Quantitative determination method for volatile components in food and / or medicinal materials
By employing a multiple headspace extraction-gas chromatography-mass spectrometry (HCGS) method, the complexity and accuracy issues of quantitative determination of volatile components in food and medicinal materials in existing technologies have been resolved. This method enables the determination of the absolute content of volatile components in food and medicinal materials, and is suitable for quality control of food and medicinal materials.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-20
- Publication Date
- 2026-03-20
AI Technical Summary
Existing methods for the quantitative determination of volatile components in food and medicinal materials are cumbersome, inefficient, prone to loss of volatile components, and can only measure relative content. There is a lack of simple, rapid, and environmentally friendly methods for determining absolute content.
Multiple headspace extraction-gas chromatography-mass spectrometry was used to analyze volatile component standard samples and food/medicinal powder samples. The absolute content of volatile components was calculated by combining linear regression and standard curve method.
It enables a simple, rapid, accurate, and environmentally friendly absolute content determination of volatile components in food and medicinal materials, making up for the shortcomings of relative content determination and suitable for quality control of food and medicinal materials.
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Figure CN121703291A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of chemical composition analysis technology for food and medicinal materials, and in particular to a method for quantitative determination of volatile components in food and / or medicinal materials. Background Technology
[0002] The study of volatile components in food and medicinal materials is a highly valuable interdisciplinary field. These trace "aroma molecules" offer far more than just flavor; they hold immense scientific and applied potential. For example, in coffee, understanding the changes in volatile components under different roasting conditions can help producers optimize roasting processes, precisely control the flavor profile of coffee, and improve its quality.
[0003] Wild chrysanthemum, a perennial herbaceous plant of the Asteraceae family, is considered both food and medicine. It possesses high medicinal value, with effects including clearing heat and detoxifying, improving eyesight, and lowering blood pressure. Dried wild chrysanthemum contains approximately 0.5% volatile oil. More than 60 compounds have been identified in the volatile oil of wild chrysanthemum. Due to differences in origin and extraction methods, the composition of their volatile oils varies considerably. Common components include camphor, borneol, and xanthocyanin.
[0004] In recent years, most studies on volatile components in food and medicinal materials have used a combination of chromatographic analysis and area normalization to perform relative quantitative determination of volatile components. The few studies that use standard curve methods for absolute content determination also involve extracting volatile components from food and medicinal materials with solvents before measurement.
[0005] The area normalization method assumes that all components in the sample respond to the detector and that all compounds have the same quantitative correction factor; therefore, it is only a relative content determination method. In practical experiments, it is often necessary to know the absolute content of the analyte, requiring methods such as the standard curve method or the standard addition method. Traditional extraction methods typically require large amounts of solvent, have low extraction efficiency, are cumbersome, and time-consuming. Furthermore, due to the long sample exposure time during extraction, some volatile components are significantly lost, leading to a certain degree of distortion in sample information. Given these problems, there is an urgent need to establish simpler, faster, more selective, widely applicable, inexpensive, and environmentally friendly sample pretreatment methods for the quantitative analysis of volatile components in food and medicinal materials.
[0006] Headspace extraction (HME) is a novel method for analyzing volatile substances in a sample matrix. It offers advantages such as low sample volume requirements, minimal or no sample preparation, solvent-free operation, and environmental friendliness. Headspace analysis can be categorized into static and dynamic headspace analysis. In addition, there are auxiliary techniques based on headspace principles, such as headspace-solid phase microextraction (HPE) and multiple headspace extraction (MHE). Multiple headspace extraction (MHE), also known as multi-stage headspace extraction, is a special type of static headspace technique that involves repeatedly sampling and analyzing the same sample from the headspace until the target analyte is no longer detectable. Theoretically, the sum of the target analyte concentrations measured in each extraction should equal the total amount of that component in the original sample. In practice, however, an unlimited number of extractions is not typically performed. Instead, the initial total amount of the analyte in the sample is calculated using mathematical models based on the peak area data obtained from a finite number of consecutive extractions.
