Method and system for determining aroma components of essence
Through the multi-dimensional analysis system of liquid chromatography-gas chromatography-supercritical fluid chromatography, the problem of separation of complex flavor components is solved, the comprehensive identification of flavor components is achieved, and the accuracy and reliability of the identification results are improved.
Patent Information
- Application Number
- CN202511039389.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-28
- Publication Date
- 2025-08-29
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The prior art is difficult to effectively separate aroma components with large polarity differences and similar structures in complex fragrances, resulting in the inability to accurately obtain volatile and non-volatile components information, affecting the identification accuracy of the source of fragrance raw materials, formula composition and production process.
A multi-dimensional analysis system for liquid chromatography-gas chromatography-supercritical fluid chromatography was constructed. Through preliminary separation based on polarity differences in liquid chromatography, secondary separation based on boiling point differences in gas chromatography, and fine separation of supercritical fluid chromatography, combined with feature extraction and pattern recognition analysis, a fingerprint database was established, and CCP control point verification was carried out.
The comprehensive separation and identification of flavor ingredients is achieved, the reliability and accuracy of the identification results are improved, the source of raw materials and formula characteristics can be accurately judged, and the requirements of high-precision analysis are met.
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Figure CN120559145A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of flavor quality identification, and in particular to a method and system for determining flavor aroma components. Background Art
[0002] In the flavor and fragrance industry, accurate determination of flavor aroma components is crucial for identifying the raw material source, formulation composition, and production process of a flavor. Traditional aroma component determination methods, such as single liquid chromatography, gas chromatography, or supercritical fluid chromatography, struggle to effectively separate components with significant polarity differences and similar structures within complex flavor systems due to their single separation mechanism. This results in an inability to accurately obtain complete information on the volatile and non-volatile components in a flavor, hindering the accurate identification of the flavor raw material source, formulation composition, or production process.
[0003] Existing two-dimensional coupling technologies, such as liquid chromatography-gas chromatography, have improved separation capabilities to a certain extent. However, for complex flavor components with a wide polarity range and large boiling point differences, there is still a problem of insufficient separation dimension. It is difficult to completely separate similar flavor components that are originally difficult to separate, and cannot meet the industry's demand for high-precision flavor component analysis. Summary of the Invention
[0004] In view of the deficiencies in the prior art, the present invention provides a method and system for measuring the aroma components of essences, which solve the problems mentioned in the above background technology.
[0005] To achieve the above objectives, the present invention is implemented through the following technical solutions: A method for determining the aroma components of an essence, comprising the following steps: S1: constructing a liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional coupled analysis system, the system comprising a liquid chromatography system, a gas chromatography system, and a supercritical fluid chromatography system connected in sequence; S2: Using the liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional coupled analysis system, separating and detecting flavor samples of different sources or formulations to obtain multidimensional chromatographic data containing volatile and non-volatile components; S3: performing feature extraction and pattern recognition analysis on the multidimensional chromatographic data to establish a fingerprint library characterizing the characteristics of a specific flavor; S4: Using the liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional coupled analysis system to detect the flavor sample to be tested, comparing the test data with the fingerprint library to identify the raw material source, formula composition or production process of the flavor to be tested; S5: CCP control point verification is performed on the identification results. The CCP control point verification includes the raw material purchase acceptance data, weighing and preparation records or the verification of filtration and deslagging effects. CCP control point verification refers to the process of significantly reducing or eliminating biological, chemical and physical hazards through control measures during food production, processing or storage.
[0006] Preferably, in step S1, constructing the liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional coupled analysis system comprises: A liquid chromatography device is provided, wherein the device comprises a C18 reverse phase chromatography column and a gradient elution component; The liquid chromatography device is connected to a gas chromatography device via a thermal desorption inlet, wherein the gas chromatography device comprises a PEG-20M or DB-5MS capillary column; The gas chromatography device is connected to a supercritical fluid chromatography device through a pressure regulating valve interface. The supercritical fluid chromatography device includes a silica gel column or a C18 bonded phase column and a CO2 fluid control system.
