CN218298148U - Detection device and detection system for content of organic acid and solvent in tobacco essence - Google Patents
Detection device and detection system for content of organic acid and solvent in tobacco essence Download PDFInfo
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- CN218298148U CN218298148U CN202221945622.8U CN202221945622U CN218298148U CN 218298148 U CN218298148 U CN 218298148U CN 202221945622 U CN202221945622 U CN 202221945622U CN 218298148 U CN218298148 U CN 218298148U
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Abstract
The application relates to a detection device and a detection system for organic acid and solvent content in tobacco essence. The detection device includes: the system comprises a gas chromatography sample introduction unit, a gas chromatography separation and diversion unit, a mass spectrometry detection unit and a thermal conductivity detection unit; the gas chromatography separation split-flow unit comprises: capillary gas chromatography columns and column splitters; the inlet of the capillary gas chromatographic column is connected with a gas chromatographic sample introduction unit; the chromatographic column splitter comprises: the liquid inlet pipe is communicated with a first liquid outlet pipe and a second liquid outlet pipe; the outlet of the capillary gas chromatographic column is connected with the liquid inlet pipe of the chromatographic column splitter; the tail end of a first liquid outlet pipe of the chromatographic column splitter is connected with a sample inlet of the mass spectrum detection unit; the tail end of a second liquid outlet pipe of the chromatographic column splitter is connected with a sample inlet of the thermal conductivity detection unit. Adopt this detection device can detect the organic acid and the solvent of essence for cigarette simultaneously, easy operation, detection efficiency is high to the testing result is accurate.
Description
Technical Field
The application relates to the technical field of analysis of tobacco essence components, in particular to a detection device and a detection system for organic acid and solvent content in tobacco essence.
Background
The tobacco essence is an important tobacco additive, and the flavoring of cigarettes by using the tobacco essence is one of important means for improving the smoking quality of cigarettes in cigarette enterprises. The tobacco essence has complex components, and mainly comprises alcohols, esters, acids and other substances. Among them, organic acids and solvents are important components. The organic acid is one of main chemical components influencing the smoking quality of the tobacco, has the effects of balancing the pH value of smoke, relieving the irritation of the smoke and increasing the smoke concentration in the combustion process of the cigarette, and has an important influence on the smoking quality of the cigarette. Therefore, the method for accurately measuring the types and the content of the organic acid in the tobacco essence has important significance for understanding the internal quality of various essence raw materials and designing essence formulas. The solvent in the tobacco essence is the highest-content component, and the common tobacco essence solvent mainly comprises water, ethanol, 1, 2-propylene glycol, glycerol and the like. The stability of the solvent content is crucial to the quality of the essence and flavor, and is an important index for judging whether the essence and flavor for cigarettes are qualified or not. At present, in the prior art, under the condition that the content of both organic acid and solvent is required to be detected, different methods are required to be adopted for respective detection, the operation is complex, the time consumption is long, and the accuracy of the detection result is required to be improved.
SUMMERY OF THE UTILITY MODEL
In order to solve or partially solve the problems existing in the related art, the application provides a detection device and a detection system for the content of organic acid and solvent in tobacco essence.
The application provides a detection device that is arranged in essence for cigarette organic acid and solvent content, it includes: the system comprises a gas chromatography sample introduction unit, a gas chromatography separation and shunt unit, a mass spectrometry detection unit and a thermal conductivity detection unit; wherein the content of the first and second substances,
the gas chromatography separation split-flow unit comprises: capillary gas chromatography columns and column splitters;
the inlet of the capillary gas chromatographic column is connected with a gas chromatographic sample introduction unit;
the chromatography column splitter comprises: the liquid inlet pipe is communicated with a first liquid outlet pipe and a second liquid outlet pipe; the outlet of the capillary gas chromatographic column is connected with a liquid inlet pipe of the chromatographic column splitter; the tail end of a first liquid outlet pipe of the chromatographic column splitter is connected with a sample inlet of the mass spectrum detection unit; and the tail end of a second liquid outlet pipe of the chromatographic column splitter is connected with a sample inlet of the thermal conductivity detection unit.