[0007] According to literature review, there are currently no reports on the direct determination of volatile components in solid samples such as food and medicinal materials using multiple headspace extraction-gas chromatography-mass spectrometry. Summary of the Invention
[0008] The purpose of this invention is to overcome the deficiencies of the prior art and provide a quantitative determination method for volatile components in food and / or medicinal materials, specifically involving a method for determining the absolute content of volatile components such as borneol and camphor, particularly a method for determining the absolute content of borneol and camphor in wild chrysanthemum and other similar materials. This invention achieves a simple, rapid, accurate, and environmentally friendly determination of the absolute content of volatile components in solid samples of food and medicinal materials through multiple headspace extraction-gas chromatography-mass spectrometry.
[0009] This invention can be achieved through the following technical solutions: The purpose of this invention is to provide a method for quantitative determination of volatile components in food and / or medicinal materials, the method comprising the following steps: The volatile component standard sample was sealed in a headspace vial, and the total peak area corresponding to the volatile component in the volatile component standard sample was measured and calculated by multiple headspace extraction-gas chromatography-mass spectrometry. The food and / or medicinal powder to be tested is sealed in a headspace vial. The total peak area corresponding to the volatile components in the food and / or medicinal powder is measured and calculated by multiple headspace extraction-gas chromatography-mass spectrometry. The absolute content of the volatile components in the food and / or medicinal powder is obtained by comparing and calculating with the standard sample of volatile components.
[0010] Furthermore, the preparation process of the volatile component standard sample includes the following steps: Weigh out the solid sample of volatile components and anhydrous magnesium sulfate, transfer them to an agate mortar, grind them, and obtain a mixture; Weigh out a portion of the mixture, discard the rest, add anhydrous magnesium sulfate, and grind.
[0011] Furthermore, the calculation of the total peak area corresponding to the volatile components in the volatile component standard sample or the total peak area corresponding to the volatile components in the food and / or medicinal powder to be tested includes the following process: Further calculations of the first-order mechanism of multiple headspace extraction yield the following results: ,in A i For the first i Peak area during the second extraction, index q This is an indicator to describe the exponential decrease in peak area during multiple headspace extraction processes. i This represents the number of extractions. This is... Linear equations of type, where The slope is The y-intercept is The peak areas obtained from the continuous extraction of volatile components from standard samples or food and / or medicinal powders are processed using the above formula and subjected to linear regression to obtain the desired peak area. as well as Substitution The total peak area corresponding to the volatile components in the standard sample or the total peak area corresponding to the volatile components in the food and / or medicinal powder to be tested can be calculated.
[0012] Furthermore, in the quantitative determination method, standard samples of volatile components of different masses are sealed in headspace vials, and the total peak area corresponding to the volatile components in the standard samples of different masses is measured and calculated by multiple headspace extraction-gas chromatography-mass spectrometry. The total peak area corresponding to the volatile component standard sample is plotted against the mass of the sample, and the data is linearly fitted by the least squares method to obtain the standard curves of all volatile component standard samples of different masses, so as to verify the feasibility.
[0013] Furthermore, the process of measuring and calculating the total peak area corresponding to the volatile components in the volatile component standard sample includes the following steps: The total ion current chromatogram of the volatile component standard sample was measured. The total ion current chromatogram of the volatile component standard sample was analyzed by the standard mass spectrometry library to identify the chromatographic peak of the volatile component to be tested. The chromatographic peak of the volatile component to be tested was integrated to obtain the peak area of the volatile component to be tested. The total peak area corresponding to the volatile component in the volatile component standard sample was calculated.
[0014] Furthermore, the process of measuring and calculating the total peak area corresponding to the volatile components in the volatile components of the food and / or medicinal powder to be tested includes the following steps: The total ion current chromatogram of the food and / or medicinal powder to be tested is obtained by measurement. The total ion current chromatogram of the food and / or medicinal powder to be tested is analyzed by using a standard mass spectrometry library to identify the chromatographic peaks of the volatile components to be tested. The chromatographic peaks of the volatile components to be tested are integrated to obtain the peak area of the volatile components to be tested. The total peak area corresponding to the volatile components in the food and / or medicinal powder to be tested is calculated.
[0015] Furthermore, the food and / or medicinal material is wild chrysanthemum.
