CN113567586B - Quality identification method of tobacco feed liquid - Google Patents
Quality identification method of tobacco feed liquid Download PDFInfo
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- 239000007788 liquid Substances 0.000 title claims abstract description 54
- 241000208125 Nicotiana Species 0.000 title claims abstract description 48
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000012360 testing method Methods 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 238000000605 extraction Methods 0.000 claims abstract description 12
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 9
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 9
- 230000010365 information processing Effects 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000006228 supernatant Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 150000001298 alcohols Chemical class 0.000 claims description 5
- 238000010828 elution Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims description 2
- 238000007689 inspection Methods 0.000 claims 2
- 238000001914 filtration Methods 0.000 claims 1
- 238000000275 quality assurance Methods 0.000 claims 1
- 238000003908 quality control method Methods 0.000 abstract description 5
- 239000000523 sample Substances 0.000 description 59
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- 238000010790 dilution Methods 0.000 description 4
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- 206010013911 Dysgeusia Diseases 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
- -1 but not limited to Chemical class 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
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- 230000000052 comparative effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
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- 238000005516 engineering process Methods 0.000 description 1
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- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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- 230000035945 sensitivity Effects 0.000 description 1
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- 235000013599 spices Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000019505 tobacco product Nutrition 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 239000013598 vector Substances 0.000 description 1
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Classifications
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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
-
- 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
- G01N30/86—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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- 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
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
-
- 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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- Physics & Mathematics (AREA)
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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)
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- Pathology (AREA)
- Engineering & Computer Science (AREA)
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- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention relates to the technical field of quality control of tobacco material liquid, in particular to a quality identification method of tobacco material liquid. The method comprises the following steps: mixing the tobacco feed liquid with an extraction solvent, and performing ultrasonic extraction after shaking; purifying the supernatant, performing high performance liquid chromatography, and collecting chromatographic fingerprints of the test sample and the standard sample; performing original data information processing on the chromatographic fingerprint, dividing chromatographic peaks into two types of large peaks and small peaks, calculating the relative percentage deviation value of the large peaks of the test sample and the standard sample, and calculating the cosine value of the included angle between the small peaks of the test sample and the standard sample; and judging the consistency of the test sample according to the obtained large peak deviation value, the obtained small peak included angle cosine value and the obtained tolerance control standard. The method can accurately identify the winning bid sample with the quality closest to that of the standard sample in the bidding samples and whether the quality among batches is stable.
Description
Technical Field
The invention relates to the technical field of quality control of tobacco material liquid, in particular to a quality identification method of tobacco material liquid.
Background
The tobacco feed liquid is a mixture which is applied to tobacco in the processing process of the tobacco products, has the functions of relieving irritation, leading the smoke to be soft and fine, improving the aftertaste, improving the physical properties of the tobacco, such as moisture retention, flexibility, combustibility, mildew resistance and the like, and has a certain aroma. Its quality stability is directly related to the quality stability of the cigarette product.
At present, the current quality control standard of the tobacco material liquid in the industry mainly comprises conventional physicochemical indexes (refractive index, relative density, acid value, miscibility, clarity and total volatile substances), safety indexes such as heavy metals, forbidden components and the like, and odor and sensory evaluation. However, the indexes have the defects of weak characterization, insufficient monitoring strength on quality stability and the like, and the chemical composition and the change of the tobacco feed liquid cannot be deeply characterized. Because the content of the solvent in the 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 liquid, and the indexes such as acid value, total volatile components and the like hardly reflect the change of different chemical components in the liquid. The smell and sensory evaluation is easily affected by subjective consciousness, environmental and individual difference and other factors, and the evaluation results have large differences.
