A method for non-destructive collection and analysis of bergamot aroma volatiles

Abstract

The present application aims at the drawbacks of low collection efficiency of plant volatile substances, which is not conducive to the analysis of plant volatile substances, and the difficulty in collecting volatile substances at different temperature environments, and provides a bergamot aroma volatile substance nondestructive collection and analysis method, which collects the aroma volatile substances generated by bergamot through a bergamot aroma volatile substance nondestructive collection device. The bergamot aroma volatile substance nondestructive collection device comprises an air pump, a filter, a gas flow meter, a container, a spoiler and a water bath temperature adjusting module, can realize the improvement of collection efficiency, realize nondestructive collection, and can adjust the collection temperature according to the collection requirements.

Description

Technical Field

[0001] This invention belongs to the field of plant volatile matter collection and analysis technology, specifically relating to a non-destructive method for collecting and analyzing volatile matter from the aroma of bergamot. Background Technology

[0002] Buddha's Hand fruit, a plant belonging to the genus Citrus in the family Rutaceae. This type of plant is mainly distributed in Zhaoqing, Yunfu, Jinhua, and other cities. It has fruit lobes split like a fist or open like fingers, with a pale yellowish-brown or light brownish-red surface and a rough skin. The peel and leaves contain aromatic oils, giving it a strong, fresh fruit fragrance.

[0003] Understanding the composition and content of volatile substances in bergamot is helpful for exploring and developing additional applications of bergamot and reusing processing by-products, thereby increasing its economic value. Currently, although various collection methods have been developed for plant volatiles, such as distillation, microwave drying, vacuum extraction, extraction, and cold maceration with fat, most of these methods will cause some damage to the aromatic volatiles of bergamot during the collection process, affecting the accuracy of subsequent analysis results. Extraction can achieve non-destructive collection. For example, Chinese patent CN211374645U discloses a flower fragrance compound collection device, including a collection hood, a solid-phase extraction tube, and a vacuum pump. The collection hood has an air inlet on one side and an air outlet on the other side. An activated carbon filter membrane is installed on the air inlet. One end of the solid-phase extraction tube is connected to the air outlet, and the other end is connected to the vacuum pump. A circular glass gasket is installed at the bottom of the collection hood, and the circular glass gasket is connected to the collection hood through a silicone gasket. The current device collects floral fragrance using a vacuum pump, allowing gas to pass through a collection hood. However, due to the limited position of the inlet and outlet ports on the hood, only a small portion of the gas comes into contact with the flowers for fragrance collection, resulting in a low concentration of collected fragrance. To collect sufficient fragrance for analysis, the collection time needs to be extended. Furthermore, the volatile compounds in bergamot differ at different temperatures. Collecting and analyzing bergamot volatile compounds at a fixed temperature is insufficient for analytical requirements. Therefore, it is necessary to collect and analyze bergamot volatile compounds under different temperature conditions. The aforementioned floral fragrance compound collection device is also difficult to adjust for temperature requirements. To improve the collection efficiency of bergamot volatile compounds, thereby facilitating subsequent analysis and enabling analysis under different temperature conditions, we propose a non-destructive collection and analysis method for bergamot fragrance volatile compounds. Summary of the Invention

[0004] This invention addresses the shortcomings of existing technologies, such as low collection efficiency of plant volatiles which hinders analysis and difficulty in collecting volatiles under different temperature conditions, by providing a non-destructive method for collecting and analyzing volatiles from the aroma of bergamot.