[0016] Furthermore, the volatile components include one or more of borneol, camphor, etc.
[0017] Furthermore, this invention provides a method for the quantitative determination of volatile components in food and / or medicinal materials. The method involves directly sealing a volatile sample (i.e., a standard sample of volatile components) in a headspace vial, measuring and calculating the peak area of the volatile components in the sample using multiple headspace extraction-gas chromatography-mass spectrometry methods; then, after measuring and calculating the peak area of the volatile components in the food or medicinal material powder, directly calculating the absolute content of the volatile components in the food or medicinal material. The specific operating steps are as follows: (1) Preparation of solid standard samples: Accurately weigh 10-30 mg of solid samples such as borneol and camphor, and 10 g of anhydrous magnesium sulfate, transfer them to an agate mortar, and grind for a certain time to obtain a mixture; weigh a portion of the mixture (1-10% of the total mass of the mixture), discard the rest, add a certain amount of anhydrous magnesium sulfate (2-10 times the mass of the weighed portion), grind for a certain time to obtain solid standard samples, i.e., standard samples of volatile components. The grinding time for each time is 3-15 min.
[0018] (2) Testing of solid standard samples: Accurately weigh 10, 20, 40, 60, 80, and 100 mg of the above solid standard samples and transfer them to 6 headspace vials, then seal them. Analyze the samples using multiple headspace extraction-gas chromatography-mass spectrometry (GC-MS) under the selected conditions. Each sample is injected multiple times consecutively. After each sampling, the headspace portion of the headspace vial is vented to restore the pressure of the headspace vial to atmospheric pressure.
[0019] (3) Theoretical calculation of peak area: The first-order mechanism of multiple headspace extraction (a mathematical model based on first-order reaction kinetics, based on the key assumption that the amount of substance escaping from the sample and entering the headspace phase during each extraction (sampling) is proportional to the amount of that component remaining in the sample at that time, assuming that the change in concentration over time conforms to first-order reaction kinetics, this theory follows the formula: - DC / dt = kc Further calculations yield the following results: ,in A i For the first i Peak area during the second extraction. A 1 represents the peak area during the first extraction, and the index is... q This is an indicator to describe the exponential decrease in peak area during multiple headspace extraction processes. i This represents the number of extractions. This is... Linear equations of type, where The slope is The y-intercept is The peak areas obtained from the continuous extraction of volatile substances (volatile components) from solid standard samples can be processed using the above formula and subjected to linear regression to obtain the... as well as Substitution The total peak area corresponding to the volatile components in the solid standard sample can be calculated.
[0020] (4) Establishment of solid standard curves: Plot the total peak area of the solid standard sample against the mass of the solid standard sample. Perform linear fitting of the data using the least squares method to obtain the standard curves for all solid standard samples, in order to verify the feasibility of the method.
[0021] (5) Detection of volatile components in food and medicinal materials: Accurately weigh a certain amount of food and / or medicinal materials, pulverize them with a pulverizer, and immediately take 40-100 mg of sample into a headspace vial, seal it, and analyze it under selected conditions by multiple headspace extraction-gas chromatography-mass spectrometry. Calculate the total peak area corresponding to the volatile components in the powder of the food and / or medicinal materials to be tested, compare it with the solid standard sample, and calculate to obtain the absolute content of volatile components in the food and medicinal materials.
[0022] Further, after step (5), perform the following step (6): (6) Confirmation of the volatile components to be tested: The NIST 11 standard mass spectrum library was searched by a chemical workstation and analyzed to confirm the chromatographic peaks of the volatile components to be tested. This is a qualitative analysis.
[0023] Furthermore, the preferred specific operational steps for selecting the conditions are as follows: Multiple headspace extractions: headspace equilibrium temperature 80-110°C o C, Circulation temperature 90-120 o C, Transmission line temperature 100-130 o C, headspace equilibration time 10-40 min, carrier gas is high-purity helium, sample pressure 10-20 psi, injection time 0.5-2 min.
[0024] Gas chromatography conditions: High-purity helium as carrier gas, flow rate of 0.5-1.2 mL / min, split or splitless injection, HP-5 MS quartz capillary column or similar column, temperature programmed analysis.