Fingerprint is a new quality control means which is popular at present, and is a technology for researching complex substance systems on the whole, and is applied to a plurality of fields. Application researches on quality control of the tobacco material liquid fingerprint are also carried out inside and outside industries. Up to now, these studies have some drawbacks, mainly represented by the following: (1) The analysis method has low universality, and the reported method cannot be suitable for analyzing various tobacco feed liquids with huge differences in physical properties and chemical properties; (2) When similarity calculation is carried out on the chromatographic fingerprints, one mode processing is carried out on all chromatographic peaks, size peaks are not separated, and therefore the calculation result shows discrimination on small chromatographic peaks. In addition to solvents, many tobacco feeds contain one or more major components (chemicals) in relatively high amounts, while numerous other chemicals, often relatively important functional flavour materials, are present in relatively low amounts; on the other hand, the influence of the dilution effect is not taken into consideration in the similarity calculation. When all the chromatographic peaks are increased or decreased in the same proportion, the overall similarity difference of the chromatographic peaks is small. Therefore, only if the technical problems are solved, the scientific and accurate control of the chromatographic fingerprint on the quality stability of the tobacco material liquid can be realized.
Disclosure of Invention
In view of the above, the invention provides a quality identification method of tobacco feed liquid. The method can accurately identify the winning bid sample with the quality closest to that of the standard sample in the bidding samples and whether the quality among batches is stable.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a quality identification method of a tobacco feed liquid, which comprises the following steps:
mixing the tobacco feed liquid with an extraction solvent, and performing ultrasonic extraction after shaking; purifying the supernatant, performing high performance liquid chromatography, and collecting chromatographic fingerprints of the test sample and the standard sample;
performing original data information processing on the chromatographic fingerprint, dividing chromatographic peaks into two types of large peaks and small peaks, and calculating the relative percentage deviation value of the large peaks of the test sample and the standard sample to obtain large peak deviation values; 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 between the small peak and the standard sample; the large peak is chromatographic peak with normalized area of 10% or more, and the small peak is chromatographic peak with normalized area of 10% or less;
and judging the consistency of the test sample according to the obtained large peak deviation value, the obtained small peak included angle cosine value and the obtained tolerance control standard.
Preferably, the tolerance control criteria are divided into the following four categories:
class I: the deviation value of a large peak is less than or equal to 20%, and the cosine value of a small peak included angle is more than or equal to 0.95;
class II: the large peak deviation value is less than or equal to 25%, and the cosine value of the small peak included angle is more than or equal to 0.90;
class III: the deviation value of a large peak is less than or equal to 30%, and the cosine value of a small peak included angle is more than or equal to 0.85;
class IV: the large peak deviation value is >30% and the small peak angle cosine value is <0.85.
Preferably, the determination of the compliance of the test sample is specifically:
in accordance with the tolerance control criteria,
the internal quality of the tobacco feed liquid meeting the I-class or II-class standard is basically consistent with that of a standard sample, and the quality is good;
the tobacco material liquid meeting III class standard has certain difference between the internal quality and the standard sample and has general stability;
the quality of the tobacco feed liquid meeting IV standard is changed severely.
Preferably, the extraction solvent is a mixture of water and alcohols including, but not limited to, methanol and/or ethanol, the volume ratio of water to alcohols (1-5): 1.
In the specific embodiment provided by the invention, the volume ratio of water to alcohol is 3:1.
Preferably, the ratio of the tobacco feed liquid to the extraction solvent is (0.1-1) in g/mL: (1-100).
Preferably, the time of ultrasonic extraction is 5 to 20 minutes.
In the specific embodiment provided by the invention, the ultrasonic extraction time is 10min.
Preferably, the purification comprises a SPE cartridge and a filter membrane.
Preferably, the filter is a filter with a pore size of 0.22. Mu.m.
Preferably, the conditions of the high performance liquid chromatography are:
the detector is a diode array detector, and the detection wavelength is 254-275 nm;
the sample injection 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 ℃;
mobile phase A is 0.01% -0.05% hydrochloric acid, 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 was 254nm or 275nm.
The sample loading was 5. Mu.L.
The model of the liquid chromatographic column ZORBAX SB-Phenyl column is: 3.5 mm. Times.150 mm,3.5 μm.
