CN112924596A - Method for measuring cut tobacco stem rate of cigarette based on nicotine content - Google Patents
Method for measuring cut tobacco stem rate of cigarette based on nicotine content Download PDFInfo
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- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 title claims abstract description 74
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- 238000002156 mixing Methods 0.000 claims description 36
- 238000000605 extraction Methods 0.000 claims description 31
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- 238000004949 mass spectrometry Methods 0.000 claims description 7
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- QUMXDOLUJCHOAY-UHFFFAOYSA-N alpha-methylbenzyl acetate Natural products CC(=O)OC(C)C1=CC=CC=C1 QUMXDOLUJCHOAY-UHFFFAOYSA-N 0.000 description 1
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- ZMRUPTIKESYGQW-UHFFFAOYSA-N propranolol hydrochloride Chemical compound [H+].[Cl-].C1=CC=C2C(OCC(O)CNC(C)C)=CC=CC2=C1 ZMRUPTIKESYGQW-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides a method for measuring cut tobacco stem rate of cigarettes based on nicotine content, which comprises the following steps: the method comprises the steps of balancing cigarette tobacco in a cigarette sample, crushing and sieving to obtain tobacco powder, adding a solvent and an internal standard solution to perform microwave-assisted extraction to obtain a sample solution, measuring the sample solution by adopting a gas chromatography-mass spectrometry method to determine the chromatographic peak area ratio of nicotine/internal standard substance in the sample solution, and determining the cigarette cut stem rate in the cigarette sample according to the linear relation between the chromatographic peak area ratio of nicotine/internal standard substance and the cigarette cut stem rate. According to the method for measuring the cut stem rate of the cigarette based on the nicotine content, the cut stem rate of the cigarette is quantitatively researched by an accurate detection means through analysis of different chemical components nicotine in cut leaves and cut stems, accurate prediction of the cut stem rate of the cigarette and quantitative evaluation of the distribution uniformity of the cut stems in the cigarette are realized, and a scientific reference means is provided for fine control and process evaluation of cigarette production.
Description
Technical Field
The invention belongs to the technical field of cigarette testing, and relates to a method for measuring cut tobacco stem rate of cigarettes based on nicotine content.
Background
The refined production of the cigarettes is the key work content of the tobacco industry, the tobacco leaf group formula uses the cut tobacco, the cut stems and the cut sheets, and the mixing of the tobacco raw materials actually achieves the uniformity of various chemical components through the mixing of physical components, thereby ensuring the sensory quality uniformity of the smoking evaluation of consumers. In various blending substances, the blending proportion of the cut stems is higher, so that the cut stem rate of the cigarettes is accurately predicted, the uniformity of the cut stem distribution among the cigarettes can be objectively and accurately evaluated, and the method has important significance for controlling the stability of the internal quality of cigarette products including sensory quality.
Through comprehensive literature research, the situation that the cut stems in cigarettes are not uniformly distributed and have a large difference with the cut stem blending theoretical proportion often occurs when a small proportion of cut stems are blended in a cigarette formula, so that the inherent quality of cigarettes in the same batch is unstable, and the sensory quality of cigarettes is influenced. Therefore, the uniform ratio of the cut stems is crucial to the stable quality of cigarettes. At present, no unified standard exists for measuring and evaluating the blending uniformity of the cut tobacco at home and abroad. The traditional method is mainly used for evaluating the uniformity degree of tobacco shred blending from the aspects of physical density, tobacco chemical characteristic value, smoke chemistry and the like, and the method has the defects of low precision, complex processing process and large error and can not scientifically and efficiently reflect the actual tobacco shred blending uniformity. Therefore, a more accurate, efficient, green and highly operable method for evaluating the blending uniformity of the cut tobacco is needed to be established. Research finds that some reports are provided in the aspect of evaluating the blending uniformity of cut stems in cut tobacco in recent years, and the research objects are mainly finished cut tobacco after blending and are less related to the distribution uniformity of the cut stems of cigarettes.
The invention patent with the application number of 201310067515.9 discloses a method for measuring blending uniformity of reconstituted cut stems. The method comprises the steps of drying and weighing the reconstituted cut stems, cut leaves, samples to be detected and a sample box, drying and weighing after soaking, and establishing a blending proportion and loss rate curve through multiple groups of measurement, so that the blending uniformity of the reconstituted cut stems is measured.
The invention patent with application number 201210324792.9 discloses a method for measuring the ratio of cut stems in cut tobacco. Separating the cut stems from the cut tobacco by adopting an organic solvent through density difference, drying and weighing the cut stems, and calculating the proportion of the cut stems in the cut tobacco. The method is simple to operate, and provides a feasible method for determining the ratio of the cut stems in the cut tobacco.
