CN103105449B - Method for evaluating cigarette filament charging uniformity based on characteristic fragrance substance - Google Patents
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Abstract
The invention provides a method for evaluating cigarette filament charging uniformity based on a characteristic fragrance substance, which comprises the following steps: screening the characteristic fragrance substance suitable for symptom uniformity, taking the characteristic fragrance substance as a landmark, using the landmark content in a product after charging to represent the distribution condition of the material liquid content in the product, and detecting, calculating and performing statistic analysis to determine the uniformity degree of a charging process. The method provided by the invention has the following technical effect that the characteristic fragrance substance in the material liquid is taken as the landmark, the cigarette charging uniformity effect can be directly quantized from a microscopic view point, the uncertainty from whole reflection of the charging accuracy through charging proportion can be avoided, from the equipment hardware, application and promotion of the result need corresponded an separation and analysis instrument and corresponded technical methods, so that the method is practical without complex technology.
Description
Technical field
The present invention relates to a kind of method of feature based fragrance matter evaluating cigarette throwing feeding homogeneity, specifically, relate to the evaluation method of charging precision and homogeneity in cigarette primary processing charging process, utilize the present invention can quantize the reinforced homogeneity of cigarette primary processing, determine cigarette charging precision.
Background technology
It is important procedure in production of cigarettes process that throwing is fed in raw material, its task be by feed liquid by producing, the requirement of formula is applied on goods (smoked sheet, stem etc.) evenly, exactly to reach seasoning, flavouring, humectation, mildew-resistant, the object such as combustion-supporting, feed liquid applies evenly with the no consistance directly having influence on cigarette product aesthetic quality, material mass, and then affects the aesthetic quality of cigarette product and the economic benefit of enterprise.
At present, domestic each cigarette enterprise is to the evaluation of accuracy reinforced in production run, mainly be less than 1.0% according to the cigarette charging accuracy requirement of regulation in " cigarette process code requirement " (State Tobacco Monopoly Bureau issues in March, 2003), the reflection of this charging precision be to be sprayed onto in feed rollers feed liquid quality in the unit interval and to enter the stability of cylinder at quality of item ratio, from the angle of macroscopic view, reinforced overall condition is evaluated, what be not enough to that comprehensively reflection adds on product surface feed liquid to is uniformly distributed situation, be difficult to the precision of the reinforced process of monitoring completely.Current, when needing to improve charging (feeding) equipment, how by artificial sense smoke panel test reinforced after the cigarette made at goods pass judgment on and optimize whether Results, this method workload is large, and more by interference from human factor, error is larger.Therefore, set up the evaluation method of cigarette primary processing charging process feed liquid application uniformity, after objective evaluation feeds in raw material in goods the degree of uniformity of feed liquid content, for the improvement of instrument and supplies, so the stability of cigarette product quality and promote and have very important meaning.
Comprehensive literature is investigated, and can find in recent years, and industry is inside and outside has some bibliographical informations in the quantitative research of charging process homogeneity, wherein major part all with 1,2-propylene glycol as label.Such as, application for a patent for invention 200910227567.1 discloses " a kind of method measuring feed liquid application uniformity in cigarette charging process ", this patent is with in feed liquid 1,2-propylene glycol is label, utilize reinforced after in smoked sheet 1, the content of 2-propylene glycol represents the distribution situation of feed liquid content in smoked sheet, is determined the degree of uniformity fed in raw material by detection, calculating and statistical study.The method is by detecting 1 in institute's sample thief (20 ~ 40g), 2-content of propylene glycol, calculate the relative standard deviation of n (n > 30) individual sample 1,2-content of propylene glycol, characterize homogeneity with relative standard deviation.But, say objectively, this patent is when detection content of propylene glycol, the sample method for making sample adopted is Oven Method, namely under 40 DEG C of conditions, offal is ground to form after drying, the result of gained is lost, and has very large deviation with the actual value of sample size, can not quantize the homogeneity of charging process very perfectly.