[0025] Mass spectrometry conditions: Ion source: EI, electron energy: 65-75 eV, electron multiplier voltage: 910 V-930 V, ion source temperature: 210-240 °C o C, Quadrupole temperature: 145-160°C o C, Scanning mode: Full scan; Quality scan range m / z: 35~500.
[0026] Confirmation of the volatile components to be tested and their peak areas: The chromatographic peaks of the volatile components to be tested were identified by searching the NIST 11 standard mass spectrometry library using a chemistry workstation and analyzing the data; this is the qualitative analysis. The peak areas of the volatile components to be tested were then integrated using the data processing system of the chemistry workstation (chromatographic data workstation) to obtain the peak areas. The total peak area and content of the volatile components to be tested can then be calculated.
[0027] Compared with the prior art, the present invention has the following beneficial effects: 1) The present invention provides a method for quantitative determination of volatile components in food and / or medicinal materials, which is a simpler, faster, more selective, more widely applicable, cheaper and more environmentally friendly sample pretreatment method for quantitative analysis of volatile components in food and medicinal materials.
[0028] 2) The present invention provides a method for quantitative determination of volatile components in food and / or medicinal materials, specifically involving the determination of the absolute content of volatile components such as borneol and camphor, particularly the determination of the absolute content of borneol and camphor in wild chrysanthemum and other materials. The present invention uses a multiple headspace extraction-gas chromatography-mass spectrometry method to simply, rapidly, accurately and environmentally friendly determine the absolute content of volatile components in solid samples of food and medicinal materials.
[0029] 3) This invention is the first to employ multiple headspace extraction-gas chromatography-mass spectrometry (GC-MS) to determine the absolute content of volatile components in wild chrysanthemum, overcoming the limitations of previous methods such as area normalization, which only yielded relative content of volatile components. This method provides a more accurate reflection of the volatile component content in wild chrysanthemum. Furthermore, this method requires a small sample volume and does not use solvents in the determination of wild chrysanthemum samples, making it environmentally friendly. This method can be used for quality control of food, medicinal materials, etc. Attached Figure Description
[0030] Figure 1 The total ion chromatograms are obtained from five consecutive headspace extraction analyses of a solid standard sample.
[0031] Figure 2 For camphor and borneol in solid standard samples x - y ( Linear regression curve.
[0032] Figure 3 This is the standard curve between the total peak area and mass of camphor.
[0033] Figure 4 This is the standard curve relating the total peak area and mass of borneol.
[0034] Figure 5 This is the total ion chromatogram of a solid standard sample.
[0035] Figure 6 The image shows the total ion chromatogram of a wild chrysanthemum sample. Detailed Implementation
[0036] The present invention will now be described in detail with reference to the accompanying drawings and specific embodiments. These embodiments are based on the technical solution of the present invention and provide detailed implementation methods and specific operating procedures. However, the scope of protection of the present invention is not limited to the following embodiments.
[0037] In the specification and claims, the terms "including" and "comprising" should be understood as "including, but not limited to". The specific details disclosed are for the purpose of making the present invention easier to understand. Those skilled in the art who implement this solution using one or more technical details are also considered to be implementing the technical solution of the present invention.
[0038] In this invention, any component models, material names, connection structures, control methods, etc., not explicitly stated are considered common technical features disclosed in the prior art.