[0007] Preferably, in step S2, the separation and detection step includes: Liquid chromatography primary separation: Use water and acetonitrile as mobile phases, and elute according to a gradient program: acetonitrile concentration increases from 5% to 30% in 0-5 minutes, increases to 80% in 5-15 minutes, and maintains at 80% for 15-20 minutes, and collects liquid fractions; Gas chromatography re-separation: maintain the initial temperature at 40-60°C for 1-3 minutes, then increase the temperature to 250-300°C at a rate of 5-15°C / min, and cut the gas phase fraction based on the total ion current of the mass spectrometer; Supercritical fluid chromatography separation: using CO2 as the fluid and adding 2-5% methanol as a modifier, separation is performed at a pressure of 10-20 MPa and a temperature of 40-60°C. The back pressure regulator controls the outlet pressure at 8-15 MPa.
[0008] Preferably, in step S3, the feature extraction and pattern recognition analysis includes: Integrate liquid chromatography retention time, gas chromatography retention index, and supercritical fluid chromatography elution order into a three-dimensional coordinate system; Least squares discriminant analysis is used to reduce the dimensionality of multidimensional data; The characteristic peaks with significant differences were screened as characteristic markers by variance analysis.
[0009] Preferably, the integration process of the three-dimensional coordinate system includes: Standardize liquid chromatography retention time, gas chromatography retention index, and supercritical fluid chromatography elution order to eliminate dimension differences; A three-dimensional coordinate system was established with the standardized liquid chromatography retention time as the X-axis, the gas chromatography retention index as the Y-axis, and the supercritical fluid chromatography elution order as the Z-axis; The retention time, retention index, and elution order of the same aroma component in the three chromatograms are correlated to generate corresponding three-dimensional coordinate points, thus forming the multidimensional characteristic coordinates of the component.
[0010] Preferably, in step S4, the comparison and identification includes: Calculate the Euclidean distance or cosine similarity between the sample to be tested and the samples in the fingerprint database; When the similarity is ≥80%, the tested sample and the corresponding sample are judged to have the same raw material source or formula characteristics; For samples with similarity <80%, the types and relative contents of the different components were further analyzed.
[0011] Preferably, in the liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional coupled analysis system, adjacent chromatography systems are connected via the following interface devices: Thermal desorption inlet for liquid chromatography-gas chromatography: converting liquid fractions into gaseous injection; Pressure regulating valve interface for gas chromatography-supercritical fluid chromatography: controls the flow rate and pressure of gas fractions entering the supercritical fluid chromatography system.
[0012] Preferably, the water used in the initial separation of liquid chromatography is prepared by adding 0.1% formic acid to pure water in terms of volume percentage, which is used to adjust the pH of the mobile phase and enhance the separation effect of polar aroma components; The methanol modifier used in the supercritical fluid chromatography separation refers to the addition of 2-5% methanol by volume to a system with CO2 as the supercritical fluid, which improves the separation efficiency of non-polar and medium-polar aroma components by changing the polarity and solubility of the supercritical fluid.
[0013] A system for measuring aroma components of an essence, comprising: Detection module: Use liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional combined analysis technology to separate and detect flavor samples and test samples to obtain multidimensional chromatographic data; Analysis module: performing feature extraction and pattern recognition analysis on the multidimensional chromatographic data and establishing a fingerprint database; Identification module: compares the multidimensional chromatographic analysis data of the sample to be tested with the fingerprint library and outputs the identification results.
[0014] Preferably, the detection module includes: Liquid chromatography unit equipped with a C18 reverse phase column and gradient elution assembly; Gas chromatography unit equipped with a PEG-20M or DB-5MS capillary column and a programmed temperature device; Supercritical fluid chromatography unit equipped with a CO2 fluid control system, back pressure regulator, and silica / C18 bonded phase column; The interface device unit includes a thermal desorption inlet and a pressure regulating valve.