[0005] The objective of this invention is achieved through the following technical solution: a method for non-destructive collection and analysis of volatile aromatic compounds from Buddha's Hand citron, comprising a non-destructive collection device for Buddha's Hand citron aroma volatiles, wherein the non-destructive collection device comprises: An air pump is used to supply air. A filter, connected to the air pump, is used to filter the air output from the first air pump. A gas flow meter, connected to the output of the filter, is used to calculate the flow rate of the gas passing through it. A container for holding Buddha's Hand citron, the container is equipped with an air inlet and an air outlet, the air inlet is connected to the air outlet of a gas flow meter; The baffle, located inside the container, is used to agitate the airflow within the container, allowing the air to make more thorough contact with the Buddha's Hand fruit. The water bath temperature control module is used to adjust the temperature of the container, the air entering the container, and the Buddha's Hand fruit inside the container; The aroma adsorption column is set at the air outlet of the container to adsorb the volatile aroma compounds produced by Buddha's Hand. The collection and analysis method further includes the following steps: Step 1: Collect the volatile components of Buddha's Hand aroma for 1-3 hours using a non-destructive collection device. Step 2: Remove the aroma adsorption column, use the eluent to elute the aroma volatiles on the aroma adsorption column to form a fruit aroma volatile solution, put it into a chromatography bottle with an inner liner, and tighten the cap. Step 3: Using gas chromatography-tandem mass spectrometry (GC-MS) in automatic injection mode, the fruit aroma volatile solution was aspirated and injected into the GC-MS injection port. The aroma volatile mixture was separated using a weakly polar chromatographic column (HP-5MS / DB-5MS), and the aroma volatiles were qualitatively and quantitatively analyzed by mass spectrometry.

[0006] Preferably, the container includes a tank body and a tank lid, which are sealed together. A plurality of fixing rods are fixedly provided on the tank lid, and the fixing rods extend into the tank body. The baffle is provided on the fixing rods.

[0007] Preferably, all the fixing rods are arranged in a circular array around the center line of the can lid, and the fixing rods are provided with multiple longitudinally distributed slots, and the baffle can be engaged in any of the slots.

[0008] Preferably, the water bath temperature regulation module includes a panel filled with heat-conducting liquid and a temperature regulation module for regulating the temperature of the heat-conducting liquid inside the panel. The upper surface of the panel is provided with grooves and several pipe grooves. The air pump and the filter are connected through a first pipe, the filter and the gas flow meter are connected through a second pipe, and the gas flow meter and the air inlet of the container are connected through a third pipe. The first pipe, the second pipe, and the third pipe are respectively embedded in different pipe grooves. The lower end of the container is embedded in the groove, and the gas flow meter is installed on the panel.

[0009] Preferably, the temperature control module includes two sets of thermoelectric coolers. The cooling surface of one set of thermoelectric coolers is attached to the panel, and a cooling fan is installed on one side of the heating surface of the set of thermoelectric coolers. The heating surface of the other set of thermoelectric coolers is attached to the panel, and a temperature controller is electrically connected to each set of thermoelectric coolers.

[0010] Preferably, the panel is equipped with a temperature sensor for detecting the temperature of the heat transfer fluid, and the panel is equipped with a display board that is electrically connected to the temperature sensor and is used to display the real-time temperature of the heat transfer fluid.

[0011] Preferably, the can is a glass jar with its opening facing downwards, and the lid is located below the jar, with a rubber sealing ring between the lid and the edge of the jar's opening. The can lid is embedded in the groove.

[0012] Preferably, the can lid is provided with a raised platform, and both the air inlet and the air outlet are located on the can body, with the upper end of the raised platform positioned between the heights of the air inlet and the air outlet. Both the can lid and the riser are made of thermally conductive material. .

[0013] As a preferred option The thermally conductive material is a metallic material or a polymer thermally conductive material.

[0014] Preferably, the filter is an activated carbon filter, and the aroma adsorption column is a glass tube filled with SuperQ adsorbent.

[0015] Preferably, the eluent in step two is a dichloromethane solution containing 1 / 60000 (v / v) n-octanol, and the amount used is 200 µL; the amount of fruit aroma volatile solution taken in step three is 2 µL.

[0016] As a preferred option, in step three, the chromatographic conditions are: injection port temperature 250 ℃; Column oven heating program: Hold at 40℃ for 3 minutes, then increase to 250℃ at 5℃ / minute, hold for 3 minutes, and then stop. Mass spectrometry conditions: EI = 70 eV, mass collection range 40-400 m / z; Identification of aroma volatiles: Qualitative analysis was performed by comparing the RI value with that of n-alkanes and by comparing with standards. Quantitative analysis of compounds was performed by a semi-quantitative method comparing the peak area with the internal standard.