The invention patent with application number 201310169230.6 discloses a method for characterizing blending uniformity of cut leaves, expanded cut stems and cut stems. The method comprises the steps of preparing standard samples of mixed cut tobaccos with different blending ratios, measuring filling values and shredding rates of the mixed cut tobaccos, correlating the blending ratios, the filling values and the shredding rates, establishing a mathematical model by adopting a multiple linear regression method, measuring the filling values and the shredding rates of the mixed cut tobaccos to be measured, predicting the blending ratios according to the mathematical model, and further representing the uniformity of the blended cut tobaccos. The method is simple and easy to operate, low in cost, accurate and rapid.
The invention patent with application number 201811098249.5 discloses a method for rapidly estimating the cut stem real-doped proportion of cut tobacco in cigarettes. The potassium and chlorine contents in the mixed material are calculated by measuring the potassium and chlorine contents in the cut tobacco and the cut tobacco, the actual proportion of the cut tobacco in the cut tobacco is calculated by accurately measuring the potassium and chlorine contents in the cut tobacco in the cigarette, the reliability is judged, and the average value is taken as the actual proportion of the cut tobacco in the cigarette. The method is simple and quick without modeling.
The invention patent with the application number of 201811097882.2 discloses a method for rapidly determining the mixing proportion of cut stems in running strips. The nicotine and chlorine content in the cut tobacco and the cut stem is obtained through testing, the nicotine and chlorine content in the cut tobacco after blending is calculated according to the blending proportion, the nicotine and chlorine content in the strip running cut is obtained through testing, the actual proportion of the cut stem in the strip running cut is calculated, the reliability is judged, and the average value is used as the actual proportion of the cut stem in the cigarette.
Document 1 (zhongquan, zuoyuan, paoyang, etc., tobacco science and technology, 10 th 2015) reports a blending uniformity evaluation method of microwave expanded cut stems in cigarettes, and realizes comprehensive evaluation of blending uniformity of microwave expanded cut stems in cigarettes from the aspects of mixing uniformity analysis, cigarette density standard deviation method analysis and mainstream smoke moving range analysis 3.
Document 2 (duyiyun, zaitai relay, chenguangping, etc., chemical engineering and equipment, 2010, 5 th) reports a research method for evaluating blending uniformity of cut tobacco by using chemical general indexes, wherein a mathematical model is established by correlating the ratio of cut tobacco, cut stems and cut flakes with basic data of chemical components such as total sugar, total plant alkaloid, chlorine, potassium, total nitrogen and volatile alkali, and the blending uniformity of the cut tobacco, the cut stems and the cut flakes is represented.
The evaluation method of cut stem blending uniformity in the above patents and documents comprises methods of physical and chemical indexes, wherein physical methods such as a flotation method and a weighing method are simple and rapid, but have the problems of low sensitivity, poor accuracy and the like; the methods of chemical characteristic value and flue gas analysis have the defects of complex analysis process, poor operability, difficult reflection of actual blending result only by theoretical calculation, and the like.
Disclosure of Invention
In view of the above disadvantages of the prior art, the present invention aims to provide a method for determining cut stem rate of cigarettes based on nicotine content, so as to achieve scientific and accurate determination of cut stem rate of finished cigarettes and rapid evaluation of cut stem distribution uniformity in cigarettes, and provide scientific basis for accurately determining quality stability of finished cigarettes.
In order to achieve the above objects and other related objects, the present invention provides a method for determining cut tobacco rod rate of cigarette based on nicotine content, comprising: the method comprises the steps of balancing cigarette tobacco in a cigarette sample, crushing and sieving to obtain tobacco powder, adding a solvent and an internal standard solution to perform microwave-assisted extraction to obtain a sample solution, measuring the sample solution by adopting a gas chromatography-mass spectrometry method to determine the chromatographic peak area ratio of nicotine/internal standard substance in the sample solution, and determining the cigarette cut stem rate in the cigarette sample according to the linear relation between the chromatographic peak area ratio of nicotine/internal standard substance and the cigarette cut stem rate.
Preferably, the tobacco shreds in the cigarette sample are obtained by cutting and stripping the cigarette paper of each cigarette along the central line.
Preferably, the temperature of the equilibrium is (22 + -1) ° c, the relative humidity of the equilibrium is (60 + -3)%, and the time of the equilibrium is (48 + -1) h.
Preferably, the pulverization is to grind into powder by using a grinder.
Preferably, the screen is a standard screen passing through 38-42 meshes. Preferably, the standard sieve has a mesh number of 40.
Preferably, the sieved powder sample is sealed and stored in a dark place.
Preferably, the solvent is methanol.
Preferably, the internal standard solution is a methanol solution of phenethylacetate.
Preferably, the methanol solution of phenethyl acetate is 30-50mg/mL methanol solution of phenethyl acetate. More preferably, the methanol solution of phenethyl acetate is a methanol solution of 40mg/mL phenethyl acetate.
Preferably, the ratio of the added mass of the tobacco shred powder to the added volume of the solvent is 0.2:5-15 g/mL. More preferably, the ratio of the mass of added tobacco powder to the volume of solvent added is 0.2:10, g/mL.
