CN111060546A - Cigarette moisture retention performance evaluation method based on low-field nuclear magnetic resonance technology - Google Patents
Cigarette moisture retention performance evaluation method based on low-field nuclear magnetic resonance technology Download PDFInfo
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Abstract
The invention relates to a cigarette moisture retention performance evaluation method based on a low-field nuclear magnetic resonance technology. The evaluation method comprises the following steps: balancing the two groups of tobacco shred samples to obtain two groups of tobacco shred samples to be detected; then, the low-field nuclear magnetic resonance technology is utilized to determine the sample signal values of the two groups of tobacco shred samples, and the T is compared according to the inversion signals21Size of (D), T21Smaller tobacco shred sample has better moisture retention performance than T21Higher tobacco samples. The method utilizes the low-field nuclear magnetic resonance technology to evaluate the moisture retention performance of the cigarettes, is simple and convenient to operate, consumes short time, and can quickly and effectively achieve the purpose of evaluating the moisture retention performance; the nondestructive testing device has the advantages of nondestructive testing, avoids waste and pollution of raw materials, reduces material loss in the development process, reduces research and development cost and improves working efficiency.
Description
Technical Field
The invention belongs to the field of tobacco, and particularly relates to a cigarette moisture retention performance evaluation method based on a low-field nuclear magnetic resonance technology.
Background
The moisture retention performance of tobacco, namely the water retention capacity of tobacco, has important influence on the quality of cigarettes. The main objectives of tobacco moisture-retention research are to improve the smoking comfort of cigarettes and to improve the moisture-retention and moisture-proof performance of cigarette products under different climatic conditions. Currently, cigarette moisture retention technologies are mainly divided into two categories: firstly, the physical moisture retention is also called as tobacco shred moisture retention: the water binding capacity of the tobacco shreds is improved mainly by adding polyhydroxy chemical substances such as propylene glycol, polysaccharide and the like; and secondly, the water holding capacity of the cut tobacco is changed by changing the internal porous structure of the cut tobacco, such as a drying mode, a tabletting method and the like. Second, chemical moisture retention, also called smoke moisture retention: the method comprises two aspects, on one hand, the moisture of the cigarette smoke is increased by adjusting the moisture of the main stream smoke; on the other hand, the stimulation of smoke to the throat and the oral cavity is improved, and the feeling of promoting the secretion of saliva is improved, so that the smoking comfort of the cigarettes is improved.
In recent years, low-field nuclear magnetic resonance (LF-NMR) technology has been widely used in the food field for detecting moisture distribution and fat content, mainly by measuring hydrogen nuclei in a substance under the action of a magnetic field and a radio frequency signalThe transverse and longitudinal relaxation times of the material to study the distribution, migration, water content and other properties associated therewith of moisture within the material. By analysis of T2The difference in relaxation times makes it easier to distinguish between a loss of free flow and a tight association of moisture by physical and chemical actions. T of tobacco material2The inversion spectrogram usually presents 3-4 peaks, wherein T21(0-1 ms) a bound water region based on chemical adsorption; t is22(1-10 ms) a semi-bonded water zone mainly based on capillary adsorption; t is23(10-100 ms) is followed by a free water zone with poor binding capacity. The relaxation time is short, and the binding capacity is strong. Transverse relaxation time T of sample2The longer the length, the greater the freedom of hydrogen nuclei, the less the constraints imposed on the environment, and the easier it is to remove water. Otherwise, T2The shorter, the more strongly bound the hydrogen nuclei are to the substance, the more difficult the hydrogen nuclei are to be removed.
The physical moisture retention technology is a hot research of the current cigarette moisture retention technology, and mainly relates to the research of cigarette humectants. The evaluation on the moisture retention performance mainly focuses on measuring the equilibrium moisture content under different humidity environments by using methods such as an oven method, a sulfuric acid drying method and the like, and the methods are complex to operate, long in time consumption and difficult to quickly and accurately reflect the moisture retention performance of the cigarettes. A method for evaluating the moisture retention performance of cigarette (application number: 201710812269.3) discloses a method for evaluating the moisture retention performance by utilizing the relation between water activity and temperature, which mainly aims at the evaluation of the moisture retention performance of tobacco shreds mixed with stems and does not relate to the evaluation of the moisture retention performance of a humectant. The research on the evaluation of the moisture retention performance of the cigarettes by the low-field nuclear magnetic technology is not many, and the research is mostly focused on the measurement of the moisture content of the tobacco by the low-field nuclear magnetic technology. A tobacco water content testing method (application number: 201610863636.8) based on time domain nuclear magnetic resonance inversion peak area discloses a tobacco water content testing method based on time domain nuclear magnetic resonance inversion peak area, and does not relate to the evaluation method research of moisture retention performance. The method for measuring the moisture content of the tobacco by low-field nuclear magnetic resonance (application number: 201410083463.9) also only discloses a method for testing the moisture content of the tobacco, and does not relate to the moisture retention performance evaluation.