The column temperature was 40 ℃.
Mobile phase a was 0.025% hydrochloric acid.
The flow rate was 0.4mL/min.
The gradient elution procedure was: 0 to 30min,100 to 50 percent of 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 a lot-to-lot sample.
The invention provides a quality identification method of a tobacco feed liquid. The method comprises the following steps: mixing the tobacco feed liquid with an extraction solvent, and performing ultrasonic extraction after shaking; purifying the supernatant, performing high performance liquid chromatography, and collecting chromatographic fingerprints of the test sample and the standard sample; performing original data information processing on the chromatographic fingerprint, dividing chromatographic peaks into two types of large peaks and small peaks, calculating the relative percentage deviation value of the large peaks of the test sample and the standard sample, and calculating the cosine value of the included angle between the small peaks of the test sample and the standard sample; and judging the consistency of the test sample according to the obtained large peak deviation value, the obtained small peak included angle cosine value and the obtained tolerance control standard. Compared with the prior art, the invention has the beneficial effects that:
1) The invention provides a quality identification method of the tobacco feed liquid for bidding and batch-to-batch quality stability for the first time by combining the characteristics of the tobacco feed liquid. Through repeated verification of a large number of experiments, the optimal analysis parameter combination is obtained, the obtained atlas information is rich, the separation effect is relatively good, and the method has universality, sensitivity and stability.
Compared with the patent document with the application number 200810049117.3: (1) The sample extraction mode adopted by the invention is vortex oscillation firstly, then ultrasonic extraction is carried out, the sample mixing is relatively uniform, and the extraction of the effective components in the sample is relatively complete. In the comparison document, the sample is directly diluted by adopting the mixed solution of ultrapure water, absolute ethyl alcohol and propylene glycol, and no subsequent operation is performed, so that the pasty sample is difficult to dissolve and is uniformly mixed (can be seen in the experiment). (2) The liquid phase analysis time of the sample in the comparison file exceeds 80min, but the sample can be analyzed only by 50min under the chromatographic column and gradient elution conditions, so that the detection efficiency is improved.
2) When the similarity calculation is carried out on the chromatograms, the mode of calculating the large peak and the small peak respectively is adopted, so that the discrimination effect of the large peak to the small peak can be eliminated, the influence of the 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 patent document 200810049117.3 discloses a method for calculating the overall similarity of two samples by adopting an included angle cosine mode, so that the effect of a small peak is weakened. Because in a mathematical sense 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 results are discriminated from the small chromatographic peaks. It is well known to those skilled in the art of fragrances and perfumes that, in addition to solvents, one or more major components (chemicals) are present in many tobacco streams, while a number of other chemicals, often more important functional fragrances, are present in lower amounts. Therefore, the problem of discrimination effect of large peaks to small peaks must be solved by adopting an included angle cosine method, so that scientific and accurate control of quality stability of the essence and the spice for cigarettes by the chromatographic fingerprint can be realized. The invention adopts the mode of calculating the large peak and the small peak respectively, solves the problem of discrimination effect of the large peak to the small peak, and has more reliable result.
3) Since the smoke liquid often contains a large amount of components which are difficult to volatilize or have strong water solubility, the smoke liquid cannot be or is not suitable for analysis by adopting gas chromatography-mass spectrometry, and therefore, the difference of samples is difficult to determine by a mode of defining chemical components. The method provided by the invention not only can acquire the integral substance composition and the change information of the tobacco material liquid, but also can avoid the blind areas existing in the conventional detection indexes and sensory evaluation, can realize the comprehensive evaluation of the internal quality of the tobacco material liquid, and is suitable for social public bidding and batch-to-batch quality stability identification of the tobacco material liquid.
Drawings
FIG. 1 is a flow chart of the method of the present invention;
FIG. 2 is a liquid chromatogram of a 23# standard sample and a bid sample thereof;
FIG. 3 is a liquid chromatogram of a 44# standard sample and a bid sample thereof;
fig. 4 is a liquid chromatogram of 8810 as such and diluted samples thereof.