Further, the capillary gas chromatography column has dimensions of: the length is 60m, the diameter is 0.25mm, and the thickness of the coating is 0.25 mu m; the capillary gas chromatographic column is an inertly treated polyethylene glycol polymer chromatographic column.
Further, the flow split ratio of the chromatographic column splitter is 1.
Further, the chromatographic column splitter is a Y-shaped quartz splitter.
Furthermore, damping columns are arranged in the first liquid outlet pipe and the second liquid outlet pipe.
Further, the inner diameter of the damping column is 0.22mm.
Further, the gas chromatography sample injection unit comprises: a sample introduction box and a gasification chamber; the sample introduction box comprises a liquid inlet; the gasification chamber is connected with the liquid inlet and is used for gasifying the liquid to be tested flowing in from the liquid inlet; the outlet of the gasification chamber is connected with the inlet of the capillary gas chromatographic column;
the gas chromatography separation and distribution unit further comprises a gas chromatography column box, and the capillary gas chromatography column and the chromatography column splitter are arranged in the gas chromatography column box.
The application still provides a detecting system that is arranged in tobacco essence organic acid and solvent content, and it includes: an extraction device, a filtration device and the detection device of any one of the above; wherein the content of the first and second substances,
the extraction device comprises an extraction bottle for placing tobacco essence and an extracting agent;
the filtering device is provided with an organic phase filtering membrane and is used for filtering the feed liquid treated by the extraction device to obtain liquid to be detected;
and the liquid to be detected enters the detection device through the gas chromatography sample introduction unit of the detection device.
Further, the extraction device also comprises a shaking table, and the extraction bottle is arranged on the shaking table.
Further, the filtration pore size of the organic phase filtration membrane was 0.22 μm.
The application provides a detection device for organic acid and solvent content in essence for cigarette can include following beneficial effect:
the detection device adopts gas chromatography for sample introduction and separation, and has good separation effect on a detected object; after the separation, the separating liquid is also divided by arranging the chromatographic column splitter, and the separating liquid is divided into two parts, so that the same separating liquid is simultaneously detected by two methods, the operation is simplified, and the detection efficiency is improved. The mass spectrum detection is adopted for the organic acid, the detection sensitivity is high, and the detection of the organic acid cannot be influenced by the existence of the solvent; and the solvent is detected by thermal conductivity, and the organic acid and the solvent are effectively separated when the liquid to be detected passes through the chromatographic column, so that the detection of the solvent cannot be influenced by the presence of the organic acid.
To sum up, the detection device of organic acid and solvent content has synthesized gas chromatography's a kind separation function in the essence for cigarette that this application provided, and mass spectrometry detects function and thermal conductivity detection function, combines above-mentioned function together through the chromatographic column shunt, adopts this detection device to detect simultaneously the organic acid and the solvent of essence for cigarette simultaneously, easy operation, detection efficiency is high to the testing result is accurate. The detection device is suitable for the condition that the content of organic acid and solvent has detection requirements, and provides technical reference for solving the internal quality of various essences and designing essence formulas.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the application.
Drawings
The foregoing and other objects, features and advantages of the application will be apparent from the following more particular descriptions of exemplary embodiments of the application as illustrated in the accompanying drawings wherein like reference numbers generally represent like parts throughout the exemplary embodiments of the application.
FIG. 1 is a block diagram of a device for detecting the content of organic acids and solvents in tobacco flavor provided in an embodiment of the present application;
fig. 2 is a schematic structural diagram of a gas chromatography separation and diversion unit in the detection apparatus for detecting the content of organic acid and solvent in tobacco flavor provided by the embodiment of the application.