[0015] In summary, this application includes at least one of the following beneficial technical effects: 1. The present invention utilizes a liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional coupled analysis system. Utilizing liquid chromatography for primary separation based on polarity differences, gas chromatography for secondary separation based on boiling point differences, and supercritical fluid chromatography for fine separation with its unique solubility and mass transfer properties, this triple separation mechanism effectively addresses the challenge of separating aroma components with similar structures. Compared to traditional technologies, its resolution is significantly improved, enabling complete acquisition of information on both volatile and non-volatile components in fragrances, providing a comprehensive data foundation for subsequent identification. 2. By performing feature extraction and pattern recognition analysis on multidimensional chromatographic data and establishing a fingerprint library, the system integrates data from different chromatographic dimensions using a three-dimensional coordinate system to deeply explore the characteristics of fragrance ingredients. The flavor sample data to be tested is compared with the fingerprint library, and the similarity between the two is calculated. When the similarity reaches a set threshold, the raw material source or formulation characteristics can be accurately determined. For samples that do not reach the threshold, the type and content of the differential components are analyzed to further achieve precise identification, significantly improving the reliability of the identification results. BRIEF DESCRIPTION OF THE DRAWINGS
[0016] Figure 1 It is a schematic diagram of the process of the present invention. DETAILED DESCRIPTION
[0017] The following is combined with Figure 1 , further details of this application are given.
[0018] Example: The embodiment of the present invention provides a method for determining the aroma components of an essence, comprising the following steps: S1: Constructing a liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional coupled analysis system, which includes a liquid chromatography system, a gas chromatography system, and a supercritical fluid chromatography system connected in sequence; S2: Using a liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional coupled analysis system, fragrance samples from different sources or formulations are separated and tested to obtain multidimensional chromatographic data containing volatile and non-volatile components; S3: Perform feature extraction and pattern recognition analysis on multidimensional chromatographic data to establish a fingerprint library that characterizes the characteristics of specific flavors; S4: Use a liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional coupled analysis system to test the flavor sample, compare the test data with the fingerprint library, and identify the raw material source, formula composition or production process of the flavor to be tested; S5: CCP control point verification is performed on the identification results. CCP control point verification includes the verification of raw material incoming acceptance data, weighing and preparation records or filtration and deslagging effects. CCP stands for Critical Control Point in English and its Chinese translation is Critical Hazard Point. CCP control point verification refers to the link in the food production, processing or storage process where biological, chemical and physical hazards are significantly reduced or eliminated through control measures. CCP control point verification forms a "result-process" double verification chain by verifying the raw material incoming acceptance data (tracing the source of ingredients), weighing and preparation records (verifying the consistency of formula execution) and filtration and deslagging effects (confirming the compliance of impurity control) with the ingredient characteristic data obtained by LC-GC-SFC multidimensional chromatography detection. That is, by cross-comparing the data of the entire production process with the test results, problems such as raw material deterioration, preparation deviation or process abnormality are located, and the identification conclusion is revised to ensure the accuracy and traceability of the identification of the source of flavor raw materials, formula composition and production process.
[0019] Specifically, liquid chromatography (LC) performs preliminary separation based on the polarity differences of substances, with components with strong polarity eluting first and components with weak polarity eluting later; gas chromatography (GC) performs secondary separation based on differences in the boiling points of substances, with low-boiling-point substances being vaporized and separated first and high-boiling-point substances being separated later; supercritical fluid chromatography (SFC) utilizes the characteristics of supercritical fluids, which have both high solubility for liquids and high diffusivity for gases, to achieve fine separation of complex components. After completing sample separation and testing, feature extraction and pattern recognition analysis are performed on multi-dimensional chromatographic data to establish a fingerprint library that aggregates the component characteristic information of specific flavors. Subsequently, the test data of the flavor samples to be tested are compared with the fingerprint library, combined with CCP control point verification, and multiple links such as raw materials and preparation processes are checked to ensure the reliability of the identification results. The multidimensional coupling system breaks through the bottleneck of the limited separation capability of a single chromatographic technology, and can comprehensively obtain information on the volatile and non-volatile components in flavors, solving the problem of difficult separation and detection of complex flavor components.
[0020] In step S1, constructing a liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional coupled analysis system includes: A liquid chromatography device is configured, wherein the device includes a C18 reverse phase chromatography column and a gradient elution component; The liquid chromatography device is connected to the gas chromatography device via a thermal desorption inlet, and the gas chromatography device contains a PEG-20M or DB-5MS capillary column; The gas chromatography device is connected to the supercritical fluid chromatography device through a pressure regulating valve interface. The supercritical fluid chromatography device includes a silica gel column or a C18 bonded phase column and a CO2 fluid control system.