Detailed Description
The invention discloses a quality identification method of a tobacco feed liquid, and a person skilled in the art can properly improve process parameters by referring to the content of the text. It is expressly noted that all such similar substitutions and modifications will be apparent to those skilled in the art, and are deemed to be included in the present invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those skilled in the relevant art that variations and modifications can be made in the methods and applications described herein, and in the practice and application of the techniques of this invention, without departing from the spirit or scope of the invention.
The tobacco feed liquid used in the embodiment of the invention is the feed liquid for Changbai mountain cigarettes.
The reagents or instruments 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 a tobacco feed liquid, which comprises the following steps:
1. preparation of sample solutions
Precisely weighing 0.3g of tobacco material liquid, placing into a conical bottle with a plug, adding 10mL of extraction solvent (the volume ratio of the extraction solvent to the ethanol is 3:1), sealing, vibrating on a vortex oscillator for 1min, performing ultrasonic extraction for 10min, taking supernatant, purifying by an SPE column and a 0.22 mu m filter membrane in sequence, and placing into a chromatographic sample bottle.
2. Acquisition of chromatographic fingerprint
And (3) performing high performance liquid chromatography on the analysis solution, and collecting chromatographic fingerprints of the sample.
The chromatographic fingerprint conditions were as follows:
the detector of the high performance liquid chromatography is a diode array detector, and the detection wavelength is 254nm;
the sample injection amount of the sample is 5 mu L;
the liquid chromatography column was a ZORBAX SB-Phenyl column (3.5 mm. Times.150 mm,3.5 μm);
column temperature is 40 ℃;
mobile phase A is 0.025% hydrochloric acid, mobile phase B is acetonitrile;
the flow rate is 0.4mL/min;
gradient elution procedure: 0-30min 100% -50% A,30-40min 100% B,40-45min 100% B,45-50min 100% A.
3. Original information processing of chromatographic fingerprint
The obtained chromatographic patterns are subjected to original data information processing and are divided into two types of large peaks (high-content components) and small peaks (low-content components). 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 chromatographic peak with normalized area of 10% or more;
the small peak (low content component) is a chromatographic peak with normalized area below 10%;
the test samples are bidding samples or inter-lot samples.
4. Compliance determination of test samples
Tolerance control standards of fingerprint spectrograms of the test sample and the standard sample are divided into the following four types:
class I: the large peak deviation is less than or equal to 20 percent, and the cosine of the small peak included angle is more than or equal to 0.95 percent;
class II: the large peak deviation is less than or equal to 25 percent, and the cosine of the small peak included angle is more than or equal to 0.90 percent;
class III: the deviation of a large peak is less than or equal to 30 percent, and the cosine of the included angle of a small peak is more than or equal to 0.85;
class IV: the large peak deviation is more than 30%, and the cosine of the small peak included angle is less than 0.85.
According to the classification standards, the internal quality of the tobacco feed liquid meeting the I and II standards is basically consistent with that of the standard sample, and the quality is good; the tobacco material liquid meeting III class standard has certain difference between the internal quality and the standard sample and has general stability; the quality of the tobacco feed liquid meeting IV standard is changed severely.
Test examples
Bidding samples (6 #, 23#, 36#, 44#, 45 #) and batch samples (A, B, C, D) were tested using the method of example 1 and the test results are shown in tables 1 and 2.
According to the calculation result of the atlas, compared with the standard sample, the test sample accords with the large peak deviation less than or equal to 20%, and in the tolerance range of the small peak included angle cosine more than or equal to 0.95, the smaller the large peak deviation is, the higher the small peak included angle cosine is, the test sample has the highest similarity with the standard sample, and the quality is closest.