Therefore, the method for evaluating the moisture retention performance of the tobacco, which is simple to operate and high in reliability, has important research significance and application value.
Disclosure of Invention
The invention aims to overcome the defects or shortcomings of complex operation, long period, large tobacco consumption and the like in the prior art, and provides a cigarette moisture retention performance evaluation method based on a low-field nuclear magnetic resonance technology. The method utilizes the low-field nuclear magnetic resonance technology to evaluate the moisture retention performance of the cigarettes, is simple and convenient to operate, consumes short time, and can quickly and effectively achieve the purpose of evaluating the moisture retention performance; the nondestructive testing device has the advantages of nondestructive testing, avoids waste and pollution of raw materials, reduces material loss in the development process, reduces research and development cost and improves working efficiency.
In order to achieve the purpose, the invention adopts the following technical scheme:
a cigarette moisture retention performance evaluation method based on a low-field nuclear magnetic resonance technology comprises the following steps:
s1, balancing a tobacco shred sample for the first time under a relative humidity A and a temperature B;
s2, respectively preparing humectant samples added with humectants from partial tobacco shreds in the balanced tobacco shred samples, and
a control sample with water added;
s3, balancing the humectant sample and the control sample in the S2 for the second time at the relative humidity A and the temperature B;
s4, respectively drying the humectant sample and the control sample until the water content is 12 +/-1%;
s5, balancing the dried humectant sample and the dried control sample at the relative humidity A and the relative temperature B for the third time, wherein the balancing time is more than 48 hours, so as to obtain a tobacco shred sample to be measured;
s6, measuring the sample signal values of the humectant sample and the control sample by using a low-field nuclear magnetic resonance spectrometer, and comparing the T of different humectant samples according to the inversion signal21Value size, T21The humectant samples with lower values had better humectant properties.
According to the inventionThrough multiple researches, the inventor finds that the T of the cut tobacco is measured by using a low-field nuclear magnetic resonance technology21The value is closely related to the moisture retention performance of the cigarette, and the T of the cigarette can be measured by a low-field nuclear magnetic resonance technology21Judging the good and good moisturizing performance of the fabric; in particular, T21Smaller tobacco shred sample has better moisture retention performance than T21Higher tobacco samples.
The method utilizes the low-field nuclear magnetic resonance technology to evaluate the moisture retention performance of the cigarettes, is simple and convenient to operate, consumes short time, and can quickly and effectively achieve the purpose of evaluating the moisture retention performance; the nondestructive testing device has the advantages of nondestructive testing, avoids waste and pollution of raw materials, reduces material loss in the development process, reduces research and development cost and improves working efficiency.
By applying the method, the improvement condition of different humectants on the moisturizing performance of the same cut tobacco can be inspected by preparing different humectant samples, and a proper addition proportion can be explored. The moisture retention performance of the same kind of humectant in different kinds of cut tobaccos can be also examined. And by the method, the optimal humectant type collocation aiming at specific tobacco is obtained.
Preferably, the relative humidity a is 60 ± 2% and the temperature B is 22 ± 1 ℃.
Preferably, in S1, the first equilibration time is 12-48 h. Most preferably, the time for the first equilibration is 12 hours.
Preferably, in S2, the humectant is one or more of polyhydric alcohols or saccharides.
Optionally, the polyhydric alcohol is propylene glycol or/and glycerol; the saccharide is one or more of algal polysaccharide, tea polysaccharide or coriolus versicolor polysaccharide.
Preferably, the humectant is a mixture of propylene glycol and coriolus versicolor polysaccharide; the mass ratio of the propylene glycol to the coriolus versicolor polysaccharide is 100: 15. When the humectant is used, it is preferably diluted with water and used.
As an embodiment, the humectant consists of propylene glycol, coriolus versicolor polysaccharide, water, and the ratio of propylene glycol: 0.1% of coriolus versicolor polysaccharide: 0.015 percent and the balance of water.
Preferably, in the humectant sample in S2, the addition amount of the humectant is 0.03-0.05 g/g of tobacco shreds.