Preferably, the ratio of the added mass of the tobacco shred powder to the added volume of the internal standard solution is 0.2:0.05-0.15 g/mL. More preferably, the ratio of the added mass of the tobacco shred powder to the added volume of the internal standard solution is 0.2:0.1, g/mL.
Preferably, the extraction conditions of the microwave-assisted extraction are as follows: the extraction power is 750-850W, the extraction temperature is 90-110 ℃, and the extraction time is 15-25 min. Preferably, the extraction conditions of the microwave-assisted extraction are: the extraction power is 800W, the extraction temperature is 100 ℃, and the extraction time is 20 min.
Preferably, the obtained sample solution is cooled after the microwave-assisted extraction, and the supernatant is filtered and placed in the dark for later use.
Preferably, the cooling is to room temperature and left to stand. The room temperature is 20-30 ℃.
Preferably, the filtration is filter membrane filtration, the filter membrane being a 0.22 μm organic filter membrane.
Preferably, the determination by gas chromatography-mass spectrometry comprises the following steps:
1) preparing a cut stem reference standard solution: respectively balancing cigarette leaf shreds and stem shreds, crushing and sieving, adding stem shred powder into the leaf shred powder, mixing to obtain tobacco shred powder, adding a solvent and an internal standard solution, and performing microwave-assisted extraction to obtain a stem shred reference standard solution with known cigarette stem shred rate;
2) sample detection: respectively detecting the cut stem reference standard solution and the sample solution by adopting a gas chromatography-mass spectrometry, comparing the retention time for qualitative determination, quantifying by adopting an internal standard curve method, determining the chromatographic peak area ratio of nicotine/internal standard substance in the cut stem reference standard solution and the sample solution, and determining the cut stem rate of the cigarette in the sample solution according to the linear relation between the chromatographic peak area ratio of nicotine/internal standard substance in the cut stem reference standard solution and the cut stem rate of the cigarette.
Preferably, in step 1), the temperature of the equilibrium is (22 ± 1) ° c, the relative humidity of the equilibrium is (60 ± 3)%, and the time of the equilibrium is (48 ± 1) h.
Preferably, in step 1), the pulverization is to be ground into powder by using a grinder.
Preferably, in step 1), the screening is 38-42 mesh standard screening. More preferably, the standard sieve has a mesh number of 40.
Preferably, in the step 1), the cut stem rate of the cigarette ranges from 17 ± 5%. The cut stem rate of the cigarette is the percentage of the mass of cut stems in each cigarette to the mass of cut tobacco.
Preferably, in the step 1), the adding quality of the cut stems in the plurality of cut tobacco powders is gradually increased by 1% according to the range of the cut stem rate of the cigarette.
Preferably, in the step 1), the mixing is to sufficiently shake the cut leaf powder and the cut stem powder until the mixture is uniform.
Preferably, in the step 1), the mixed tobacco shred powder is sealed and stored in dark place.
Preferably, in step 1), the solvent is methanol.
Preferably, in step 1), the internal standard solution is a methanol solution of phenylethyl acetate. The tobacco does not contain phenethyl acetate.
Preferably, the methanol solution of phenethyl acetate is 30-50mg/mL methanol solution of phenethyl acetate. More preferably, the methanol solution of phenethyl acetate is a methanol solution of 40mg/mL phenethyl acetate.
Preferably, in the step 1), the ratio of the added mass of the cut tobacco powder to the added volume of the solvent is 0.2:5-15 g/mL. More preferably, the ratio of the mass of added tobacco powder to the volume of solvent added is 0.2:10, g/mL.
Preferably, in the step 1), the ratio of the added mass of the cut tobacco powder to the added volume of the internal standard solution is 0.2:0.05-0.15 g/mL. More preferably, the ratio of the added mass of the tobacco shred powder to the added volume of the internal standard solution is 0.2:0.1, g/mL.
Preferably, in step 1), the extraction conditions of the microwave-assisted extraction are as follows: the extraction power is 750-850W, the extraction temperature is 90-110 ℃, and the extraction time is 15-25 min. Preferably, the extraction conditions of the microwave-assisted extraction are: the extraction power is 800W, the extraction temperature is 100 ℃, and the extraction time is 20 min.
More preferably, the sample solution obtained after the microwave-assisted extraction is cooled, and the supernatant is filtered and placed in the dark for use.
More preferably, the cooling is to room temperature and left to stand. The room temperature is 20-30 ℃.
More preferably, the filtration is a filter membrane filtration, the filter membrane being a 0.22 μm organic filter membrane.