[0017] Compared with the prior art, the present invention has the following beneficial effects: This invention employs a non-destructive collection device for the aromatic volatiles produced by Buddha's Hand citron, enabling non-destructive collection. The baffle plate in the non-destructive collection device for volatile compounds of Buddha's Hand aroma can agitate the airflow in the container, allowing the air to come into more full contact with the Buddha's Hand, thereby increasing the concentration of collected volatile compounds and improving collection efficiency. 3. The water bath temperature control module can be used to adjust the temperature of the container, the air entering the container, and the Buddha's Hand fruit inside the container, and can extract the volatiles produced by the Buddha's Hand fruit under different ambient temperatures as needed.

[0018] 4. The data obtained by this invention, after analysis, closely approximates the sensory results under different environments, avoiding human interference from sensory evaluation, and can be used for the evaluation of the aroma quality of Buddha's Hand fruit. Attached Figure Description

[0019] Figure 1 A schematic diagram of a device for the non-destructive collection of volatile compounds from the aroma of Buddha's Hand citron. Figure 2 A schematic diagram of the structure of the non-destructive collection device for bergamot aroma volatiles after removing the air pump, filter, and can lid; Figure 3 This is a schematic diagram of the bottom structure of the panel; The diagram is labeled as follows: 1. Air pump, 2. Filter, 3. Gas flow meter, 4. Container, 5. Air inlet, 6. Air outlet, 7. Tank body, 8. Tank lid, 9. Fixing rod, 10. Slot, 11. Elevating platform, 12. Baffle plate, 13. Water bath temperature control module, 14. Panel, 16. Display panel, 17. Semiconductor cooling chip, 18. Cooling fan, 19. Temperature controller, 20. Groove, 21. Pipe groove, 22. First pipe, 23. Second pipe, 24. Third pipe, 25. Aroma adsorption column. Detailed Implementation

[0020] The present invention will be further described below with reference to the embodiments illustrated in the accompanying drawings: like Figure 1 , Figure 2 , Figure 3 As shown, a method for non-destructive collection and analysis of volatile aroma compounds from Buddha's Hand citron is disclosed. This method involves collecting the volatile aroma compounds produced by Buddha's Hand citron using a non-destructive collection device, which includes: Air pump 1, used to supply air. Filter 2, connected to air pump 1, is used to filter the air output by the first air pump 1. Filter 2 is an activated carbon filter 2.

[0021] Gas flow meter 3 is connected to the output of filter 2 to calculate the flow rate of the gas passing through it. Container 4 is used to hold Buddha's Hand citron. Container 4 has an air inlet 5 and an air outlet 6. The air inlet 5 is connected to the outlet end of the gas flow meter 3. Container 4 includes a can body 7 and a can lid 8, which are sealed together. The can lid 8 is fixed with multiple fixing rods 9, which extend into the can body 7. The fixing rods 9 are arranged in a circular array around the center line of the can lid 8, and the fixing rods 9 have multiple longitudinally distributed slots 10. The can body 7 is a glass jar. The opening of the can body 7... The can is positioned with its opening facing downwards. The can lid 8 is located below the can body 7, and a rubber sealing ring is provided between the opening edge of the can lid 8 and the can body 7. The can lid 8 is provided with a lifting platform 11. The air inlet 5 and the air outlet 6 are both located on the can body 7. The height of the upper end of the lifting platform 11 is between the heights of the air inlet 5 and the air outlet 6. Both the can lid 8 and the lifting platform 11 are made of thermally conductive materials, such as metal materials like copper, aluminum, or copper-aluminum composite materials, or polymer thermally conductive materials like thermally conductive plastics.

[0022] The spoiler 12 is installed inside the container 4 to agitate the airflow inside the container 4 so that the air can come into more full contact with the Buddha's Hand. The spoiler 12 can be snapped into any slot 10 on the fixing rod 9.