Table 1 sample bid for tobacco smoke
TABLE 2 examples of quality stability determination between tobacco batch
Comparative test example
Example 1 liquid chromatography fingerprints of samples (8810-75%, 8810-50%, 8810-25%) as received and at different dilution ratios were analyzed for similarity, and the results showed that: if the similarity calculation is carried out without dividing the size peaks, adopting an overall similarity evaluation method, wherein the similarity degree of 3 diluted samples is more than or equal to 0.95 compared with the original samples; if similarity calculation is carried out on the size peaks, the deviation of the large peaks is more than or equal to 25%, and although the composition components of the four samples are basically consistent, the content is different, and the quality fluctuates. This indicates that the use of the overall similarity calculation to evaluate the consistency of the different sample masses is inaccurate (table 3, fig. 4).
TABLE 3 quality determination of tobacco liquid 8810 (different dilution ratios)
Example 2 liquid chromatography fingerprints of the C standard samples and batches of samples were analyzed for similarity, and the results showed that: if the similarity calculation is carried out without dividing the size peaks, adopting an overall similarity evaluation method, and comparing 3 batches of samples with standard samples, wherein the similarity is more than or equal to 0.95 and is qualified; if the similarity calculation is respectively carried out on the peaks with different sizes, compared with a standard sample, the cosine of the small peak included angle of C-02 is less than 0.95, the cosine of the small peak included angle of C-03 is less than 0.90, and the quality of samples of the two batches is fluctuated and is unqualified. This suggests that the use of the overall similarity calculation to evaluate the consistency of the different sample masses is inaccurate.
TABLE 4 determination of quality stability between tobacco Material liquid C batches
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (5)
1. The quality identification method of the tobacco feed liquid is characterized by comprising the following steps of:
mixing the tobacco feed liquid with an extraction solvent, and performing ultrasonic extraction after shaking; purifying the supernatant, performing high performance liquid chromatography, and collecting chromatographic fingerprints of the test sample and the standard sample; the extraction solvent is a mixture of water and alcohols, the alcohols are methanol or ethanol, and the volume ratio of the water to the alcohols is (1-5) 1;
performing original data information processing on the chromatographic fingerprint, dividing chromatographic peaks into two types of large peaks and small peaks, and calculating the relative percentage deviation value of the large peaks of the test sample and the standard sample to obtain large peak deviation values; 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 between the small peak and the standard sample; 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 10% or less;
judging the consistency 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;
the tolerance control criteria are divided into the following four categories:
class I: the deviation value of a large peak is less than or equal to 20%, and the cosine value of a small peak included angle is more than or equal to 0.95;
class II: the large peak deviation value is less than or equal to 25%, and the cosine value of the small peak included angle is more than or equal to 0.90;
class III: the deviation value of a large peak is less than or equal to 30%, and the cosine value of a small peak included angle is more than or equal to 0.85;
class IV: a large peak deviation value >30% and a small peak included angle cosine value <0.85;
the method for judging the coincidence of the test sample specifically comprises the following steps:
in accordance with the said tolerance control criteria,
the internal quality of the tobacco feed liquid meeting the I-class or II-class standard is basically consistent with that of a standard sample, and the quality is good;
the tobacco material liquid meeting III class standard has certain difference between the internal quality and the standard sample and has general stability;
tobacco feed liquid meeting IV standard has more severe quality change;
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 injection 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% -0.05% hydrochloric acid, and the mobile phase B is acetonitrile;
the flow rate is 0.1-1.0 mL/min;
gradient elution.
2. The quality inspection method according to claim 1, wherein the ratio of the tobacco feed liquid to the extraction solvent in g/mL is (0.1-1): (1-100).
3. The quality inspection method according to claim 1, wherein the ultrasonic extraction time is 5-20 min.
4. The quality assurance method according to claim 1, wherein the purification comprises SPE-passing columns and filtration membranes.
5. The method according to any one of claims 1 to 4, wherein the test sample is a bid sample or a lot-to-lot sample.
Priority Applications (1)
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