CN113567586A - Quality identification method of feed liquid for cigarettes - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 41
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 40
- 238000012360 testing method Methods 0.000 claims abstract description 30
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
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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
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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
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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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
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- 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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
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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
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention relates to the technical field of quality control of feed liquid for cigarettes, in particular to a quality identification method of feed liquid for cigarettes. The method comprises the following steps: mixing the tobacco material liquid with an extraction solvent, oscillating, and performing ultrasonic extraction; purifying the supernatant, performing high performance liquid chromatography, and collecting chromatographic fingerprint of the test sample and the standard sample; performing original data information processing on the chromatographic fingerprint, dividing chromatographic peaks into a large peak and a small peak, calculating the relative percentage deviation value of the large peak of the test sample and a standard sample, and calculating the cosine value of the included angle between the small peak of the test sample and the standard sample; and judging the conformity of the test sample according to the obtained large peak deviation value, the cosine value of the small peak included angle and the tolerance control standard. By the method, the winning bid sample with the quality closest to that of the standard sample in the bid sample can be accurately identified, and whether the quality of the batch is stable or not can be accurately identified.
Description
Technical Field
The invention relates to the technical field of quality control of feed liquid for cigarettes, in particular to a quality identification method of feed liquid for cigarettes.
Background
The tobacco material liquid is a mixture which is applied to tobacco in the processing process of tobacco products, has the functions of reducing irritation, softening smoke, improving aftertaste, improving the physical properties of the tobacco, such as moisture retention, flexibility, combustibility, mildew resistance and the like, and has certain fragrance. The quality stability of the cigarette is directly related to the quality stability of cigarette products.
At present, the existing quality control standard of the cigarette feed liquid in the industry mainly comprises conventional physicochemical indexes (refractive index, relative density, acid value, solubility, clarity, total amount of volatile substances), safety indexes such as heavy metals and forbidden components, smell and sensory evaluation. However, the indexes have the defects of weak representation, insufficient monitoring strength on quality stability and the like, and the chemical composition and the change of the feed liquid for the cigarettes cannot be deeply represented. Because the content of the solvent in the feed liquid for cigarettes is very high, and some physical indexes such as refractive index, relative density and the like are mainly influenced by the solvent, the two indexes cannot accurately and sensitively reflect the change of effective chemical components in the feed liquid, and the indexes such as acid value, total amount of volatile components and the like also hardly reflect the change of different chemical components in the feed liquid. The smelling and sensory evaluation are easily affected by changes of subjective consciousness, environmental and individual differences and other factors, and the evaluation results have large differences.
Fingerprint spectrum is a new quality control means which is popular at present, is a technology for integrally researching a complex substance system, and is applied to many fields. Application research of quality control of feed liquid fingerprint spectrum for cigarettes is also carried out inside and outside the industry. Up to now, these studies have some drawbacks, mainly expressed in the following areas: (1) the universality of the analysis method is not strong, and the reported method cannot be applied to the analysis of various tobacco feed liquids with huge differences in physical properties and chemical properties; (2) when similarity calculation is carried out on the chromatographic fingerprint, one mode processing is carried out on all chromatographic peaks, and the large peak and the small peak are not divided, so that the calculation result discriminates the small chromatographic peaks. In addition to the solvent, a plurality of cigarette feed liquids contain one or more main components (chemical substances) with larger content, and a plurality of other chemical substances which are usually important functional fragrant substances with lower content; on the other hand, the influence of the dilution effect is not considered in the similarity calculation. When all chromatographic peaks increase or decrease in equal proportion, the overall similarity difference of the chromatographic peaks is small. Therefore, only by solving the technical problems, the scientific and accurate control of the chromatographic fingerprint spectrum on the quality stability of the feed liquid for the cigarettes can be realized.