[0039] This invention belongs to the field of chemical composition analysis technology of food and medicinal materials, and relates to a quantitative determination method for volatile components in food and / or medicinal materials, and a quality control method for food and medicinal materials. Specifically, it relates to a method for determining the absolute content of volatile components such as borneol and camphor in food and medicinal materials, especially a method for determining the absolute content of borneol and camphor in wild chrysanthemum, which adopts a multiple headspace extraction-gas chromatography-mass spectrometry method. First, a standard sample containing a certain amount of volatile components (such as borneol and camphor) is sealed in a headspace vial. The total peak area is measured and calculated using multiple headspace extraction-gas chromatography-mass spectrometry (GC-MS). Then, the food and / or medicinal powder to be tested (such as wild chrysanthemum) is pulverized and sealed in a headspace vial. The total peak area of the volatile components (borneol and camphor, etc.) in the food and / or medicinal powder (wild chrysanthemum powder) is determined and calculated using multiple headspace extraction-gas chromatography-mass spectrometry (GC-MS). By comparing with the standard sample, the absolute content of volatile components (borneol and camphor, etc.) in the food and / or medicinal powder (wild chrysanthemum powder) can be directly calculated. This invention is the first to use multiple headspace extraction-gas chromatography-mass spectrometry to determine the absolute content of volatile components in food and / or medicinal materials (wild chrysanthemum), overcoming the shortcomings of previous methods such as area normalization, which only yielded relative content of volatile components. This method more accurately reflects the content of volatile components in wild chrysanthemum. Furthermore, this method requires a small sample volume and does not use solvents in the determination of wild chrysanthemum samples, making it environmentally friendly. This method can be used for quality control of food, medicinal materials, etc.
[0040] The following embodiments are only used to further illustrate the present invention and should not be construed as limiting the scope of protection of the present invention. Any non-essential improvements and adjustments made by those skilled in the art based on the principles described in the present invention are within the scope of protection of the present invention.
[0041] Example 1 The purpose of this invention is to overcome the shortcomings of the existing technology and provide a simple, rapid, accurate and environmentally friendly method for determining the absolute content of volatile components in solid samples of food and medicinal materials.
[0042] To achieve the above objectives, this embodiment provides a method for quantitative determination of volatile components in food and / or medicinal materials, wherein the food and / or medicinal material is wild chrysanthemum, and the volatile components include borneol and camphor, comprising the following steps: (1) Preparation of solid standard sample: Accurately weigh 20 mg of camphor, 15 mg of borneol and 10 g of anhydrous magnesium sulfate, transfer them to an agate mortar and grind for 5 min to obtain a mixture; accurately weigh 0.4 g from the mixture, add 1.6 g of anhydrous magnesium sulfate, grind for 5 min to obtain a solid standard sample.
[0043] (2) Testing of solid standard samples: Accurately weigh 10, 20, 40, 60, 80, and 100 mg of the above solid standard samples and transfer them to six 20 mL headspace vials, then seal them. Analyze the samples using multiple headspace extraction-gas chromatography-mass spectrometry (GC-MS) under the selected conditions. Each sample is injected five times consecutively. After each sampling, the headspace portion of the headspace vial is vented to restore the pressure of the headspace vial to atmospheric pressure. Figure 1 The total ion chromatograms are obtained from five consecutive headspace extraction analyses of a solid standard sample.
[0044] (3) Theoretical calculation of peak area: Further calculation of the first-order mechanism of multiple headspace extraction yields the following results. ,in A i For the first i Peak area during the second extraction. A 1 represents the peak area during the first extraction, and the index is... q This is an indicator to describe the exponential decrease in peak area during multiple headspace extraction processes. i This represents the number of extractions. This is... Linear equations of type, where The slope is The y-intercept is The peak area obtained from the continuous extraction of borneol from 100 mg of sample in the solid standard curve was processed and linearly regressed according to the above formula to obtain... Figure 2 ,from Figure 2 It can be obtained from the middle as well as Substitution The total peak area corresponding to the volatile components in the solid standard sample can be calculated. Using the same method, the total peak areas corresponding to the volatile components in 10, 20, 40, 60, and 80 mg samples were obtained.
[0045] (4) Establishment of solid standard curve: Plot the total peak area of all samples against the mass of the samples. Perform linear fitting of the data using the least squares method to obtain the solid standard curve, thereby verifying the feasibility of the method.
[0046] The standard curve equation relating the total peak area and mass of camphor is as follows: y =1.2700×10 8 x +556141; among which x Camphor mass (mg) y The peak area of camphor in the chromatogram; the squared correlation coefficient: R 2 =0.9992; Linear range: 0.004-0.04 mg; Standard curve see Figure 3 The standard curve equation relating the total peak area and mass of borneol is as follows:y =3.3874×10 8 x +229415; of which x Borneol mass (mg) y The peak area of borneol in the chromatogram; the squared correlation coefficient: R 2 =0.9992; Linear range: 0.003-0.03 mg; Standard curve see Figure 4 The linear relationship is good, indicating that the method is feasible.