In addition, patent of invention 200810022416.8 discloses and a kind ofly detects the method for perfuming homogeneity of cigarette production based on label, and the homogeneity of cigarette primary processing perfuming operation that what the method was investigated is, the research object related to is essence (namely showing perfume (or spice)).Consider that in cigarette primary processing process, reinforced (i.e. feed liquid) and perfuming (namely showing perfume (or spice)) operation also exist very large difference, such as feed liquid is different with the material property of table perfume (or spice), difference is very large, equipment, machined parameters etc. besides involved by process are different, therefore, the uniform evaluation method of charging process can not be directly enclosed within by the detection method of perfuming operation homogeneity simply.Besides, in this patent homogeneity expression be that relative standard deviation (i.e. SD) is expressed, directly could not provide uniformity coefficient, cheap visual amount uniformity results.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, provide a kind of feature based fragrance matter to carry out the method for evaluating cigarette feeding homogeneity.The object of the method selects out suitable characteristic chicken flavor material, in this, as mark, then be characterizing objects with mark, solvent-extracted pre-treating method is taked to carry out pre-treatment to sample, by GC/MS, the mark after reinforced in goods is analyzed, and then the homogeneity of cigarette charging is evaluated.
The method of feature based fragrance matter evaluating cigarette throwing feeding homogeneity of the present invention, comprise the following steps: first filter out the characteristic chicken flavor material being suitable for characterizing homogeneity, with characteristic chicken flavor material for mark, utilize reinforced after in goods mark content represent the distribution situation of feed liquid content in goods, by detecting, calculating and the degree of uniformity of statistical study determination charging process.
The method of feature based fragrance matter evaluating cigarette throwing feeding homogeneity of the present invention, comprises the following steps:
1) selected characteristic fragrance matter:
Characteristic chicken flavor material is chosen with following 4 principles and obtains: (1) be the material that contains in interpolation feed liquid, and this material plays certain positive effect to cigarette product flavouring essence quality, namely increases fragrance, improves cigarette smoking quality; (2) be the material itself do not contained in goods before throwing charging process.Even if or contain, but compared with the content of this material in feed liquid, before operation processing, in goods, the content of this material is little; (3) physicochemical property should be stablized, and is easily extracted by qualitative and quantitative analysis; (4) should be safe on toxicological evaluation, meet the relevant regulations of country about tobacco additive agent permission to use.
Choosing method is: get cigarette and do not feed in raw material at goods 2 equal portions, 1 part as blank sample, another 1 part reinforced by normal feeding quantity after as spiked sample; Make GC/MS after two increment product are carried out solvent extraction respectively to analyze, in the chromatogram total ion current figure of spiked sample, find out the component peaks obviously increased, and become swarming in this, as this cigarette charging of difference whether characteristic chicken flavor,
Wherein, GC/MS analysis condition is: chromatographic column is the special capillary chromatographic column of polarity MS (60m × 0.25mm × 0.25 μm); Carrier gas: He, flow is 1.0mL/min; Injector temperature: 260 DEG C; Spin manifold temperature: initial temperature 60 DEG C, keeps 1min, rises to 250 DEG C with 10 DEG C/min, keeps 5min; Transmission line temperature: 280 DEG C; Ionization energy: 70eV; EI ion source temperature: 230 DEG C; Quadrupole rod temperature: 150 DEG C; Mass scan range: 30 ~ 500amu; Solvent delay: 6min; Scan pattern: SCAN;
2) marker detection:
Sample after good from on-site sampling adopts the sample preparation of chopping method, namely use for laboratory filament cutter is started, sample is put into filament cutter injection port, carry out chopping, tobacco cut width is 0.9 ~ 1.0mm, sample after cutting loads in polybag immediately, abundant shake, mixing, this is ready-made sample, then ethanol is used to be solvent, solvent extraction is carried out to a certain amount of sample, obtains sample introduction liquid after filtration, carry out GC/MS analysis, scanning of the mass spectrum pattern adopts Selective ion mode scanning, and quota ion is the characteristic ion of the characteristic chicken flavor material in step 1);
Wherein, GC/MS analysis condition is: chromatographic column is the special capillary chromatographic column of polarity MS (60m × 0.25mm × 0.25 μm); Carrier gas: He, flow is 1.0mL/min; Injector temperature: 260 DEG C; Spin manifold temperature: initial temperature 60 DEG C, keeps 1min, rises to 250 DEG C with 10 DEG C/min, keeps 5min; Transmission line temperature: 280 DEG C; Ionization energy: 70eV; EI ion source temperature: 230 DEG C; Quadrupole rod temperature: 150 DEG C; Mass scan range: 30 ~ 500amu; Solvent delay: 6min; Scan pattern: SIM;
3) sample: carry out sampling parameters respectively and determine test: 1. sampling amount test: in the constant duration sampling of feed rollers outlet fixed position, interval time 60 s, sample 60 times altogether, get at every turn simultaneously reinforced after at goods 10 g, 30 g, 50 g, 70 g and each 1 time of 90 g samples; 2. sample number of times test: according to the sampling amount 1. determined, in the constant duration sampling of feed rollers outlet fixed position, interval time 60, s, sampled 10 times, 20 times, 30 times and 40 times respectively; 3. sampling interval time test: according to the sampling amount 1., 2. determined and sampling number of times, in feed rollers outlet fixed position, constant duration 60 s, 90 s and 120 s sample respectively;
According to concrete test findings, adopt statistical study means, obtaining preferably sampling parameters is: sampling amount 30g, sampling 30 times, and sample interval is 60s.