Preferably, in step 2), in the gas chromatography-mass spectrometry, the determination conditions of the gas chromatography are as follows:
a chromatographic column: HP-5MS capillary chromatography column (30m x 0.25mm id x 0.25 μm df); sample inlet temperature: 270 ℃ and 290 ℃, preferably 280 ℃; sample introduction amount: 1.0-10.0 μ L, preferably 1.0 μ L; carrier gas: high-purity helium, wherein the purity of carrier gas is more than or equal to 99.999 percent; flow rate of carrier gas: constant flow rate of 0.5-1.5ml/min, preferably 1.0 ml/min; the split ratio is as follows: 90-110: 1, preferably 100: 1.
preferably, in step 2), in the gas chromatography-mass spectrometry, the temperature rise program of the gas chromatography is as follows: the initial temperature is kept at 55-65 ℃ for 1-3min, and the temperature is increased to 270-290 ℃ at the rate of 7-9 ℃/min and kept for 7-9 min.
More preferably, the temperature-raising program of the gas chromatograph is: the initial temperature was maintained at 60 ℃ for 2min and increased to 280 ℃ at a rate of 8 ℃/min for 8 min.
Preferably, in step 2), in the gas chromatography-mass spectrometry, the determination conditions of the mass spectrum are as follows:
an ionization mode: an Electron Impact (EI) ion source; ionization energy: 70 eV; ion source temperature: 225 ℃ and 235 ℃, preferably 230 ℃; quadrupole temperature: 145-155 ℃, preferably 150 ℃; transmission line temperature: 275 ℃ and 285 ℃, preferably 280 ℃; solvent retardation: 3-5min, preferably 4 min; the scanning mode is as follows: full scan (TIC) qualitative, Selective Ion Monitoring (SIM) quantitative.
More preferably, the quantitative ions selected in the mass spectrometry assay are: nicotine 84.1, internal standard 91.0; the auxiliary quantitative ions selected in the mass spectrometry are respectively as follows: nicotine 133.1, internal standard 104.0.
Preferably, in step 2), the internal standard curve method comprises the following steps:
A) preparing a series of cut stem reference standard solutions with different cut stem rates of cigarettes according to the step 1), respectively carrying out GC-MS detection to obtain a linear relation between a chromatographic peak area ratio of nicotine/internal standard substance and the cut stem rate of the corresponding cigarettes, drawing a corresponding standard working curve, and calculating to obtain a regression equation of the standard working curve of the cut stem reference standard solution;
B) and C, carrying out GC-MS detection on the sample solution, substituting the chromatographic peak area ratio of nicotine/internal standard substance in the obtained sample solution into the regression equation of the standard working curve of the cut stem reference standard solution in the step A), and calculating to obtain the cut stem rate of the cigarette in the sample solution.
More preferably, in the standard working curve, the ratio of the chromatographic peak area of nicotine to the chromatographic peak area of the internal standard is taken as the ordinate (Y axis), and the cut-to-tobacco ratio of the corresponding cigarette is taken as the abscissa (X axis).
The mechanism that the chromatographic peak area ratio of the nicotine/internal standard substance and the cut tobacco stem rate have a linear relation is as follows: the difference of the nicotine content of the cut stems and the cut tobacco of the cigarettes is large, and the proportion is stable, so that the nicotine content in the cut tobacco with a specific cut stem rate of the cigarettes is stable; in the tobacco shreds of cigarettes with different cut stem rates, the contents of the cut stems and the tobacco shreds are changed in a linear proportion, namely, the nicotine content is changed in a proportion along with the change of the cut stem rate of the cigarettes, so that the cut stem rate of the cigarettes is in a linear relation with the nicotine content; and the nicotine content and the chromatographic peak area ratio of the nicotine/internal standard substance have a linear relation, so that the chromatographic peak area ratio of the nicotine/internal standard substance and the cut tobacco stem rate have a linear relation.
As described above, the method for measuring cut stem rate of cigarette based on nicotine content provided by the invention has the following beneficial effects:
(1) according to the method for measuring the cut stem rate of the cigarette based on the nicotine content, provided by the invention, the cut stem rate of the cigarette is directly taken as the horizontal coordinate, the ratio of the peak area of nicotine and the internal standard is taken as the vertical coordinate, a standard working curve is established, a nicotine standard product is not needed, only the nicotine characteristic values of tobacco samples with different cut stem rates of the cigarette blended manually are measured, and the error in the detection process is further reduced.
(2) According to the method for measuring the cut tobacco stem rate of the cigarette based on the nicotine content, the cut tobacco stems in the powder state are mixed, the physical state uniformity of substances to be mixed is guaranteed, the uniform mixing degree is improved, and the prediction precision of a standard working curve is improved.
(3) According to the method for measuring the cut stem rate of the cigarette based on the nicotine content, the weighed sample amount can be equivalent to the quality of cut tobacco in one cigarette, so that the representativeness of a total sample is ensured, and the accuracy of quantitative analysis is also met.
(4) According to the method for measuring the cut tobacco stem rate of the cigarette based on the nicotine content, microwave-assisted extraction is adopted for pretreatment, the extraction efficiency is high, and the extraction operation process is simple and rapid.