[0047] (5) Detection of volatile components in wild chrysanthemum samples: Take 10.0 g of wild chrysanthemum, crush it with a pulverizer, and immediately take 50 mg of the sample into a headspace vial. Seal it and analyze it under the selected conditions by multiple headspace extraction-gas chromatography-mass spectrometry. Calculate the total peak area of the volatile components to be tested, compare it with the solid standard sample, and calculate (using the single-point standard curve method, area 1 / area 2 = content 1 / content 2, and if area 1, area 2 and content 1 are known, content 2 can be calculated) to obtain the absolute content of volatile components in wild chrysanthemum.
[0048] (6) The process of confirming the volatile components to be tested and the peak area in steps (3) and (5) specifically includes the following steps: searching the NIST 11 standard mass spectrum library through a chemical workstation, performing analysis, and confirming the chromatographic peaks of the volatile components to be tested. This is a qualitative analysis. Figure 5 This is the total ion chromatogram of a solid standard sample. Figure 6 The image shows the total ion chromatogram of a wild chrysanthemum sample.
[0049] The conditions for multiple headspace extraction-gas chromatography-mass spectrometry are as follows: (1) Multiple headspace extraction conditions: headspace equilibrium temperature 100 o C, Circulation temperature 110 o C, Transmission line temperature 120 o C, headspace equilibration time 30 min, carrier gas is high-purity helium, sample pressure 15 psi, injection time 0.5 min.
[0050] (2) Gas chromatography conditions: High-purity helium was used as the carrier gas at a flow rate of 1.0 mL / min. Splitless injection was used. An HP-5 MS quartz capillary column was employed. Temperature programmed analysis was used. The temperature programmed process was as follows: initial temperature 60 °C. o C, hold for 1 minute, at 12 o Temperature increased to 160 °C / min. o C, hold for 1 minute, then at 12 o Temperature increased to 280°C / min o Keep at C for 2 minutes.
[0051] (3) Mass spectrometry conditions: Ion source: EI, electron energy: 70 eV, electron multiplier voltage: 930 V, ion source temperature: 230 °C o C, Quadrupole temperature: 150 o C, Scanning mode: Full scan; Quality scan range m / z: 35~500.
[0052] The above description of the embodiments is provided to enable those skilled in the art to understand and use the invention. It will be apparent to those skilled in the art that various modifications can be made to these embodiments, and the general principles described herein can be applied to other embodiments without inventive effort. Therefore, the present invention is not limited to the above embodiments, and any improvements and modifications made by those skilled in the art based on the disclosure of the present invention without departing from the scope of the invention should be within the protection scope of the present invention.
Claims
1. A method for quantitative determination of volatile components in food and / or medicinal materials, characterized in that, The quantitative determination method includes the following steps: The volatile component standard sample was sealed in a headspace vial, and the total peak area corresponding to the volatile component in the volatile component standard sample was measured and calculated by multiple headspace extraction-gas chromatography-mass spectrometry. The food and / or medicinal powder to be tested is sealed in a headspace vial. The total peak area corresponding to the volatile components in the food and / or medicinal powder is measured and calculated by multiple headspace extraction-gas chromatography-mass spectrometry. The absolute content of the volatile components in the food and / or medicinal powder is obtained by comparing and calculating with the standard sample of volatile components.
2. The method for quantitative determination of volatile components in food and / or medicinal materials according to claim 1, characterized in that, The preparation process of the volatile component standard sample includes the following steps: Weigh out the solid sample containing volatile components and anhydrous magnesium sulfate, grind them, and obtain a mixture; Weigh out a portion of the mixture, discard the rest, add anhydrous magnesium sulfate, and grind.
