several kinds of fragrance matters of cigarette shreds of claim 1, it is characterized in that mark concentration is 5g/L in the said naphthalene.
6. according to the said detection method that is used for measuring simultaneously several kinds of fragrance matters of cigarette shreds of claim 1, it is characterized in that the analytical conditions for gas chromatography of gas chromatography mass spectrometer is: chromatographic column adopting be elasticity capillary column HP-5MS; Injector temperature is 250 ℃, and carrier gas is a He gas, and flow velocity is 1.0 mL/min; Sample size is 1.0 μ L; Split ratio is 20:1, adopts temperature programme and split sampling mode, and heating schedule is: be warming up to 50 ℃ and keep 1min; Rise to 160 ℃ and keep 2min with 8 ℃/min speed by 50 ℃ then, then rise to 280 ℃ and keep 15min with 8 ℃/min speed; The analysis condition of the mass detector of gas chromatography mass spectrometer is: solvent delay is 2min, and ionization voltage is 70ev, and ion source temperature is 230 ℃, and the transmission line temperature is 280 ℃, and the scan ion scope is at 35～450amu; The scanning of the mass spectrum pattern adopts full scan and selects the ion scan dual mode to scan simultaneously.
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| CN103226136A (en) * | 2012-10-15 | 2013-07-31 | 红塔烟草(集团)有限责任公司 | Detection and determination method for flavor type of cigarette |
| CN103226135A (en) * | 2012-10-15 | 2013-07-31 | 红塔烟草(集团)有限责任公司 | Detection and determination method for flavor type of flue-cured tobacco |
| CN103983721A (en) * | 2014-04-17 | 2014-08-13 | 江苏中烟工业有限责任公司 | Method for determination of cut cigarette tobacco preparation charging uniformity based on multi-index characteristic substance weight determination |
| CN104792895A (en) * | 2015-04-21 | 2015-07-22 | 陕西中烟工业有限责任公司 | Method for determining menthol in tobacco flavor and perfume |
| CN106018628A (en) * | 2016-08-08 | 2016-10-12 | 云南中烟工业有限责任公司 | Method for detecting furfurals in saliva of smokers |
| CN106053619A (en) * | 2016-05-11 | 2016-10-26 | 中国烟草总公司郑州烟草研究院 | A high-throughput analysis method for measuring volatile and semi-volatile components in particulate matters of cigarette main stream smoke |
| CN109541050A (en) * | 2018-11-09 | 2019-03-29 | 重庆市食品药品检验检测研究院 | A kind of gas chromatography measures malt phenols content method in edible vegetable oil simultaneously |
| CN109580830A (en) * | 2018-12-28 | 2019-04-05 | 成都康美药业生产有限公司 | The detection method of trans-anethole content in a kind of fennel seeds |
| CN110133171A (en) * | 2019-05-28 | 2019-08-16 | 红云红河烟草(集团)有限责任公司 | A kind of method and its identification method improving natural perfume for cigarette flavor component |
| CN110243959A (en) * | 2019-06-11 | 2019-09-17 | 华中农业大学 | A kind of separation of endogenous fragrance component in Carnation flowers and identification method |
| CN113203823A (en) * | 2021-04-21 | 2021-08-03 | 中国烟草总公司郑州烟草研究院 | Application of hydroxyl-containing compound, matrix improver and method for analyzing flavor components in tobacco |
| CN114088584A (en) * | 2021-11-01 | 2022-02-25 | 河南中烟工业有限责任公司 | Method for detecting and correcting diffusion rate of feed liquid applied in heating cigarette |
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| CN114113411A (en) * | 2021-12-15 | 2022-03-01 | 深圳天祥质量技术服务有限公司 | Method for simultaneously detecting 5 harmful substances in consumer goods |
| CN114113368A (en) * | 2021-10-27 | 2022-03-01 | 河南中烟工业有限责任公司 | Mouth-by-mouth transfer control method for heating sweet and fragrant monomers in cigarettes |
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| CN106053619B (en) * | 2016-05-11 | 2018-10-09 | 中国烟草总公司郑州烟草研究院 | Volatilization in a kind of high throughput assay cigarette mainstream smoke condensate, half volatile ingredient analysis method |
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| CN109580830A (en) * | 2018-12-28 | 2019-04-05 | 成都康美药业生产有限公司 | The detection method of trans-anethole content in a kind of fennel seeds |
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| CN110243959A (en) * | 2019-06-11 | 2019-09-17 | 华中农业大学 | A kind of separation of endogenous fragrance component in Carnation flowers and identification method |
| CN113203823A (en) * | 2021-04-21 | 2021-08-03 | 中国烟草总公司郑州烟草研究院 | Application of hydroxyl-containing compound, matrix improver and method for analyzing flavor components in tobacco |
| CN114113368A (en) * | 2021-10-27 | 2022-03-01 | 河南中烟工业有限责任公司 | Mouth-by-mouth transfer control method for heating sweet and fragrant monomers in cigarettes |
| CN114088583B (en) * | 2021-11-01 | 2024-03-19 | 河南中烟工业有限责任公司 | Method for establishing diffusion model of applied feed liquid in heating cigarette |
| CN114088584A (en) * | 2021-11-01 | 2022-02-25 | 河南中烟工业有限责任公司 | Method for detecting and correcting diffusion rate of feed liquid applied in heating cigarette |
| CN114088583A (en) * | 2021-11-01 | 2022-02-25 | 河南中烟工业有限责任公司 | Method for establishing applied liquid diffusion model in heating cigarette |
| CN114088584B (en) * | 2021-11-01 | 2024-03-19 | 河南中烟工业有限责任公司 | Detection and correction method for diffusion rate of applied feed liquid in heating cigarette |
| CN114113411A (en) * | 2021-12-15 | 2022-03-01 | 深圳天祥质量技术服务有限公司 | Method for simultaneously detecting 5 harmful substances in consumer goods |
| CN114778720A (en) * | 2022-03-31 | 2022-07-22 | 红塔烟草(集团)有限责任公司 | P & T-GC-MS method for detecting characteristic aroma components in tow flavored filter stick |
| CN116297956B (en) * | 2023-03-17 | 2024-01-30 | 江苏中烟工业有限责任公司 | Method for evaluating release and transfer behaviors of acidic fragrant raw materials in cigarettes of different circumferences |
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