(5) The method for measuring the cut stem rate of the cigarette based on the nicotine content adopts GC-MS detection and SIM qualitative detection, the obtained spectrogram base line is stable, the integral is accurate, the deviation caused by the instrument precision is far smaller than the deviation of the uneven degree among samples, and the quantitative detection result is accurate.
(6) According to the method for measuring the cut stem rate of the cigarette based on the nicotine content, the standard working curve of the cut stem rate and the nicotine characteristic value of different cigarettes in the cut tobacco is established for the first time and is used for analyzing the cut stem rate of the finished cigarette, so that the uniformity of the distribution of the cut stems of the cigarettes is reflected, and the result is objective and accurate compared with the simple theoretical calculation.
(7) The method for measuring the cut stem rate of the cigarette based on the nicotine content is systematic, objective and scientific, is simple to operate, saves time, has good reproducibility and low detection limit, has strong practicability, has very important significance for evaluating the product quality and the stability of a cut tobacco making process, and can provide important technical support for fine control of cigarette production.
(8) The method for measuring the cut stem rate of the cigarette based on the nicotine content is convenient to operate, simple in quantification, accurate and effective, and capable of achieving accurate prediction of the cut stem rate of the cigarette and quantitative evaluation of the distribution uniformity of the cut stems in the cigarette by analyzing different chemical components nicotine in cut leaves and cut stems and utilizing an accurate detection means to quantitatively research the cut stem rate of the cigarette, and providing a scientific reference means for fine control and process evaluation of cigarette production.
Drawings
Figure 1 shows a standard working curve of the ratio of cut-stem percentage of a cigarette to the peak area of nicotine/internal standard in the present invention.
FIG. 2 is a histogram showing the cut tobacco percentage distribution of an actual cigarette sample according to the present invention.
Detailed Description
The present invention is further illustrated below with reference to specific examples, which are intended to be illustrative only and not to limit the scope of the invention.
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
The reagents and equipment used in the following examples are as follows:
1. reagent
Cut tobacco (100% purity, manufactured by Tianjin cigarette factory), cut stem (100% purity, manufactured by Tianjin cigarette factory), methanol (chromatographically pure, Germany Merck), phenethyl acetate (analytically pure, manufactured by Kemi Europe corporation) and ultrapure water (manufactured by ultrapure water instrument).
2. Instrument for measuring the position of a moving object
7890B-5975C gas chromatography mass spectrometer (Agilent, USA); HP-5MS capillary chromatography column (Agilent, USA); ZM200 mill (Retsch, germany); CEM microwave extractors Matthews, NC, USA); 0.22 μm organic phase filter membrane, disposable syringe (Shanghai Anpu experiment science and technology Co., Ltd.); glassware of various sizes (witeg, germany); Milli-Q ultra pure water instruments (Millipore, USA); an XS204 electronic balance (0.0001g, Mettler, Switzerland); organic phase filtration membrane (nylon, 0.22 μm, Shanghai' an spectrum).
Example 1
1. Preparation of sample solution
Randomly drawing 1 brand A cigarette, counting 200 cigarettes in total, and cutting the cigarette paper of each cigarette along the central line and stripping to obtain the cut tobacco. All the cut tobacco of each cigarette is independently placed in a sample box and balanced for 48 hours in a constant temperature and humidity environment with the temperature of 22 ℃ and the relative humidity of 60 percent. Fully grinding the cut tobacco into powder in a glass mortar by a grinder, sieving the powder by a 40-mesh standard sieve, placing the powder in a brown bottle, and sealing and storing the bottle in dark.
Then accurately weighing 0.2000g of the tobacco shred powder obtained above, placing the tobacco shred powder in a microwave digestion tank, adding a solvent: 10mL of methanol, and the internal standard solution added: 100 μ L of 40mg/mL phenethylacetate in methanol. Placing the microwave digestion tank in a microwave extraction instrument for microwave-assisted extraction, wherein the extraction conditions of the microwave-assisted extraction are as follows: the extraction power is 800W, the extraction temperature is 100 ℃, and the extraction time is 20 min.
After extraction, cooling to room temperature and standing, taking supernatant, filtering with 0.22 μm organic filter membrane to obtain sample solution # 1, placing in brown chromatographic bottle, and analyzing by GC-MS.