[0023] The water bath temperature regulation module 13 is used to adjust the temperature of the container 4, the air entering the container 4, and the Buddha's Hand mushroom inside the container 4. The water bath temperature regulation module 13 includes a panel 14 filled with heat-conducting liquid and a temperature control module for regulating the temperature of the heat-conducting liquid inside the panel 14. To facilitate the user's understanding of the temperature of the heat-conducting liquid inside the panel 14, a temperature sensor for detecting the temperature of the heat-conducting liquid is installed inside the panel 14. The panel 14 is equipped with a display board 16 electrically connected to the temperature sensor and used to display the real-time temperature of the heat-conducting liquid. The heat-conducting liquid is water. The temperature control module includes two sets of semiconductor cooling chips 17. The cooling surface of one set of semiconductor cooling chips 17 is attached to the panel 14, and this set of semiconductor cooling chips 17 is the cooling group. A cooling fan 18 is installed on one side of the heating surface of this set of semiconductor cooling chips 17. The heating surface of the other set of semiconductor cooling chips 17 is attached to the panel 14, and this set of semiconductor cooling chips 17 is the heating group. Each set of semiconductor cooling chips 17 is electrically connected to a temperature controller 19. The upper surface of panel 14 is provided with grooves 20 and multiple pipe slots 21. The air pump 1 is connected to the filter 2 through a first pipe 22, the filter 2 is connected to the gas flow meter 3 through a second pipe 23, and the gas flow meter 3 is connected to the air inlet 5 of container 4 through a third pipe 24. The first pipe 22, the second pipe 23, and the third pipe 24 are respectively embedded in different pipe slots 21. The lower end of container 4 is embedded in the groove 20, that is, the can lid 8 is embedded in the groove 20, and the gas flow meter 3 is mounted on panel 14. Compared with the commonly used electric heating wire and compressor refrigeration structure, the structure using semiconductor cooling chip 17 for refrigeration / heating has a smaller overall size, and the temperature can be more stable by setting the panel 14, which is filled with heat-conducting liquid for temperature regulation.

[0024] The aroma adsorption column 25 is set at the air outlet 6 of the container 4 to adsorb the aroma volatiles produced by Buddha's Hand. The aroma adsorption column 25 is a glass tube filled with SuperQ adsorbent.

[0025] The collection and analysis method further includes the following steps: Step 1: Collect bergamot aroma volatiles using a non-destructive collection device for 1-3 hours. Specifically, first place the bergamot on the raised platform 11 inside container 4, with the bergamot positioned between the height of the air inlet 5 and the air outlet 6. Then, adjust the temperature of the water bath temperature control module 13 according to the analysis requirements. When the required analysis temperature is higher than the room temperature, set the required analysis temperature through the temperature controller 19 connected to the semiconductor cooling chip 17 of the heating unit, and the heating unit will heat the heat-conducting liquid in the panel 14. When the required analysis temperature is lower than the room temperature, set the required analysis temperature through the temperature controller 19 connected to the semiconductor cooling chip 17 of the cooling unit, and the heating unit will heat the heat-conducting liquid in the panel 14. The heating element cools the heat transfer fluid in panel 14. The temperature of the heat transfer fluid in panel 14 is observed through the display panel 16. When the set temperature is reached, the air pump 1 is turned on. The air supplied by the air pump 1 passes through the first pipe 22. The panel 14 adjusts the temperature of the air passing through the first pipe 22. The air then passes through the filter 2 to obtain clean air. The clean air enters the second pipe 23 and is adjusted at a second temperature by the panel 14. After passing through the gas flow meter 3, it enters the container 4 through the third pipe 24. The gas flow meter 3 and the third pipe 24 are both installed on the panel 14. At this time, it is in a heat preservation state to maintain the temperature of the clean air inside. After clean air enters container 4, it is stirred by baffle 12 to make the airflow more fully contact with the Buddha's Hand. The air mixed with the volatiles of Buddha's Hand passes through aroma adsorption column 25 and is adsorbed by SuperQ adsorbent inside the glass tube. Because the lower end of container 4 is embedded in groove 20, the temperature of container 4 is also regulated by panel 14. The lid 8 and the lifting platform 11 of container 4 are both made of heat-conducting material. When Buddha's Hand is placed on the lifting platform 11, its temperature is also regulated by the temperature of the heat-conducting liquid in panel 14.