[0021] Specifically, the C18 reverse phase chromatography column retains non-polar or weakly polar substances through hydrophobic interaction, and the gradient elution component can flexibly adjust the composition of the mobile phase to separate components of different polarity under appropriate conditions. The thermal desorption inlet heats and vaporizes the liquid fraction and transfers it to the gas chromatography device. The PEG-20M or DB-5MS capillary column further separates the components based on the difference in the distribution coefficient of the substance in the stationary phase and the mobile phase. The pressure regulating valve interface ensures the stability of the pressure between the gas chromatography device and the supercritical fluid chromatography device. The silica gel column or C18 bonded phase column in the supercritical fluid chromatography device is combined with the CO2 fluid control system to utilize the special properties of the CO2 fluid in the supercritical state to achieve efficient separation of complex components.
[0022] Clarifying the specific composition and function of each device and connecting component ensures the stability and efficiency of the multidimensional coupling system. The combination of a C18 reversed-phase column and gradient elution assembly enhances the separation capability of liquid chromatography for complex samples. The thermal desorption inlet and pressure regulating valve interface ensure smooth fraction transfer and pressure matching between different chromatographic devices, reducing component loss and analytical errors. The special configuration of the supercritical fluid chromatography device enhances the separation of difficult-to-separate substances, enabling the entire coupling system to more accurately separate flavor components and provide high-quality data for subsequent analysis.
[0023] In step S2, the separation and detection step includes: Liquid chromatography primary separation: Use water and acetonitrile as mobile phases, and elute according to a gradient program: acetonitrile concentration increases from 5% to 30% in 0-5 minutes, increases to 80% in 5-15 minutes, and maintains at 80% for 15-20 minutes, and collects liquid fractions; Gas chromatography re-separation: maintain the initial temperature at 40-60°C for 1-3 minutes, then increase the temperature to 250-300°C at a rate of 5-15°C / min, and cut the gas phase fraction based on the total ion current of the mass spectrometer; Supercritical fluid chromatography separation: using CO2 as the fluid and adding 2-5% methanol as a modifier, separation is performed at a pressure of 10-20 MPa and a temperature of 40-60°C. The back pressure regulator controls the outlet pressure at 8-15 MPa.
[0024] Specifically, liquid chromatography's gradient elution improves the separation efficiency of polar components; gas chromatography's programmed temperature effectively separates components with different boiling points; and supercritical fluid chromatography, through modifiers and pressure and temperature control, enhances the separation of complex components. The synergistic effect of these three techniques enables efficient and comprehensive separation and detection of various aroma components in fragrances, obtaining detailed and accurate compositional information, fully leveraging the advantages of different chromatographic techniques.
[0025] In step S3, feature extraction and pattern recognition analysis include: Integrate liquid chromatography retention time, gas chromatography retention index, and supercritical fluid chromatography elution order into a three-dimensional coordinate system; Least squares discriminant analysis is used to reduce the dimensionality of multidimensional data; The characteristic peaks with significant differences were screened as characteristic markers by variance analysis.
[0026] Specifically, when integrating the liquid chromatography retention time, gas chromatography retention index, and supercritical fluid chromatography elution order into a three-dimensional coordinate system, a hybrid algorithm combining Z-score normalization and minimum-maximum normalization is used to address the characteristic differences of the three types of chromatographic data: Liquid chromatography retention time ; in, and are the mean and standard deviation of the retention time of all samples, respectively, which are dimensionless and retain the distribution characteristics through Z-score; Gas chromatography retention index ; Directly use the minimum-maximum normalization to map the retention index to the [0,1] interval to ensure consistency with other dimension scales; Supercritical fluid chromatography elution order ; in, For the total number of peaks, the discrete elution order is converted into a continuous value to avoid the influence of the ordinal number on the distance calculation; Three-dimensional coordinate construction: the standardized 、 、 As 、 、 Axis coordinates, forming a unique three-dimensional coordinate point , each point represents a multidimensional separation feature of a specific component.
[0027] The establishment of a three-dimensional coordinate system realizes the multi-dimensional expression of the characteristics of flavor ingredients. Compared with single-dimensional information, it can reflect the characteristics of ingredients more comprehensively and accurately. The data processing methods of least squares discriminant analysis and variance analysis improve the data processing efficiency and the accuracy of feature extraction. It can quickly screen out key characteristic markers from complex multi-dimensional chromatographic data, providing a reliable basis for the establishment of an accurate fingerprint library, thereby improving the efficiency and accuracy of flavor identification analysis.