2. Preparation of cut stem reference standard solution
Respectively selecting 5 batches of cut leaf samples and cut stem samples, sampling 5kg of each sample in a continuous production state, respectively placing 10 parts of total samples in sample boxes, and balancing for 48 hours in a constant-temperature and constant-humidity environment with the temperature of 22 ℃ and the relative humidity of 60%. Fully grinding the cut leaves and the cut stems into powder in a glass mortar by a grinder, and sieving the powder by a standard sieve of 40 meshes to obtain cut leaf powder and cut stem powder. Adding a series of cut stem powder with different proportions into the cut leaf powder, fully oscillating until uniformly mixing to obtain cut tobacco powder, placing in a brown bottle, and sealing and storing in dark. Calculating the actual tobacco shred ratio in the tobacco shred powder, wherein each sample contains 50g of leaf shreds and stem shreds in total, setting the blending proportion range and gradient, the range of the tobacco shred ratio is 17 +/-5%, the adding quality of the stem shreds is gradually increased by 1% gradient according to the range of the tobacco shred ratio, and obtaining a series of tobacco shred powders with known tobacco shred ratios, wherein the blending condition of the specific stem shreds is shown in table 1.
TABLE 1 tobacco shred powder sample blending data table of different tobacco shred cut rate
Then accurately weighing a series of 0.2000g of the obtained tobacco shred powder in a microwave digestion tank, adding a solvent: 10mL of methanol, and the internal standard solution added: 100 μ L of 40mg/mL phenethylacetate in methanol. Placing the microwave digestion tank in a microwave extraction instrument for microwave-assisted extraction, wherein the extraction conditions of the microwave-assisted extraction are as follows: the extraction power is 800W, the extraction temperature is 100 ℃, and the extraction time is 20 min.
And after extraction is finished, cooling to room temperature and standing, taking supernatant, filtering with a 0.22-micrometer organic filter membrane to obtain a series of cut stem reference standard solutions with known cut stem rate of the cigarettes, placing in a brown chromatographic bottle, and performing GC-MS analysis.
3. Measurement of
And respectively detecting the cut stem reference standard solution and the sample solution No. 1 by adopting a gas chromatography-mass spectrometry method, comparing retention time for qualitative determination, and quantifying by adopting an internal standard curve method. Firstly, performing GC-MS detection on a series of cut stem reference standard solutions with different cut stem rates of cigarettes respectively to obtain a linear relation between a chromatographic peak area ratio of nicotine/internal standard substance and the cut stem rate of the corresponding cigarette, drawing a corresponding standard working curve, and calculating to obtain a regression equation of the standard working curve of the cut stem reference standard solution. And performing GC-MS detection on the sample solution 1#, substituting the chromatographic peak area ratio of nicotine/internal standard substance in the obtained sample solution 1#, into a regression equation of a standard working curve of the cut stem reference standard solution, calculating the cut stem rate of the cigarette in the sample solution 1#, and evaluating the distribution uniformity according to the known cut stem rate of the cigarette in the cut stem reference standard solution. In the standard working curve, the ratio of the chromatographic peak area of nicotine to the chromatographic peak area of the internal standard is taken as the ordinate (Y axis), and the cut stem rate of the corresponding cigarette is taken as the abscissa (X axis).
Wherein, the measuring conditions of the gas chromatography are as follows: a chromatographic column: HP-5MS capillary chromatography column (30m x 0.25mm id x 0.25 μm df); sample inlet temperature: 280 ℃; sample introduction amount: 1.0 μ L; carrier gas: high-purity helium, wherein the purity of carrier gas is more than or equal to 99.999 percent; flow rate of carrier gas: constant flow rate, 1.0 ml/min; the split ratio is as follows: 100: 1; temperature rising procedure: the initial temperature was maintained at 60 ℃ for 2min and increased to 280 ℃ at a rate of 8 ℃/min for 8 min.
The mass spectrum measurement conditions were: an ionization mode: an Electron Impact (EI) ion source; ionization energy: 70 eV; ion source temperature: 230 ℃; quadrupole temperature: 150 ℃; transmission line temperature: 280 ℃; solvent retardation: 4 min; the scanning mode is as follows: full scan (TIC) qualitative, Selective Ion Monitoring (SIM) quantitative. The quantitative ions selected in the mass spectrometry were: nicotine 84.1, internal standard 91.0; the auxiliary quantitative ions selected in the mass spectrometry are respectively as follows: nicotine 133.1, internal standard 104.0. The specific data are shown in Table 2.
TABLE 2 characteristic ion selection Table for nicotine and internal standard
Example 2
Respectively carrying out gas chromatography-mass spectrometry analysis on a series of cut stem reference standard solutions with different cut stem rates of cigarettes prepared in the step 2 of the example 1, and establishing a standard working curve by taking the average value of the chromatographic peak area ratios Sr values of 5 nicotine and an internal standard under the same cut stem rate of different batches as a vertical coordinate (Y axis) and the corresponding cut stem rate of the cigarettes as a horizontal coordinate (X axis). It has good linear relation and correlation coefficient R20.99 or more, as shown in Table 3 and FIG. 1.
TABLE 3
Note: y: the Sr value; x: cut stem rate
Example 3
1 part of the prepared sample solution prepared in the step 1 of the example 1 is continuously injected for 10 times for analysis, and the RSD of the Sr value of the chromatographic peak area ratio of nicotine to the internal standard is 1.21 percent and less than 3 percent, which indicates that the precision of the instrument is good. The specific data are shown in Table 4.