More preferably, in the humectant sample in S2, the addition amount of the humectant is 0.04 g/g.
Preferably, in S3, the time for the second equilibration is 12-48 h. More preferably, the time of the second equilibration is the same as the time of the first equilibration.
The first balance and the second balance belong to balance treatment in the cigarette processing process, and the third balance belongs to core treatment for moisture retention performance evaluation, so that the time for the third balance must be strictly controlled to be more than 48 h.
Preferably, in S4, the drying treatment mode is hot air drying, the drying temperature is 55 ℃, and the drying is carried out until the moisture content is 12 +/-1%.
Preferably, in S5, the relative humidity of the third equilibrium is 50-80%.
Preferably, S6, before the determination of the signal value of the sample, the method further comprises the step of parameter debugging: debugging the water film and the single sample by adopting a Q-FID sequence, debugging the sample by adopting a Q-CPMG sequence after recording the debugged Q-FID sequence, and recording the parameters of the Q-CPMG; and using the obtained parameters to determine the sample signal values of the humectant sample and the control sample.
Preferably, the low-field NMR spectrometer is a MesoMR23-060H-1 low-field NMR imaging analyzer.
Compared with the prior art, the invention has the following beneficial effects:
the method utilizes the low-field nuclear magnetic resonance technology to evaluate the moisture retention performance of the cigarettes, is simple and convenient to operate, consumes short time, and can quickly and effectively achieve the purpose of evaluating the moisture retention performance; the nondestructive testing device has the advantages of nondestructive testing, avoids waste and pollution of raw materials, reduces material loss in the development process, reduces research and development cost and improves working efficiency.
Drawings
FIG. 1 is a water distribution diagram of cut tobacco ① and cut blank tobacco ① with humectant added at a relative humidity of 60%;
FIG. 2 is a water distribution diagram of cut tobacco ② and cut blank tobacco ② with humectant added at a relative humidity of 60%;
FIG. 3 is a water distribution diagram of cut tobacco ③ and cut blank tobacco ③ with humectant added at a relative humidity of 60%.
Fig. 4 is a graph of moisture desorption rates for samples of cut tobacco ③ with humectant added and cut tobacco blank ③.
Detailed Description
The invention is further illustrated by the following examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. Experimental procedures without specific conditions noted in the examples below, generally according to conditions conventional in the art or as suggested by the manufacturer; the raw materials, reagents and the like used are, unless otherwise specified, those commercially available from the conventional markets and the like. Any insubstantial changes and substitutions made by those skilled in the art based on the present invention are intended to be covered by the claims.
Example 1
The embodiment provides a cigarette moisture retention performance evaluation method based on a low-field nuclear magnetic resonance technology, which comprises the following steps:
firstly, processing tobacco shred samples:
s1, balancing a tobacco shred sample for the first time;
s2, respectively preparing humectant samples added with humectants from partial tobacco shreds in the balanced tobacco shred samples, and
a control sample with water added;
s3, repeating the balance condition in the step S1, and carrying out secondary balance on the humectant sample in the step S2 and the control sample;
s4, respectively drying the humectant sample and the control sample until the water content is 12 +/-1%;
s5, balancing the humectant sample subjected to drying treatment in the S4 and the control sample for the third time under the balancing condition of the S1, wherein the balancing time is 48 hours, and thus obtaining the tobacco shred sample to be measured.
Two, low field nuclear magnetic resonance technology for measuring T21Value of
The instrument used in the low-field MRI technology in this embodiment is a MesoMR23-060H-1 low-field MRI analyzer.
The research steps of the low-field nuclear magnetic resonance technology are as follows:
(1) parameter debugging: firstly, a Q-FID sequence is adopted to debug a water film and a single sample, after the debugged Q-FID sequence is recorded, the Q-CPMG sequence is adopted to debug the sample, and the parameters of the Q-CPMG are recorded.
(2) Weighing a certain amount of tobacco shred samples, and recording the mass of the samples.
(3) And (3) sample testing: and measuring the tobacco shred samples with known weights according to the detection parameters to obtain corresponding sample signal values.
(4) Comparing T according to the inversion signal of tobacco shred sample21. Tobacco shred sample at the same relative humidity, T21Smaller tobacco shred sample has better moisture retention performance than T21Higher tobacco samples.
In this example, the specific conditions are as follows:
test object, shredded tobacco ① (Hunan Xiaxing orange two shredded tobacco)
Test moisture retention agent: compounded with humectant (0.1% of coriolus versicolor polysaccharide as propylene glycol and 0.015% of coriolus versicolor polysaccharide, and the balance of water).