4) expression of homogeneity: sample, according to step 2 according to the sampling parameters in step 3)) method detect, the reinforced homogeneity that applies of throwing is according to following formulae discovery:
Wherein:
CU-feeding homogeneity, %;
The content of mark in Xi-the i-th sample, mg/kg;
the mean value of mark content in-sample, mg/kg;
The sampling number of times of n-sample.
The size reflection cigarette charging degree of uniformity of CU value, CU value is larger, and feeding homogeneity is better.
The present invention has following technique effect: the specific fragrance matter component in selection feed liquid, as mark, has directly quantized cigarette charging even results from the angle of microcosmic, avoids and macroscopically reflects by feed ratio entirety the uncertainty that charging precision brings; From device hardware aspect in fact, the application of achievement only needs corresponding compartment analysis instrument and relevant technical method (GC/MS and corresponding pre-processing device), practical, does not have complicated technique.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further, but do not limit the present invention.
embodiment 1: choosing of characteristic chicken flavor material
Art scheme gets reinforced smoked sheet 2 equal portions, 1 part as blank sample, another 1 part is fed in raw material by normal feeding quantity.Make GC/MS after two increment product are carried out solvent extraction respectively to analyze.Analysis condition is: HP-Innowax capillary chromatographic column (60m × 0.25mm × 0.25 μm); Carrier gas: He, flow 1.0mL/min; Injector temperature: 260 DEG C; Spin manifold temperature: initial temperature 60 DEG C, keeps 1min, rises to 250 DEG C with 10 DEG C/min, keeps 5min; Transmission line temperature: 280 DEG C; Ionization energy: 70eV; EI ion source temperature: 230 DEG C; Quadrupole rod temperature: 150 DEG C; Mass scan range: 30 ~ 500amu; Solvent delay: 6min; Scan pattern: SCAN.
Find through map identification, after reinforced, in smoked sheet sample, add some volatility, semi-volatile compounds.In conjunction with the analysis result of non-spiked sample, after reinforced, in smoked sheet, the content of ethyl maltol (hereinafter referred to as EM) increases considerably, and is confirmed to be the characteristic chicken flavor composition in feed liquid.Verify GB2760-2011 " food additives use standard " again, find that this material allows to use, meet the relevant request for utilization of country.Consult further, find the ultimate food adjuvant that ethyl maltol is a kind of safety non-toxic, purposes is wide, effective, consumption is few, it is the fragrant and sweet taste synergistic agent that tobacco, food, beverage, meat products, seafood, essence, fruit wine, daily cosmetics etc. are good, to the improving fragrance of food and enhancing, there is remarkable result, sweet food is played and increases sweet effect, and there is antibacterial, antiseptic property, the food storing phase can be extended.
Analyze through above, according to the selection principle of mark, determine that EM is the mark this time characterizing charging process homogeneity.