Meanwhile, 10 parts of the same batch of samples are weighed in parallel, and sample preparation solutions prepared in the step 1 of the example 1 are subjected to sequential sample injection analysis, so that the RSD of the Sr value of the chromatographic peak area ratio of nicotine to the internal standard is 1.54 percent and less than 5 percent, which indicates that the method has good reproducibility. The specific data are shown in Table 4.
TABLE 4
Example 4
And (3) verifying the standard working curve based on the linear relation between the chromatographic peak area ratio of the nicotine/internal standard substance and the cut stem rate of the corresponding cigarette, which is established in the step 3 in the embodiment 1.
And respectively carrying out internal verification on the sample points of the established curves by utilizing the established working curves. Meanwhile, the established working curves are used for respectively carrying out external verification on 10 laboratory proportioning samples. The absolute deviation and the relative deviation of the predicted value and the actual value of each sample are respectively calculated to verify the prediction effect of the standard working curve, and the results are shown in table 5.
Table 5 verification results
As can be seen from table 5, the internal verification absolute deviation is within 0.25%, and the relative deviation is within 1.32%; the absolute deviation of the external verification is within 0.91%, and the relative deviation is within 4.73%. The prediction result is accurate and reliable.
Example 5
The standard working curve based on the linear relationship between the chromatographic peak area ratio of nicotine/internal standard substance and the cut-tobacco rate of the corresponding cigarette, which is established in step 3 of example 1, is used for predicting the cut-tobacco rate of 200 cigarette samples, and evaluating the distribution uniformity, and the result is shown in fig. 2. As can be seen from FIG. 2, the cut stem rate of the cigarette sample is in relatively obvious normal distribution, with the range of 5.89%, the mean value of 16.98%, and the standard deviation of 1.13%. The result can objectively reflect the stem distribution uniformity of the group of samples, and has very important practical significance for mastering and controlling the quality stability of cigarette products.
In conclusion, the invention provides a systematic, objective and scientific method. Has very important significance for evaluating the product quality and the stability of the silk making process. The method has the advantages of simple operation, time saving, good reproducibility, accurate result and strong practicability. According to the method for measuring the cut stem rate of the cigarette based on the nicotine content, the cut stem rate of the cigarette is quantitatively researched by an accurate detection means through analysis of different chemical components nicotine in cut leaves and cut stems, accurate prediction of the cut stem rate of the cigarette and quantitative evaluation of the distribution uniformity of the cut stems in the cigarette are realized, and a scientific reference means is provided for fine control and process evaluation of cigarette production. Therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. A method for measuring cut tobacco stems rate based on nicotine content comprises the following steps: the method comprises the steps of balancing cigarette tobacco in a cigarette sample, crushing and sieving to obtain tobacco powder, adding a solvent and an internal standard solution to perform microwave-assisted extraction to obtain a sample solution, measuring the sample solution by adopting a gas chromatography-mass spectrometry method to determine the chromatographic peak area ratio of nicotine/internal standard substance in the sample solution, and determining the cigarette cut stem rate in the cigarette sample according to the linear relation between the chromatographic peak area ratio of nicotine/internal standard substance and the cigarette cut stem rate.
2. The method for measuring the cut stem rate of cigarettes based on the nicotine content as claimed in claim 1, wherein the equilibrium temperature is 21-23 ℃, the equilibrium relative humidity is 57-63%, and the equilibrium time is 47-49 h.
3. The method for measuring cut rolled tobacco stems rate based on nicotine content according to claim 1, wherein the solvent is methanol; the ratio of the added mass of the tobacco shred powder to the added volume of the solvent is 0.2:5-15 g/mL.
4. The method for measuring cut rolled tobacco stems based on nicotine content according to claim 1, wherein the internal standard solution is a methanol solution of phenethylacetate; the ratio of the added mass of the tobacco shred powder to the added volume of the internal standard solution is 0.2:0.05-0.15 g/mL.
5. The method for measuring the cut stem rate of cigarettes based on the nicotine content as claimed in claim 1, wherein the microwave-assisted extraction conditions are as follows: the extraction power is 750-850W, the extraction temperature is 90-110 ℃, and the extraction time is 15-25 min.
6. The method for measuring cut rolled tobacco stems rate based on nicotine content according to claim 1, wherein the measurement by gas chromatography-mass spectrometry comprises the following steps:
1) preparing a cut stem reference standard solution: respectively balancing cigarette leaf shreds and stem shreds, pulverizing, sieving, adding stem shred powder into the leaf shred powder, mixing to obtain tobacco shred powder, adding solvent and internal standard solution, performing microwave-assisted extraction to obtain stem shred reference standard solution with known cigarette stem shred rate
2) Sample detection: respectively detecting the cut stem reference standard solution and the sample solution by adopting a gas chromatography-mass spectrometry, comparing the retention time for qualitative determination, quantifying by adopting an internal standard curve method, determining the chromatographic peak area ratio of nicotine/internal standard substance in the cut stem reference standard solution and the sample solution, and determining the cut stem rate of the cigarette in the sample solution according to the linear relation between the chromatographic peak area ratio of nicotine/internal standard substance in the cut stem reference standard solution and the cut stem rate of the cigarette.