[0026] Step 2: Remove the aroma adsorption column 25 and elute the aroma volatiles on the aroma adsorption column 25 with 200 µL of dichloromethane solution containing 1 / 60000 (v / v) n-octanol to form a floral aroma volatile solution. Place the solution into a chromatographic vial with an inner liner and tighten the cap. Step 3: Gas chromatography-mass spectrometry analysis. Using GC-MS autosampler mode, 2 µL of floral volatile solution was injected into the GC-MS injector. The mixture of aromatic volatiles was separated using a weakly polar chromatographic column at an injection port temperature of 250℃. Column oven heating program: Hold at 40℃ for 3 minutes, then increase to 250℃ at 5℃ / minute, hold for 3 minutes, and then stop. The aroma volatiles were qualitatively and quantitatively analyzed by mass spectrometry under the following conditions: EI = 70 eV and mass collection range 40-400 m / z. Identification of aroma volatiles: Qualitative analysis was performed by comparing the RI value with that of n-alkanes and by comparing with standards. Quantitative analysis of compounds was performed by a semi-quantitative method comparing the peak area with the internal standard.

[0027] Table 1 below shows the volatile component detection data of Jinhua Buddha's Hand 'Qingyi Tongzi' at three different temperatures of 15℃, 25℃, and 35℃. The temperature was adjusted using the water bath temperature adjustment module 13 in the Buddha's Hand aroma volatile matter non-destructive collection device.

[0028] Table 1. Detection of volatile components in bergamot at different temperatures At 15℃, 39 flavor compounds were detected in Jinhua Buddha's Hand 'Qingyi Tongzi' citrus fruit; at 25℃, 44 flavor compounds were detected; and at 35℃, 47 flavor compounds were detected. At lower temperatures, the content of terpenes decreased significantly, while the relative content of alcohols and aldehydes increased, making the floral and fruity aroma more pronounced. At 35℃, the volatilization of terpenes increased dramatically, and aldehydes also increased, resulting in a more pronounced diffusion of the Buddha's Hand aroma.

[0029] The present invention uses a water bath temperature regulation module 13 in a non-destructive collection device for bergamot aroma volatiles to regulate the temperature of container 4, the air entering container 4, and the bergamot inside container 4. The temperature can be adjusted according to the collection and analysis requirements, thereby more accurately analyzing the volatile components of bergamot.

[0030] It should be understood that in the claims and description of this invention, all instances of "comprising..." should be understood as having an open meaning, that is, their meaning is equivalent to "containing at least...", and should not be understood as having a closed meaning, that is, their meaning should not be understood as "containing only...".

[0031] The specific embodiments described herein are merely illustrative of the spirit of the invention. Those skilled in the art to which this invention pertains may make various modifications or additions to the described specific embodiments or use similar methods to replace them, without departing from the spirit of the invention or exceeding the scope defined by the appended claims.

Claims

1. A method for non-destructive collection and analysis of volatile compounds from the aroma of bergamot, characterized in that, The aroma volatiles produced by Buddha's Hand are collected by a non-destructive collection device, wherein the non-destructive collection device comprises: An air pump is used to supply air. A filter, connected to the air pump, is used to filter the air output from the first air pump. A gas flow meter, connected to the output of the filter, is used to calculate the flow rate of the gas passing through it. A container for holding Buddha's Hand citron, the container is equipped with an air inlet and an air outlet, the air inlet is connected to the air outlet of a gas flow meter; The baffle, located inside the container, is used to agitate the airflow within the container, allowing the air to make more thorough contact with the Buddha's Hand fruit. The water bath temperature control module is used to adjust the temperature of the container, the air entering the container, and the Buddha's Hand fruit inside the container; The aroma adsorption column is set at the air outlet of the container to adsorb the volatile aroma compounds produced by Buddha's Hand. The collection and analysis method further includes the following steps: Step 1: Collect the volatile components of Buddha's Hand aroma for 1-3 hours using a non-destructive collection device. Step 2: Remove the aroma adsorption column and elute the aroma volatiles on the aroma adsorption column with 200 µL of dichloromethane solution containing 1 / 60000 (v / v) n-octanol to form a fruit aroma volatile solution. Place the solution into a chromatographic vial with an inner liner and tighten the cap. Step 3: Gas chromatography-mass spectrometry analysis. Using GC-MS autosampler mode, 2 µL of fruit aroma volatile solution was injected into the GC-MS injector. The aroma volatile mixture was separated using a weakly polar chromatographic column at an injection port temperature of 250℃. Column oven heating program: Hold at 40℃ for 3 minutes, then increase to 250℃ at 5℃ / minute, hold for 3 minutes, and then stop. The aroma volatiles were qualitatively and quantitatively analyzed by mass spectrometry under the following conditions: EI = 70 eV and mass collection range 40-400 m / z. Identification of aroma volatiles: Qualitative analysis was performed by comparing the RI value with that of n-alkanes and by comparing with standards. Quantitative analysis of compounds was performed by a semi-quantitative method comparing the peak area with that of internal standards.