[0028] The integration process of the three-dimensional coordinate system includes: Standardize liquid chromatography retention time, gas chromatography retention index, and supercritical fluid chromatography elution order to eliminate dimension differences; A three-dimensional coordinate system was established with the standardized liquid chromatography retention time as the X-axis, the gas chromatography retention index as the Y-axis, and the supercritical fluid chromatography elution order as the Z-axis; The retention time, retention index, and elution order of the same aroma component in the three chromatograms are correlated to generate corresponding three-dimensional coordinate points, thus forming the multidimensional characteristic coordinates of the component.
[0029] Specifically, through standardization processing and coordinate system establishment, the problem of fusing different chromatographic data was effectively solved, so that multidimensional chromatographic data can be presented in an intuitive and accurate manner. The generation of three-dimensional coordinate points realizes the quantification and precise expression of the characteristics of flavor components, providing an accurate data basis for subsequent comparison and identification based on the fingerprint library, which helps to more accurately distinguish the composition differences of different flavors and improve the accuracy and reliability of flavor identification analysis.
[0030] In step S4, the comparison and identification includes: Calculate the Euclidean distance or cosine similarity between the sample to be tested and the samples in the fingerprint database; When the similarity is ≥80%, the tested sample and the corresponding sample are judged to have the same raw material source or formula characteristics; For samples with similarity <80%, the types and relative contents of the different components were further analyzed.
[0031] Specifically, the Euclidean distance or cosine similarity between the sample to be tested and the samples in the fingerprint library is calculated, and the degree of similarity between the two is measured by quantitative indicators. When the similarity reaches a certain standard, it is determined that the sample to be tested and the corresponding sample have the same raw material source or formula characteristics; for samples whose similarity does not meet the standard, the types and relative contents of the different components are further analyzed, and the reasons for the differences are deeply explored from the component level to achieve accurate identification of the flavor. Using Euclidean distance or cosine similarity to calculate similarity provides an objective, quantitative basis for flavor identification, avoiding errors caused by subjective judgment. In-depth analysis of samples that fail to meet similarity standards can uncover subtle differences in composition. Even flavors with similar ingredients can be accurately identified based on their raw material sources or formulations. This significantly improves the accuracy and reliability of flavor identification analysis, meeting the flavor industry's demand for high-precision identification technology.
[0032] In the liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional coupled analysis system, adjacent chromatography systems are connected through the following interface devices: Thermal desorption inlet for liquid chromatography-gas chromatography: converting liquid fractions into gaseous injection; Pressure regulating valve interface for gas chromatography-supercritical fluid chromatography: controls the flow rate and pressure of gas fractions entering the supercritical fluid chromatography system.
[0033] Specifically, the configuration of the thermal desorption inlet and the pressure regulating valve interface solves the difficult problem of fraction transfer and pressure matching between different chromatographic systems: the thermal desorption inlet uses direct vaporization and inert surface treatment technology to efficiently convert liquid fractions into gas and accurately introduce them into the gas chromatograph, significantly reducing component adsorption loss and peak broadening problems; the pressure regulating valve interface uses multi-stage back pressure regulation and dynamic flow rate control mechanisms to achieve a smooth transition between the low pressure of gas chromatography and the high pressure of supercritical fluid chromatography, effectively eliminating the impact of pressure fluctuations on the separation effect. The two work together to ensure the stable operation of the liquid-gas-supercritical fluid chromatography multidimensional coupling system, ensuring that the analytical accuracy and data reliability of volatile and non-volatile flavor components are maintained during the cross-dimensional separation process.
[0034] The water used in the initial separation of liquid chromatography is prepared by adding 0.1% formic acid to pure water on a volume basis to adjust the pH of the mobile phase and enhance the separation effect of polar aroma components; The methanol modifier used in supercritical fluid chromatography separation refers to the addition of 2-5% methanol by volume to a system with CO2 as the supercritical fluid. By changing the polarity and solubility of the supercritical fluid, the separation efficiency of non-polar and medium-polar aroma components is improved.