embodiment 2: marker detection
Marker detection method: the sample after good from on-site sampling adopts the sample preparation of chopping method, namely use for laboratory filament cutter is started, sample is put into filament cutter injection port, carry out chopping, tobacco cut width is 0.9 ~ 1.0mm, sample after cutting loads in polybag immediately, abundant shake, mixing, this is ready-made sample, then ethanol is used to be solvent, solvent extraction is carried out to a certain amount of sample, obtains sample introduction liquid after filtration, carry out GC/MS analysis, scanning of the mass spectrum pattern adopts Selective ion mode scanning, and quota ion is the characteristic ion of characteristic chicken flavor material;
Wherein, GC/MS analysis condition is: chromatographic column is the special capillary chromatographic column of polarity MS (60m × 0.25mm × 0.25 μm); Carrier gas: He, flow is 1.0mL/min; Injector temperature: 260 DEG C; Spin manifold temperature: initial temperature 60 DEG C, keeps 1min, rises to 250 DEG C with 10 DEG C/min, keeps 5min; Transmission line temperature: 280 DEG C; Ionization energy: 70eV; EI ion source temperature: 230 DEG C; Quadrupole rod temperature: 150 DEG C; Mass scan range: 30 ~ 500amu; Solvent delay: 6min; Scan pattern: SIM;
The making of working curve: accurately take 0.5 g EM standard specimen, be settled to ethanol in the volumetric flask of 100 mL, shaken well.Accurately pipette standard specimen solution 1,2,5,10 and 20 mL respectively, be settled to ethanol in the volumetric flask of 100 mL.GC/MS analysis is carried out to standard serial solution, obtains linear work curve, in table 1.
Repeatability checking: according to the solvent extraction in test method, repeats whole analytic process 6 times with the smoked sheet sample after same feeding in raw material, the results are shown in Table 2.The data of table 2 illustrate that the method repeatability is good.
Recovery test: adopt standard substance additive process to measure the EM recovery.In smoked sheet sample to be measured, add the standard specimen of different amount, measure according to the solvent extraction in test method, result of calculation is in table 3.The EM recovery is between 95.95% ~ 106.45% as can be seen from Table 3, and illustration method is relatively more abundant to the extraction of EM in smoked sheet, and method accurately and reliably.
embodiment 3: sample
Sample method:: carry out sampling parameters respectively and determine test: 1. sampling amount test: in the constant duration sampling of feed rollers outlet fixed position, interval time 60 s, sample 60 times altogether, get at every turn simultaneously reinforced after at goods 10 g, 30 g, 50 g, 70 g and each 1 time of 90 g samples; 2. sample number of times test: according to the sampling amount 1. determined, in the constant duration sampling of feed rollers outlet fixed position, interval time 60, s, sampled 10 times, 20 times, 30 times and 40 times respectively; 3. sampling interval time test: according to the sampling amount 1., 2. determined and sampling number of times, in feed rollers outlet fixed position, constant duration 60 s, 90 s and 120 s sample respectively;
Detect: according to the method for testing of above-mentioned mark EM, rear tobacco sample reinforced in different sampling amount situation is detected, the results are shown in Table 4.Under the condition of level of significance α=0.05, application method of analysis of variance compares different sampling amount mark EM content average, and the results of analysis of variance is in table 5.From analysis result: level of significance is less than 0.05, under different sampling amount condition is described, EM content average has significant difference.
Further analysis, application least significant difference method (LSD), does Multiple range test (α=0.05) to different sampling amount EM content average, the results are shown in Table 6.As shown in Table 6, when sampling amount is 10 g, in average, significant difference is there is with the sample of other sampling amounts, and sampling amount is when being 30 ~ 90 g, between each sampling amount, the EM content average difference of sample is not remarkable, namely when sampling amount is 30 ~ 90 g, the dispersion degree no significant difference of EM content in sample; Consider efficiency and the economy of test simultaneously, determine sampling amount when 30 g test as reality.
embodiment 4: the mensuration of homogeneity
The expression of homogeneity: sample, according to step 2 according to the sampling parameters in step 3)) method detect, the reinforced homogeneity that applies of throwing is according to following formulae discovery:
Wherein:
CU-feeding homogeneity, %;
The content of mark in Xi-the i-th sample, mg/kg;
the mean value of mark content in-sample, mg/kg;
The sampling number of times of n-sample.
Sample according to the sampling parameters method determined, carry out analysis according to the mark method of testing set up and detect, then carry out Evaluation for Uniformity, measurement result is in table 7.