Disclosure of Invention
In view of the above, the invention provides a quality identification method of feed liquid for cigarettes. By the method, the winning bid sample with the quality closest to that of the standard sample in the bid sample can be accurately identified, and whether the quality of the batch is stable or not can be accurately identified.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a quality identification method of feed liquid for cigarettes, which comprises the following steps:
mixing the tobacco material liquid with an extraction solvent, oscillating, and performing ultrasonic extraction; purifying the supernatant, performing high performance liquid chromatography, and collecting chromatographic fingerprint of the test sample and the standard sample;
performing original data information processing on the chromatographic fingerprint, dividing chromatographic peaks into a large peak and a small peak, and calculating the relative percentage deviation value of the large peak of the test sample and the standard sample to obtain a large peak deviation value; calculating the cosine value of the included angle between the small peak of the test sample and the standard sample to obtain the cosine value of the included angle of the small peak; the large peak is a chromatographic peak with a normalized area of 10% or more, and the small peak is a chromatographic peak with a normalized area of less than 10%;
and judging the conformity of the test sample according to the obtained large peak deviation value, the cosine value of the small peak included angle and the tolerance control standard.
Preferably, the tolerance control criteria are divided into the following four categories:
class I: the deviation value of the large peak is less than or equal to 20 percent, and the cosine value of the included angle of the small peak is more than or equal to 0.95;
class II: the large peak deviation value is less than or equal to 25 percent, and the cosine value of the included angle of the small peak is more than or equal to 0.90;
class III: the large peak deviation value is less than or equal to 30 percent, and the cosine value of the included angle of the small peak is more than or equal to 0.85;
and IV: the large peak deviation value is > 30% and the small peak included angle cosine value is < 0.85.
Preferably, the determination of the conformity of the test sample specifically comprises:
according to the standard of the control of the tolerance,
the material liquid for the cigarettes which accords with the I or II standard has basically consistent and better quality with the standard sample;
the material liquid for the cigarettes meeting the class III standard has certain difference between the internal quality and the standard sample and general stability;
the quality of the feed liquid for the cigarettes meeting the IV-type standard changes violently.
Preferably, the extraction solvent is a mixture of water and alcohols, the alcohols include but are not limited to methanol and/or ethanol, and the volume ratio of the water to the alcohols is (1-5): 1.
In the specific example provided by the present invention, the volume ratio of water to alcohol is 3: 1.
Preferably, the using amount ratio of the feed liquid for the cigarettes to the extraction solvent is (0.1-1): (1-100).
Preferably, the time of ultrasonic extraction is 5-20 min.
In the specific embodiment provided by the invention, the time for ultrasonic extraction is 10 min.
Preferably, purification involves passing through an SPE cartridge and a filter.
Preferably, the filter is a filter with a pore size of 0.22 μm.
Preferably, the conditions of the high performance liquid chromatography are as follows:
the detector is a diode array detector, and the detection wavelength is 254-275 nm;
the sample feeding amount of the sample is 1-10 mu L;
the liquid chromatographic column is a ZORBAX SB-Phenyl column;
the column temperature is 35-45 ℃;
the mobile phase A is 0.01 to 0.05 percent of hydrochloric acid, and the mobile phase B is acetonitrile;
the flow rate is 0.1-1.0 mL/min;
gradient elution procedure.
Preferably, the conditions of the high performance liquid chromatography are:
the detection wavelength is 254nm or 275 nm.
The amount of sample was 5. mu.L.
The model of the liquid chromatography column ZORBAX SB-Phenyl column is as follows: 3.5mm × 150mm, 3.5 μm.
The column temperature was 40 ℃.
Mobile phase a was 0.025% hydrochloric acid.
The flow rate was 0.4 mL/min.
The gradient elution procedure was: 0-30min, 100% -50% A; 30-40min, 100% B; 40-45min, 100% B; 45-50min, 100% A.
In the present invention, the test sample is a bid sample or an inter-lot sample.
The invention provides a quality identification method of feed liquid for cigarettes. The method comprises the following steps: mixing the tobacco material liquid with an extraction solvent, oscillating, and performing ultrasonic extraction; purifying the supernatant, performing high performance liquid chromatography, and collecting chromatographic fingerprint of the test sample and the standard sample; performing original data information processing on the chromatographic fingerprint, dividing chromatographic peaks into a large peak and a small peak, calculating the relative percentage deviation value of the large peak of the test sample and a standard sample, and calculating the cosine value of the included angle between the small peak of the test sample and the standard sample; and judging the conformity of the test sample according to the obtained large peak deviation value, the cosine value of the small peak included angle and the tolerance control standard. Compared with the prior art, the invention has the beneficial effects that:
1) the invention provides a quality identification method of feed liquid for cigarettes for bidding and batch-to-batch quality stability for the first time by combining the characteristics of the feed liquid for cigarettes. A large number of experiments repeatedly verify that the optimal analysis parameter combination is obtained, the obtained map information is rich, the separation effect is good, and the method has universality, sensitivity and stability.