[0035] Specifically, 0.1% formic acid is added to the water used in the initial separation of liquid chromatography. Formic acid can adjust the pH of the mobile phase, change the interaction between the solute and the stationary phase, and enhance the separation effect of polar aroma components; 2-5% methanol modifier is added to the supercritical fluid chromatography fine separation. Methanol can change the polarity and solubility of the supercritical fluid, thereby improving the solubility and separation ability of the supercritical fluid for non-polar and medium-polar aroma components, and achieving a more precise separation of complex components. The special configuration of mobile phase and modifier optimizes the separation capabilities of specific polar components at different chromatographic stages. The addition of formic acid to the mobile phase improves the separation efficiency and selectivity of polar components in liquid chromatography, while the methanol modifier enhances the separation of non-polar and moderately polar components in supercritical fluid chromatography. The combination of these two enables the multidimensional coupled system to more comprehensively and efficiently separate aroma components across a wide range of polarities in fragrances, improving the completeness and accuracy of component detection.
[0036] A system for measuring aroma components of an essence, comprising: Detection module: Use liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional combined analysis technology to separate and detect flavor samples and test samples to obtain multidimensional chromatographic data; Analysis module: perform feature extraction, pattern recognition analysis on multidimensional chromatographic data and establish fingerprint database; Identification module: compares the multidimensional chromatographic analysis data of the sample to be tested with the fingerprint library and outputs the identification results.
[0037] The detection module includes: Liquid chromatography unit equipped with a C18 reverse phase column and gradient elution assembly; Gas chromatography unit equipped with a PEG-20M or DB-5MS capillary column and a programmed temperature device; Supercritical fluid chromatography unit equipped with a CO2 fluid control system, back pressure regulator, and silica / C18 bonded phase column; The interface device unit includes a thermal desorption inlet and a pressure regulating valve.
[0038] Specifically, through modular design, all aspects of flavor component analysis are integrated, achieving automation and systematization from sample detection to result output. The detection module ensures accurate and comprehensive data acquisition; the analysis module efficiently processes data and builds a precise fingerprint library; and the identification module quickly and accurately completes sample identification. The collaborative operation of these modules significantly improves the efficiency and accuracy of flavor component analysis compared to traditional manual analysis methods, reduces human error, and provides a highly efficient and reliable analysis tool for the flavor industry.
[0039] The examples of this specific embodiment are all preferred embodiments of this application and are not intended to limit the scope of protection of this application. Identical components are represented by the same reference numerals. Therefore, any equivalent changes made based on the structure, shape, and principle of this application should be included in the scope of protection of this application.
Claims
1. A method for determining the aroma components of an essence, characterized in that: The following steps are involved: S1: constructing a liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional coupled analysis system, the system comprising a liquid chromatography system, a gas chromatography system, and a supercritical fluid chromatography system connected in sequence; S2: Using the liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional coupled analysis system, separating and detecting flavor samples of different sources or formulations to obtain multidimensional chromatographic data containing volatile and non-volatile components; S3: performing feature extraction and pattern recognition analysis on the multidimensional chromatographic data to establish a fingerprint library characterizing the characteristics of a specific flavor; S4: Using the liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional coupled analysis system to detect the flavor sample to be tested, comparing the test data with the fingerprint library to identify the raw material source, formula composition or production process of the flavor to be tested; S5: CCP control point verification is performed on the identification results. The CCP control point verification includes the raw material purchase acceptance data, weighing and preparation records or the verification of filtration and deslagging effects. CCP control point verification refers to the process of significantly reducing or eliminating biological, chemical and physical hazards through control measures during food production, processing or storage.
2. The method for determining the aroma components of essence according to claim 1, wherein: In step S1, constructing the liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional coupled analysis system includes: A liquid chromatography device is provided, wherein the device comprises a C18 reverse phase chromatography column and a gradient elution component; The liquid chromatography device is connected to a gas chromatography device via a thermal desorption inlet, wherein the gas chromatography device comprises a PEG-20M or DB-5MS capillary column; The gas chromatography device is connected to a supercritical fluid chromatography device through a pressure regulating valve interface. The supercritical fluid chromatography device includes a silica gel column or a C18 bonded phase column and a CO2 fluid control system.