Description of the reference numerals
1-gas chromatography sample introduction unit
2-gas chromatography separation shunting unit
21-capillary gas chromatographic column
22-chromatographic column splitter
221-liquid inlet pipe
222-first liquid outlet pipe
223-second liquid outlet pipe
224 damping column
23-gas chromatographic column box
3-Mass Spectrometry detection Unit
4-thermal conductivity detection unit
Detailed Description
Embodiments of the present application will be described in more detail below with reference to the accompanying drawings. While embodiments of the present application are illustrated in the accompanying drawings, it should be understood that the present application may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in this application and the appended claims, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any and all possible combinations of one or more of the associated listed items.
It should be understood that although the terms "first," "second," "third," etc. may be used herein to describe various information, these information should not be limited to these terms. These terms are only used to distinguish one type of information from another. For example, first information may also be referred to as second information, and similarly, second information may also be referred to as first information, without departing from the scope of the present application. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, "a plurality" means two or more unless specifically limited otherwise.
The embodiment of the application provides a detection device of organic acid and solvent content in essence for cigarette, adopts this detection device to detect when can carrying out organic acid and solvent in the essence for cigarette simultaneously, all has the condition of measuring the demand to organic acid and solvent content, adopts the device to do benefit to the simplified operation, improves detection efficiency. The technical solutions of the embodiments of the present application are described in detail below with reference to the accompanying drawings.
Referring to fig. 1 and fig. 2, an embodiment of the present application provides a device for detecting organic acid and solvent content in a tobacco flavor, which includes: the system comprises a gas chromatography sample introduction unit 1, a gas chromatography separation and diversion unit 2, a mass spectrometry detection unit 3 and a thermal conductivity detection unit 4; wherein, the first and the second end of the pipe are connected with each other,
the gas chromatography separation split-flow unit 2 includes: a capillary gas chromatography column 21 and a column splitter 22;
the inlet of the capillary gas chromatographic column 21 is connected with the gas chromatographic sample injection unit 1;
referring to fig. 2, the column splitter 22 includes: a liquid inlet pipe 221, and a first liquid outlet pipe 222 and a second liquid outlet pipe 223 communicated with the liquid inlet pipe 221; the outlet of the capillary gas chromatographic column 21 is connected with the liquid inlet pipe 221 of the chromatographic column splitter 22; the tail end of the first liquid outlet pipe 222 of the chromatographic column splitter 22 is connected with a sample inlet of the mass spectrometry detection unit 3; the end of the second liquid outlet pipe 223 of the chromatographic column splitter 22 is connected with the sample inlet of the thermal conductivity detection unit 4.
The detection device provided by the embodiment comprises a gas chromatography sample introduction unit 1, a gas chromatography separation and shunt unit 2, a mass spectrometry detection unit 3 and a thermal conductivity detection unit 4. The gas chromatography sample introduction unit 1 is used for introducing liquid to be detected so as to instantly gasify the liquid to be detected, and the gasified sample is introduced into the capillary gas chromatography column 21 under the action of carrier gas. The specific structure of the gas chromatography sample injection unit 1 may be the same as that of the prior art, and specifically may include: a sample introduction box and a gasification chamber; the sample introduction box comprises a liquid inlet; the gasification chamber is connected with the liquid inlet and is used for gasifying the liquid to be tested flowing in from the liquid inlet; the outlet of the vaporizer is connected to the inlet of a capillary gas chromatography column 21.
The gas chromatography separation and diversion unit 2 is used for separating the liquid to be detected on one hand and also splitting the separated liquid on the other hand so as to perform mass spectrometry detection and thermal conductivity detection respectively and simultaneously. Gas chromatography is a good separation means to separate the components of a complex mixture. Specifically, the device comprises a capillary gas chromatography column 21 and a chromatography column splitter 22, wherein the capillary gas chromatography column 21 is used for realizing separation of different components, and the chromatography column splitter 22 is used for splitting a separation liquid.