3. The method for quantitative determination of volatile components in food and / or medicinal materials according to claim 1, characterized in that, The calculation of the total peak area corresponding to the volatile components in the standard sample or the total peak area corresponding to the volatile components in the food and / or medicinal powder to be tested includes the following process: Further calculations of the first-order mechanism of multiple headspace extraction yield the following results: ,in A i For the first i Peak area during the second extraction, index q This is an indicator to describe the exponential decrease in peak area during multiple headspace extraction processes. i The peak areas obtained from the continuous extraction of volatile components from standard samples or food and / or medicinal powders are processed and linearly regressed according to the above formula to obtain the extraction number. as well as Substitution The total peak area corresponding to the volatile components in the standard sample or the total peak area corresponding to the volatile components in the food and / or medicinal powder to be tested can be calculated.
4. The method for quantitative determination of volatile components in food and / or medicinal materials according to claim 1, characterized in that, In the quantitative determination method, standard samples of volatile components of different masses are sealed in headspace vials, and the total peak area corresponding to the volatile components in the standard samples of different masses is measured and calculated by multiple headspace extraction-gas chromatography-mass spectrometry. The total peak area corresponding to the volatile component standard sample was plotted against the sample mass. The data was linearly fitted using the least squares method to obtain standard curves for all volatile component standard samples of different masses, in order to verify the feasibility.
5. The method for quantitative determination of volatile components in food and / or medicinal materials according to claim 1, characterized in that, The conditions for multiple headspace extraction in the multiple headspace extraction-gas chromatography-mass spectrometry method include: Headspace equilibrium temperature 80-110 o C, Circulation temperature 90-120 o C, Transmission line temperature 100-130 o C, headspace equilibration time 10-40 min, carrier gas is high-purity helium, sample pressure 10-20 psi, injection time 0.5-2 min.
6. The method for quantitative determination of volatile components in food and / or medicinal materials according to claim 1, characterized in that, The gas chromatography conditions in the multiple headspace extraction-gas chromatography-mass spectrometry (GC-MS) method include: The carrier gas was high-purity helium, with a flow rate of 0.5-1.2 mL / min. The sample was injected in a split or splitless manner using an HP-5 MS quartz capillary column, and the analysis was performed using temperature programmed temperature control.
7. The method for quantitative determination of volatile components in food and / or medicinal materials according to claim 6, characterized in that, The temperature rise process is as follows: initial temperature 50-60°C. o C, keep for 1-2 minutes, at 10-12 o Heat to 150-160°C / min. o C, maintain for 1-2 minutes, then increase by 10-12 o Temperature increased to 210-280 °C / min o Keep at C for 1-2 minutes.
8. The method for quantitative determination of volatile components in food and / or medicinal materials according to claim 1, characterized in that, The mass spectrometry conditions in the multiple headspace extraction-gas chromatography-mass spectrometry (GC-MS) method include: Ion source: EI, electron energy: 65-75 eV, electron multiplier voltage: 910 V-930 V, ion source temperature: 210-240 °C o C, Quadrupole temperature: 145-160°C o C, Scanning mode: Full scan; Quality scan range m / z: 35~500.
9. The method for quantitative determination of volatile components in food and / or medicinal materials according to claim 1, characterized in that, The process of measuring and calculating the total peak area corresponding to volatile components in a standard sample of volatile components includes the following steps: The total ion current chromatogram of the volatile component standard sample was measured. The total ion current chromatogram of the volatile component standard sample was analyzed by the standard mass spectrometry library to identify the chromatographic peak of the volatile component to be tested. The chromatographic peak of the volatile component to be tested was integrated to obtain the peak area of the volatile component to be tested. The total peak area corresponding to the volatile component in the volatile component standard sample was calculated. The process of measuring and calculating the total peak area corresponding to the volatile components in the volatile components of the food and / or medicinal powder to be tested includes the following steps: The total ion current chromatogram of the food and / or medicinal powder to be tested is obtained by measurement. The total ion current chromatogram of the food and / or medicinal powder to be tested is analyzed by using a standard mass spectrometry library to identify the chromatographic peaks of the volatile components to be tested. The chromatographic peaks of the volatile components to be tested are integrated to obtain the peak area of the volatile components to be tested. The total peak area corresponding to the volatile components in the food and / or medicinal powder to be tested is calculated.
10. The method for quantitative determination of volatile components in food and / or medicinal materials according to claim 1, characterized in that, The food and / or medicinal material is wild chrysanthemum; The volatile components include one or more of borneol and camphor.