In contrast to patent document No. 200810049117.3: (1) the sample extraction method adopted by the invention firstly carries out vortex oscillation and then carries out ultrasonic extraction, the samples are mixed uniformly, and the effective components in the samples are extracted completely. In contrast, in the comparison document, the sample is directly diluted by using the mixed solution of ultrapure water, absolute ethyl alcohol and propylene glycol without subsequent operations, so that the pasty sample is difficult to dissolve and is uniformly mixed (as can be seen in the experiment). (2) The liquid phase analysis time of the sample in the comparison file exceeds 80min, but the invention adopts the chromatographic column and the gradient elution condition, can finish the analysis of the sample by only 50min, and improves the detection efficiency.
2) When similarity calculation is carried out on the chromatogram, a mode of respectively calculating a large peak and a small peak is adopted, so that not only can discrimination effect of the large peak on the small peak be eliminated, but also influence of dilution effect can be eliminated, the winning bid sample with the quality closest to that of the standard sample can be accurately identified, and the accuracy rate basically reaches 100%.
The document 200810049117.3 discloses calculating the overall similarity of two samples by the cosine of the included angle, which weakens the effect of small peaks. Because mathematically speaking, the cosine of the angle is the cosine of the angle between the multidimensional space vectors. When the size of a certain dimension (i.e. a certain chromatographic peak) is significantly higher than that of other chromatographic peaks, the weight of the chromatographic peak in the calculation result is large, and the contribution of the small chromatographic peak to the cosine value of the included angle can be reduced or covered. In other words, the calculation discriminates against small chromatographic peaks. It is well known to those skilled in the art of flavors and fragrances that, in addition to solvents, a large amount of one or more major components (chemical substances) may be present in many tobacco feed liquids, while a large amount of other chemical substances, which are generally important functional flavor substances, are present in lower amounts. Therefore, the problem of discrimination effect of a large peak to a small peak must be solved by adopting an included angle cosine method, and scientific and accurate control of the quality stability of the tobacco essence and flavor by the chromatographic fingerprint spectrum can be realized. The invention adopts the mode of respectively calculating the big peak and the small peak, solves the problem of discrimination effect of the big peak to the small peak, and has more reliable result.
3) The difference of the samples is difficult to determine by a method of determining chemical components because the feed liquid for the cigarettes usually contains a large amount of components which are difficult to volatilize or have strong water solubility and cannot or is not suitable for analysis by gas chromatography-mass spectrometry. The method provided by the invention can not only obtain the whole material composition and the change information of the feed liquid for the cigarettes, but also avoid the blind areas existing in the traditional conventional detection indexes and sensory evaluation, can realize the comprehensive evaluation of the internal quality of the feed liquid for the cigarettes, and is suitable for the socialized open bidding of the feed liquid for the cigarettes and the quality stability identification work among batches.
Drawings
FIG. 1 is a flow chart of the method of the present invention;
FIG. 2 is a liquid chromatogram of 23# standard sample and its bid sample;
FIG. 3 is a liquid chromatogram of a 44# standard sample and its bid sample;
FIG. 4 is a liquid chromatogram of 8810 as it is and its diluted sample.
Detailed Description
The invention discloses a quality identification method of feed liquid for cigarettes, and a person skilled in the art can appropriately improve process parameters by referring to the content. It is expressly intended that all such similar substitutes and modifications which would be obvious to one skilled in the art are deemed to be included in the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The feed liquid for cigarettes used in the embodiment of the invention is feed liquid for Changbai mountain cigarettes.
The reagents or apparatus used in the present invention are commercially available.