The test steps are as follows:
1. preparing a reagent, namely preparing 100mL of compound humectant solution according to the proportion of 4% of humectant relative to ① mass of cut tobacco.
2. Balancing the tobacco shreds: accurately weighing 2 parts of 20.000g of sample cut tobacco with the number of A, B, and balancing for 12 hours under the environment with the relative humidity of 60% and the temperature of 22 ℃;
3. spraying humectant, namely spraying the compound humectant (recorded as cut tobacco ① and humectant) on the cut tobacco with the number B, spraying equal amount of distilled water (recorded as cut tobacco ①) on the cut tobacco with the number A,
4. rebalancing: the tobacco shred sample sprayed with the humectant is balanced for 12 hours in an environment with the relative humidity of 60% and the temperature of 22 ℃;
5. drying: drying tobacco shred at 55 deg.C with hot air to water content of 12 + -1%.
6. And (3) balancing the dried tobacco shred samples at the temperature of 22 ℃ for 48 hours under the relative humidity of 50%, 60%, 70% and 80%, so as to obtain the processed tobacco shred samples (each sample under different relative humidity is prepared by repeating the steps 1-5).
7. Debugging parameters of the low-field nuclear magnetic resonance apparatus: CPMG sequence parameters: SF 20MHz, O1 816892.10Hz, TW 3000ms, PRG 3, SW 200KHz, TD 60006, NECH 2000, TE 0.150ms, P1 11.52 μ s, P2 24.00 μ s, NS 2, RFD 0.020ms, RG1 5.0db, and DRG1 3.
8. And (4) measuring a sample and inverting the map.
9. The data were analyzed and the moisturizing performance was evaluated.
Data results are shown in table 1.
TABLE 1 relaxation time comparison of humectant-added shredded tobacco ① with cut blank shredded tobacco ① at different relative humidities
As can be seen from Table 1, tobacco shred ① with added compound humectant has different relative humidities: (<80%) is lower than the relaxation time T of blank cut tobacco21As can be seen from FIG. 1, the relaxation time of the tobacco shred samples added with the humectant is shifted to the left, the relaxation time is shortened, the water binding capacity is enhanced, and the moisture retention performance of the tobacco shred ① added with the humectant is improved compared with that of the blank tobacco shred when the relative humidity is 60 percent<Similar conclusions were also made at 80% relative humidity.
Example 2
The embodiment provides a cigarette moisturizing performance evaluation method based on a low-field nuclear magnetic resonance technology, in the evaluation method, a test object is cut tobacco ② 45 (cut tobacco of Mandarin orange in Baoshan Yunnan), a humectant is the same as that in embodiment 1, the rest is the same as that in embodiment 1, and test results are shown in Table 2.
TABLE 2 relaxation time comparison of Yunnan cut tobacco with humectant and blank cut tobacco at different relative humidity
As can be seen from Table 2, cut tobacco ② with added humectant was found to have different relative humidities: (<80%) is lower than the relaxation time T of blank cut tobacco21The relaxation time of the cut tobacco ② is increased along with the increase of the relative humidity, particularly when the relative humidity is 60% -70%, an obvious inflection point appears, and the relaxation time is obviously increased21Becomes larger.
Example 3
In the method, the test object is cut tobacco ③ (full formula cut tobacco), the humectant is the same as that in example 1, the rest is the same as that in example 1, and the test results are shown in Table 3.
TABLE 3 relaxation time comparison of humectant-added tobacco shred ③ with blank tobacco shred at different relative humidities
As shown in Table 3, the relaxation times of cut tobacco ③ with humectant at different relative humidities (50% -80%) were all lower than the relaxation time T of blank cut tobacco21As can be seen from fig. 3, compared with the blank cut tobacco, the relaxation time of the cut tobacco sample added with the humectant is shifted to the left, the relaxation time is shortened, the moisture binding capacity is enhanced, and it can be seen that the moisturizing performance of the cut tobacco ③ added with the humectant is improved compared with the blank cut tobacco.
Example 4
The embodiment provides a cigarette moisture retention performance evaluation method based on a low-field nuclear magnetic resonance technology, in the evaluation method, a test object is cut tobacco ② (cut tobacco of Mandarin orange in Mount Yunnan), humectants ①, ② and ③ are propylene glycol, Coriolus versicolor polysaccharide and a compound humectant which is the same as that in the embodiment 1, the balance is measured for 48 hours under the condition that the relative humidity is 60%, and the rest is consistent with that in the embodiment 1, and the test results are shown in a table 4.