3. The method for determining the aroma components of essence according to claim 1, wherein: In step S2, the separation and detection step includes: Liquid chromatography primary separation: Use water and acetonitrile as mobile phases, and elute according to a gradient program: acetonitrile concentration increases from 5% to 30% in 0-5 minutes, increases to 80% in 5-15 minutes, and maintains at 80% for 15-20 minutes, and collects liquid fractions; Gas chromatography re-separation: maintain the initial temperature at 40-60°C for 1-3 minutes, then increase the temperature to 250-300°C at a rate of 5-15°C / min, and cut the gas phase fraction based on the total ion current of the mass spectrometer; Supercritical fluid chromatography separation: using CO2 as the fluid and adding 2-5% methanol as a modifier, separation is performed at a pressure of 10-20 MPa and a temperature of 40-60°C. The back pressure regulator controls the outlet pressure at 8-15 MPa.
4. The method for determining the aroma components of essence according to claim 1, wherein: In step S3, the feature extraction and pattern recognition analysis includes: Integrate liquid chromatography retention time, gas chromatography retention index, and supercritical fluid chromatography elution order into a three-dimensional coordinate system; Least squares discriminant analysis is used to reduce the dimensionality of multidimensional data; The characteristic peaks with significant differences were screened as characteristic markers by variance analysis.
5. The method for determining the aroma components of essence according to claim 4, characterized in that: The integration process of the three-dimensional coordinate system includes: Standardize liquid chromatography retention time, gas chromatography retention index, and supercritical fluid chromatography elution order to eliminate dimension differences; A three-dimensional coordinate system was established with the standardized liquid chromatography retention time as the X-axis, the gas chromatography retention index as the Y-axis, and the supercritical fluid chromatography elution order as the Z-axis; The retention time, retention index, and elution order of the same aroma component in the three chromatograms are correlated to generate corresponding three-dimensional coordinate points, thus forming the multidimensional characteristic coordinates of the component.
6. The method for determining the aroma components of essence according to claim 1, characterized in that: In step S4, the comparison and identification includes: Calculate the Euclidean distance or cosine similarity between the sample to be tested and the samples in the fingerprint database; When the similarity is ≥80%, the tested sample and the corresponding sample are judged to have the same raw material source or formula characteristics; For samples with similarity <80%, the types and relative contents of the different components were further analyzed.
7. The method for determining the aroma components of essence according to claim 1, characterized in that: In the liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional coupled analysis system, adjacent chromatography systems are connected via the following interface devices: Thermal desorption inlet for liquid chromatography-gas chromatography: converting liquid fractions into gaseous injection; Pressure regulating valve interface for gas chromatography-supercritical fluid chromatography: controls the flow rate and pressure of gas fractions entering the supercritical fluid chromatography system.
8. The method for determining the aroma components of essence according to claim 3, characterized in that: The water used in the initial separation of the liquid chromatography is prepared by adding 0.1% formic acid to pure water in terms of volume percentage, which is used to adjust the pH of the mobile phase and enhance the separation effect of polar aroma components; The methanol modifier used in the supercritical fluid chromatography separation refers to the addition of 2-5% methanol by volume to a system with CO2 as the supercritical fluid, which improves the separation efficiency of non-polar and medium-polar aroma components by changing the polarity and solubility of the supercritical fluid.
9. A system for measuring the aroma components of an essence, characterized in that: A method for determining the aroma components of an essence according to any one of claims 1 to 8, comprising: Detection module: Use liquid chromatography-gas chromatography-supercritical fluid chromatography multidimensional combined analysis technology to separate and detect flavor samples and test samples to obtain multidimensional chromatographic data; Analysis module: performing feature extraction and pattern recognition analysis on the multidimensional chromatographic data and establishing a fingerprint database; Identification module: compares the multidimensional chromatographic analysis data of the sample to be tested with the fingerprint library and outputs the identification results.
10. The system for measuring flavor and aroma components according to claim 9, characterized in that: The detection module includes: Liquid chromatography unit equipped with a C18 reverse phase column and gradient elution assembly; Gas chromatography unit equipped with a PEG-20M or DB-5MS capillary column and a programmed temperature device; Supercritical fluid chromatography unit equipped with a CO2 fluid control system, back pressure regulator, and silica / C18 bonded phase column; The interface device unit includes a thermal desorption inlet and a pressure regulating valve.
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