Claims (1)
1. the method for a feature based fragrance matter evaluating cigarette throwing feeding homogeneity, it is characterized in that, comprise the following steps: first filter out the characteristic chicken flavor material being suitable for characterizing homogeneity, with characteristic chicken flavor material for mark, after utilization is reinforced, in goods, mark content represents the distribution situation of feed liquid content in goods, by detecting, calculating and the degree of uniformity of statistical study determination charging process, concrete steps are as follows:
1) selected characteristic fragrance matter:
Characteristic chicken flavor material is chosen with following 4 principles and obtains: (1) be the material that contains in interpolation feed liquid, and this material plays certain positive effect to cigarette product flavouring essence quality, namely increases fragrance, improves cigarette smoking quality; (2) be the material itself do not contained in goods before throwing charging process, even if or contain, but compared with the content of this material in feed liquid, before operation processing, in goods, the content of this material is little; (3) physicochemical property should be stablized, and is easily extracted by qualitative and quantitative analysis; (4) be safe on toxicological evaluation, meet the relevant regulations of country about tobacco additive agent permission to use,
Choosing method is: get cigarette and do not feed in raw material at goods 2 equal portions, 1 part as blank sample, another 1 part reinforced by normal feeding quantity after as spiked sample; Make GC/MS after two increment product are carried out solvent extraction respectively to analyze, in the chromatogram total ion current figure of spiked sample, find out the component peaks obviously increased, and become swarming in this, as this cigarette charging of difference whether characteristic chicken flavor,
Wherein, GC/MS analysis condition is: chromatographic column is the special capillary chromatographic column of polarity MS of 60m × 0.25mm × 0.25 μm, carrier gas: He, and flow is 1.0mL/min; Injector temperature: 260 DEG C; Spin manifold temperature: initial temperature 60 DEG C, keeps 1min, rises to 250 DEG C with 10 DEG C/min, keeps 5min; Transmission line temperature: 280 DEG C; Ionization energy: 70eV; EI ion source temperature: 230 DEG C; Quadrupole rod temperature: 150 DEG C; Mass scan range: 30 ~ 500amu; Solvent delay: 6min; Scan pattern: SCAN;
2) marker detection:
Sample after good from on-site sampling adopts the sample preparation of chopping method, namely use for laboratory filament cutter is started, sample is put into filament cutter injection port, carry out chopping, tobacco cut width is 0.9 ~ 1.0mm, sample after cutting loads in polybag immediately, abundant shake, mixing, this is ready-made sample, then ethanol is used to be solvent, solvent extraction is carried out to a certain amount of sample, obtains sample introduction liquid after filtration, carry out GC/MS analysis, scanning of the mass spectrum pattern adopts Selective ion mode scanning, and quota ion is step 1) in the characteristic ion of characteristic chicken flavor material;
Wherein, GC/MS analysis condition is: the special capillary chromatographic column of polarity MS of chromatographic column to be specification be 60m × 0.25mm × 0.25 μm; Carrier gas: He, flow is 1.0mL/min; Injector temperature: 260 DEG C; Spin manifold temperature: initial temperature 60 DEG C, keeps 1min, rises to 250 DEG C with 10 DEG C/min, keeps 5min; Transmission line temperature: 280 DEG C; Ionization energy: 70eV; EI ion source temperature: 230 DEG C; Quadrupole rod temperature: 150 DEG C; Mass scan range: 30 ~ 500amu; Solvent delay: 6min; Scan pattern: SIM;
3) sample: carry out sampling parameters respectively and determine test: 1. sampling amount test: in the constant duration sampling of feed rollers outlet fixed position, interval time 60s, sample 60 times altogether, get at every turn simultaneously reinforced after at goods 10g, 30g, 50g, 70g and 90g sample each 1 time; 2. sample number of times test: according to the sampling amount 1. determined, in the constant duration sampling of feed rollers outlet fixed position, interval time, 60s, sampled 10 times, 20 times, 30 times and 40 times respectively; 3. sampling interval time test: according to the sampling amount 1., 2. determined and sampling number of times, in constant duration 60s, 90s and 120s sampling respectively of feed rollers outlet fixed position, based on the impact of on-line period parameter on sample tests, carry out statistical study, obtain preferably technique sampling parameters;
4) expression of homogeneity: according to step 3) in sampling parameters sample, according to step 2) method detect, the reinforced homogeneity that applies of throwing is according to following formulae discovery:
Wherein:
CU-feeding homogeneity, %;
X
ithe content of mark in-the i-th sample, mg/kg;
the mean value of mark content in-sample, mg/kg;
The sampling number of times of n-sample;
The size reflection cigarette charging degree of uniformity of CU value, CU value is larger, and feeding homogeneity is better.
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