TABLE 4 relaxation time comparison of Yunnan cut tobacco with different humectant and blank cut tobacco at 60 deg.C
As can be seen from Table 4, relaxation time T of cut tobacco ② with humectant21Meanwhile, the relaxation time of the cut tobacco samples added with different humectants is compared, the relaxation time of the cut tobacco samples added with the humectant ③ is the lowest, the humectant ② is the lowest, and the humectant ① is the last, so that the humectant performance of the compound humectant is obviously superior to that of propylene glycol.
Example 5:
firstly, a processed tobacco shred ③ sample (the processing method is the same as that of the embodiment 3) is placed at the temperature of 22 +/-2 ℃ and the relative humidity of about 60 +/-2% and is balanced for 48 hours, then 10 parts of 1.000g of the sample are weighed and placed at the temperature of 22 +/-2 ℃ and the relative humidity of (40 +/-2%) and are balanced, the moisture content change in 72 hours is tested, a group of samples are taken at intervals (every 4 hours in the first 32 hours and every 12 hours in the last 40 hours) and are tested by an oven method, and the error is not more than 0.1%.
Observing the moisture desorption rate curves of samples of cut tobacco ③ added with the humectant and blank cut tobacco ③ (see figure 4), finding that the cut tobacco ③ added with the humectant and the blank cut tobacco reach equilibrium water content within about 32 hours, the equilibrium water content of the cut tobacco ③ added with the humectant is obviously higher than that of the blank cut tobacco, the equilibrium water content of the cut tobacco added with the humectant is reduced to be smaller than that of the blank cut tobacco within 0-32 hours in the same time period, the moisture desorption rate is slow, the compound humectant has certain moisture retention effect on the cut tobacco in the full formula, the moisture dissipation rate of the cut tobacco in the full formula can be slowed down, after 32 hours, the equilibrium water content of the cut tobacco added with the humectant is higher than that of the blank cut tobacco, and the sensory moisture retention performance of the cigarette can be effectively improved, which is consistent with the evaluation result (example 3) of the method.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A cigarette moisture retention performance evaluation method based on a low-field nuclear magnetic resonance technology is characterized by comprising the following steps:
s1, balancing a tobacco shred sample for the first time under a relative humidity A and a temperature B;
s2, respectively preparing humectant samples added with humectants from partial tobacco shreds in the balanced tobacco shred samples, and
a control sample with water added;
s3, balancing the humectant sample and the control sample in the S2 for the second time at the relative humidity A and the temperature B;
s4, respectively drying the humectant sample and the control sample until the water content is 12 +/-1%;
s5, balancing the dried humectant sample and the dried control sample at the relative humidity A and the relative temperature B for the third time, wherein the balancing time is more than 48 hours, so as to obtain a tobacco shred sample to be measured;
s6, measuring the sample signal values of the humectant sample and the control sample by using a low-field nuclear magnetic resonance spectrometer, and comparing the T of different humectant samples according to the inversion signal21Value size, T21The humectant samples with lower values had better humectant properties.
2. The method according to claim 1, wherein the relative humidity A is 60 ± 2% and the temperature B is 22 ± 1 ℃.
3. The evaluation method according to claim 1, wherein in S2, the humectant is one or more of polyhydric alcohols and saccharides.
4. The evaluation method according to claim 1, wherein the polyhydric alcohol is propylene glycol or/and glycerin; the saccharide is one or more of algal polysaccharide, tea polysaccharide or coriolus versicolor polysaccharide.
5. The evaluation method according to claim 1, wherein in S2, the humectant is added in an amount of 0.03 to 0.05g/g of tobacco shreds in the humectant sample.
6. The evaluation method according to claim 1, wherein the drying treatment in S4. is hot air drying, the drying temperature is 50-60 ℃, and the drying is carried out until the moisture content is 12 +/-1%.
7. The evaluation method according to claim 1, wherein, S6, before the determination of the signal value of the sample, the method further comprises the step of parameter adjustment: debugging the water film and the single sample by adopting a Q-FID sequence, debugging the sample by adopting a Q-CPMG sequence after recording the debugged Q-FID sequence, and recording the parameters of the Q-CPMG; and using the obtained parameters to determine the sample signal values of the humectant sample and the control sample.
8. The method of claim 1, wherein the low-field nmr analyzer is a MesoMR23-060H-1 low-field nmr imaging analyzer.
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Application publication date: 20200424 |