The invention is further illustrated by the following examples:
example 1
The invention provides a quality identification method of feed liquid for cigarettes, which comprises the following steps:
1. preparation of sample solution
Precisely weighing 0.3g of feed liquid for cigarettes, placing the feed liquid in a conical flask with a plug, adding 10mL of an extraction solvent (the used extraction solvent is water-ethanol with the volume ratio of 3:1), sealing the plug, shaking the plug on a vortex oscillator for 1min, then carrying out ultrasonic extraction for 10min, taking supernatant, purifying the supernatant by an SPE column and a 0.22 mu m filter membrane in sequence, and placing the purified supernatant in a chromatographic sample feeding bottle.
2. Collection of chromatographic fingerprint
And (4) carrying out high performance liquid chromatography on the analysis solution, and collecting the chromatographic fingerprint of the sample.
The chromatographic fingerprint conditions are as follows:
the detector of the high performance liquid chromatography is a diode array detector, and the detection wavelength is 254 nm;
the sample amount of the sample is 5 mu L;
the liquid chromatography column is ZORBAX SB-Phenyl column (3.5mm × 150mm, 3.5 μm);
the column temperature was 40 ℃;
mobile phase a is 0.025% hydrochloric acid and mobile phase B is acetonitrile;
the flow rate is 0.4 mL/min;
gradient elution procedure: 100% -50% A in 0-30min, 100% B in 30-40min, 100% B in 40-45min, and 100% A in 45-50 min.
3. Raw information processing of chromatographic fingerprint
The obtained chromatogram is subjected to original data information processing and divided into a large peak (high-content component) and a small peak (low-content component). And respectively calculating the relative percentage deviation (high content component change threshold) of the large peak of the test sample and the standard sample, and calculating the cosine value of the included angle between the small peak of the test sample and the standard sample.
The large peak (high content component) is a chromatographic peak with a normalized area of 10% or more;
the small peak (low content component) is a chromatographic peak with a normalized area of 10% or less;
the test samples are bid samples or batch samples.
4. Conformity determination of test sample
The tolerance control standards of the fingerprint spectrograms of the test sample and the standard sample are divided into the following four types:
class I: the deviation of the large peak is less than or equal to 20 percent, and the cosine of the included angle of the small peak is more than or equal to 0.95;
class II: the deviation of the large peak is less than or equal to 25 percent, and the cosine of the included angle of the small peak is more than or equal to 0.90;
class III: the deviation of the large peak is less than or equal to 30 percent, and the cosine of the included angle of the small peak is more than or equal to 0.85;
and IV: the large peak deviation is more than 30 percent, and the cosine of the included angle of the small peak is less than 0.85.
According to the classification standard, the material liquid for the cigarettes which accords with the I-type and II-type standards has basically consistent internal quality and better quality with the standard sample; the material liquid for the cigarettes meeting the class III standard has certain difference between the internal quality and the standard sample and general stability; the quality of the feed liquid for the cigarettes meeting the IV-type standard changes violently.
Test examples
The bidding samples (6#, 23#, 36#, 44#, 45#) and the lot samples (A, B, C, D) were tested by the method of example 1, and the test results are shown in tables 1 and 2.
According to the calculation result of the map, compared with a standard sample, the test sample meets the condition that the large peak deviation is less than or equal to 20%, and the cosine of the small peak included angle is greater than or equal to 0.95 within the tolerance range, the smaller the large peak deviation is, the greater the cosine of the small peak included angle is, the highest similarity between the test sample and the standard sample is, and the quality is the closest.
TABLE 1 Bidding sample determination for tobacco feed liquid
TABLE 2 quality stability determination between batches of tobacco feed liquid
Comparative test example
Example 1 a similarity analysis was performed on the liquid chromatography fingerprints of 8810 samples (8810-75%, 8810-50%, 8810-25%) as such and at different dilution ratios, and the results showed that: if similarity calculation is carried out without dividing the size peak, the similarity degree of 3 diluted samples is more than or equal to 0.95 compared with the original sample by adopting an overall similarity evaluation method; if similarity calculation is carried out on the large peak and the small peak respectively, it can be seen that the deviation of the large peak is more than or equal to 25 percent, although the composition components of the four samples are basically consistent, the contents are different, and the quality fluctuates. This indicates that the calculation of global similarity to evaluate the consistency of different sample masses is not accurate (table 3, fig. 4).