2. The method for non-destructive collection and analysis of volatile compounds from the aroma of bergamot as described in claim 1, characterized in that, The container includes a tank body and a tank lid, which are sealed together. Several fixing rods are fixedly provided on the tank lid, and the fixing rods extend into the tank body. The baffle is provided on the fixing rods.

3. The method for non-destructive collection and analysis of volatile compounds from the aroma of bergamot as described in claim 2, characterized in that, All the aforementioned fixing rods are arranged in a circular array around the center line of the can lid, and the fixing rods are provided with multiple longitudinally distributed slots, and the baffle can be engaged in any of the slots.

4. A method for non-destructive collection and analysis of volatile compounds from the aroma of bergamot as described in claim 2 or 3, characterized in that, The water bath temperature regulation module includes a panel filled with heat-conducting liquid and a temperature control module for regulating the temperature of the heat-conducting liquid inside the panel. The upper surface of the panel is provided with grooves and several pipe grooves. The air pump and the filter are connected through a first pipe, the filter and the gas flow meter are connected through a second pipe, and the gas flow meter and the air inlet of the container are connected through a third pipe. The first pipe, the second pipe, and the third pipe are respectively embedded in different pipe grooves. The lower end of the container is embedded in the groove, and the gas flow meter is mounted on the panel.

5. The method for non-destructive collection and analysis of volatile compounds from the aroma of bergamot according to claim 4, characterized in that, The temperature control module includes two sets of thermoelectric coolers. The cooling surface of one set of thermoelectric coolers is attached to the panel, and a cooling fan is installed on one side of the heating surface of the thermoelectric cooler. The heating surface of the other set of thermoelectric coolers is attached to the panel, and a temperature controller is electrically connected to each set of thermoelectric coolers.

6. The method for non-destructive collection and analysis of volatile compounds from the aroma of bergamot according to claim 5, characterized in that, The panel is equipped with a temperature sensor for detecting the temperature of the heat transfer fluid, and a display panel that is electrically connected to the temperature sensor and is used to display the real-time temperature of the heat transfer fluid is provided on the panel.

7. The method for non-destructive collection and analysis of volatile compounds from the aroma of bergamot according to claim 6, characterized in that, The can is a glass jar with its opening facing downwards. The lid is located below the jar and a rubber sealing ring is provided between the lid and the edge of the opening of the jar. The lid is embedded in the groove.

8. The method for non-destructive collection and analysis of volatile compounds from the aroma of bergamot according to claim 7, characterized in that, The can lid is equipped with a raised platform. The air inlet and air outlet are both located on the can body. The upper part of the raised platform is located between the heights of the air inlet and the air outlet. Both the can lid and the raised platform are made of thermally conductive material.

9. The method for non-destructive collection and analysis of volatile compounds from the aroma of bergamot according to claim 7, characterized in that, The thermally conductive material is a metallic material or a polymer thermally conductive material.

10. The method for non-destructive collection and analysis of volatile compounds from the aroma of bergamot according to claim 1, characterized in that, The filter is an activated carbon filter, and the aroma adsorption column is a glass tube filled with SuperQ adsorbent.

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