7. The method for measuring cut rolled tobacco stems based on nicotine content according to claim 6, wherein in the step 2), in the gas chromatography-mass spectrometry, the measurement conditions of the gas chromatography are as follows:
a chromatographic column: HP-5MS capillary chromatography column, 30m × 0.25mm id × 0.25 μm df; sample inlet temperature: 270 ℃ and 290 ℃; sample introduction amount: 1.0-10.0 μ L; carrier gas: high-purity helium, wherein the purity of carrier gas is more than or equal to 99.999 percent; flow rate of carrier gas: constant flow rate of 0.5-1.5 ml/min; the split ratio is as follows: 90-110: 1.
8. the method for measuring cut rolled tobacco stems based on nicotine content according to claim 6, wherein in the step 2), in the gas chromatography-mass spectrometry, the temperature rise program of the gas chromatography is as follows: the initial temperature is kept at 55-65 ℃ for 1-3min, and the temperature is increased to 270-290 ℃ at the rate of 7-9 ℃/min and kept for 7-9 min.
9. The method for measuring cut rolled tobacco stems based on nicotine content according to claim 6, wherein in the step 2), in the gas chromatography-mass spectrometry, the measurement conditions of the mass spectrometry are as follows:
an ionization mode: electron bombardment ion source; ionization energy: 70 eV; ion source temperature: 225 ℃ and 235 ℃; quadrupole temperature: 145-155 ℃; transmission line temperature: 275 ℃ and 285 ℃; solvent retardation: 3-5 min; the scanning mode is as follows: full scan TIC qualitative, selective ion monitoring SIM quantitative.
10. The method for measuring cut tobacco stems rate based on nicotine content according to claim 9, wherein the quantitative ions selected in the mass spectrometry are: nicotine 84.1, internal standard 91.0; the auxiliary quantitative ions selected in the mass spectrometry are respectively as follows: nicotine 133.1, internal standard 104.0.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114609006A (en) * | 2022-03-10 | 2022-06-10 | 安徽中烟工业有限责任公司 | Characterization method for tobacco leaf and tobacco shred crushing in cigarette processing process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012075950A1 (en) * | 2010-12-08 | 2012-06-14 | 广东中烟工业有限责任公司 | Method for rapidly determining 16 species of inorganic anions and organic acids in tobacco simultaneously |
| CN109297854A (en) * | 2018-09-20 | 2019-02-01 | 云南中烟工业有限责任公司 | A kind of stem run in item silk mixes the rapid assay methods of ratio in fact |
| CN111521716A (en) * | 2020-06-09 | 2020-08-11 | 甘肃烟草工业有限责任公司 | Cigarette raw material mixing uniformity evaluation method based on design value |
| CN111610276A (en) * | 2020-06-09 | 2020-09-01 | 甘肃烟草工业有限责任公司 | Cigarette raw material mixing proportion distribution measuring method based on tobacco characteristic components |
-
2021
- 2021-01-27 CN CN202110112158.8A patent/CN112924596A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012075950A1 (en) * | 2010-12-08 | 2012-06-14 | 广东中烟工业有限责任公司 | Method for rapidly determining 16 species of inorganic anions and organic acids in tobacco simultaneously |
| CN109297854A (en) * | 2018-09-20 | 2019-02-01 | 云南中烟工业有限责任公司 | A kind of stem run in item silk mixes the rapid assay methods of ratio in fact |
| CN111521716A (en) * | 2020-06-09 | 2020-08-11 | 甘肃烟草工业有限责任公司 | Cigarette raw material mixing uniformity evaluation method based on design value |
| CN111610276A (en) * | 2020-06-09 | 2020-09-01 | 甘肃烟草工业有限责任公司 | Cigarette raw material mixing proportion distribution measuring method based on tobacco characteristic components |
Non-Patent Citations (4)
| Title |
|---|
| 刘帅东等: "基于均匀试验设计的常规化学成分与掺配比例相关性研究", 《河南科技》 * |
| 匡添等: "莫合烟中烟碱的提取工艺筛选", 《新疆医科大学学报》 * |
| 谭新良等: "烟叶挥发性成分的热脱附-气相色谱-质谱内标分析法研究", 《湖南师范大学自然科学学报》 * |
| 马立超等: "加速溶剂萃取-气相色谱-串联质谱法检测烟草中生物碱", 《分析试验室》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114609006A (en) * | 2022-03-10 | 2022-06-10 | 安徽中烟工业有限责任公司 | Characterization method for tobacco leaf and tobacco shred crushing in cigarette processing process |
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