TABLE 3 quality determination of tobacco feed liquid 8810 (different dilution ratios)
Example 2 similarity analysis was performed on the liquid chromatography fingerprints of the standard sample C and the batch samples, and the results show that: if similarity calculation is carried out without dividing the size peak, the 3 batches of samples are compared with the standard sample by adopting an overall similarity evaluation method, the similarity degree is more than or equal to 0.95, and the samples are qualified; if similarity calculation is carried out on the large peak and the small peak respectively, compared with a standard sample, the cosine of the included angle of the small peak of C-02 is less than 0.95, the cosine of the included angle of the small peak of C-03 is less than 0.90, and the quality of the samples of the two batches fluctuates and is unqualified. This indicates that the way of calculating the overall similarity to evaluate the consistency of the different sample qualities is not accurate.
TABLE 4 quality stability determination between cigarette feed liquid C batches
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A quality identification method of feed liquid for cigarettes is characterized by comprising the following steps:
mixing the tobacco material liquid with an extraction solvent, oscillating, and performing ultrasonic extraction; purifying the supernatant, performing high performance liquid chromatography, and collecting chromatographic fingerprint of the test sample and the standard sample;
performing original data information processing on the chromatographic fingerprint, dividing chromatographic peaks into a large peak and a small peak, and calculating the relative percentage deviation value of the large peak of the test sample and the standard sample to obtain a large peak deviation value; calculating the cosine value of the included angle between the small peak of the test sample and the standard sample to obtain the cosine value of the included angle of the small peak; the large peak is a chromatographic peak with a normalized area of 10% or more, and the small peak is a chromatographic peak with a normalized area of less than 10%;
and judging the conformity of the test sample according to the obtained large peak deviation value, the cosine value of the small peak included angle and the tolerance control standard.
2. The method of claim 1, wherein the tolerance control criteria are classified into the following four categories:
class I: the deviation value of the large peak is less than or equal to 20 percent, and the cosine value of the included angle of the small peak is more than or equal to 0.95;
class II: the large peak deviation value is less than or equal to 25 percent, and the cosine value of the included angle of the small peak is more than or equal to 0.90;
class III: the large peak deviation value is less than or equal to 30 percent, and the cosine value of the included angle of the small peak is more than or equal to 0.85;
and IV: the large peak deviation value is > 30% and the small peak included angle cosine value is < 0.85.
3. The method for quality assessment according to claim 2, wherein said determining the compliance of the test sample is specifically:
in accordance with the tolerance control criteria described above,
the material liquid for the cigarettes which accords with the I or II standard has basically consistent and better quality with the standard sample;
the material liquid for the cigarettes meeting the class III standard has certain difference between the internal quality and the standard sample and general stability;
the quality of the feed liquid for the cigarettes meeting the IV-type standard changes violently.
4. The quality identification method according to claim 1, wherein the extraction solvent is a mixture of water and alcohols, the alcohols include but are not limited to methanol and/or ethanol, and the volume ratio of water to alcohols is (1-5): 1.
5. The quality identification method according to claim 1, wherein the using amount ratio of the tobacco feed liquid to the extraction solvent is (0.1-1): (1-100).
6. The quality identification method according to claim 1, wherein the ultrasonic extraction time is 5-20 min.
7. The method of claim 1, wherein the purification comprises SPE column and filter.
8. The method of claim 1, wherein the conditions of the high performance liquid chromatography are as follows:
the detector is a diode array detector, and the detection wavelength is 254-275 nm;
the sample feeding amount of the sample is 1-10 mu L;
the liquid chromatographic column is a ZORBAX SB-Phenyl column;
the column temperature is 35-45 ℃;
the mobile phase A is 0.01 to 0.05 percent of hydrochloric acid, and the mobile phase B is acetonitrile;
the flow rate is 0.1-1.0 mL/min;
gradient elution procedure.
9. The method of claim 8, wherein the gradient elution procedure is: 0-30min, 100% -50% A; 30-40min, 100% B; 40-45min, 100% B; 45-50min, 100% A.
10. The method of any one of claims 1 to 9, wherein the test sample is a bid sample or an inter-lot sample.
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