At present, the gas chromatography is used for quantitative analysis of organic acids, and a common method is to firstly perform derivatization reaction on the organic acids and then use a capillary gas chromatography column for detection. Because strong polar compounds in the organic acid without derivatization have strong interaction with active sites on the chromatographic column, tailing or peak separation is poor, the difficulty of quantitative analysis at low concentration is increased, and the method is not suitable for the quantitative analysis of the organic acid. In addition, in this embodiment, since the solvent of the tobacco flavor needs to be measured, a large amount of highly polar compounds such as water exist in the separation liquid, which undoubtedly aggravates the above problem. Therefore, the capillary gas chromatographic column 21 preferably adopts an inertly treated polyethylene glycol polymer chromatographic column, which has a strong polarity, so as to facilitate the adsorption of organic acids, thereby ensuring a good separation effect on organic acids; on the other hand, the interaction between strong polar compounds such as organic acid, water and the like and the chromatographic column can be reduced through inert treatment, and the loss of the column is weakened. Therefore, the adoption of the polyethylene glycol polymer chromatographic column subjected to inert treatment can realize direct sample injection of the organic acid without derivatization treatment, thereby shortening the detection step and improving the detection accuracy. More preferably, a DB-FATWAX ultrahigh inert chromatographic column of Agilent company is adopted, the chromatographic column has good separation effect on all organic acids in the essence for cigarettes, and the peak shape is sharp and symmetrical and is the best. The dimensions of the capillary gas chromatography column 21 are preferably: 60m in length, 0.25mm in diameter and 0.25 μm in coating thickness.
The liquid to be detected passes through the capillary gas chromatographic column, the organic acid and the solvent are separated, and due to the difference in physical properties of the organic acid and the solvent, the method for simultaneously detecting the two compounds is not considered, but the method which is more suitable for the two compounds is respectively selected for simultaneous detection aiming at the two compounds. In order to implement simultaneous detection of the same separation liquid by two methods, in this embodiment, the separation liquid is split by the chromatographic column splitter 22, and is divided into two parts, the first detection liquid flows out from the first liquid outlet pipe 222, and the second detection liquid flows out from the second liquid outlet pipe 223, so that the two detection liquids can be respectively and simultaneously introduced into different analytical instruments for detection, thereby providing a precondition for subsequent MS/TCD detection. Further, in order to ensure that the first detection solution and the second detection solution flow out in equal amounts, the column splitter 22 has a split ratio of 1. Referring specifically to FIG. 2, the column splitter 22 is preferably a Y-shaped quartz splitter. Further, in order to balance the gas pressure of the carrier channel in the whole gas chromatography separation and distribution unit 2 and ensure that the gas flow rate in the channel is not changed, damping columns 224 are respectively arranged in the first liquid outlet pipe 222 and the second liquid outlet pipe 223. Further, the inner diameter of the damping cylinder 224 is preferably 0.22mm. In order to avoid the influence of foreign substances, the gas chromatography separation/division unit 2 preferably further includes a gas chromatography column casing 23, and the capillary gas chromatography column 21 and the column splitter 22 are provided in the gas chromatography column casing 23.
The detection device can simultaneously adopt different methods to simultaneously determine the contents of the organic acid and the solvent. Specifically, for the content determination of organic acid, a mass spectrum detection unit 3 is adopted, which comprises a mass spectrometer, the mass spectrum technology is that a vaporized molecular sample is converted into charged particles in a high-vacuum ion source, the charged particles enter a mass analyzer after ionization, extraction and focusing, mass-to-charge ratio separation is carried out according to time front and back or a space position under the action of a magnetic field or an electric field, the left and back particles are detected by a particle detector, MS fragments and corresponding strength obtained under certain conditions are just like a fingerprint image and are easy to identify, and the method has the advantage of high sensitivity, so that the mass spectrum method is adopted to detect the separation liquid flowing out from a first liquid outlet pipe 222 of a chromatographic column splitter 22 so as to determine the content of the organic acid in the detection liquid. For the content determination of the solvent, the invention adopts the thermal conductivity detection unit 4, the thermal conductivity detector of which has response to both inorganic matters and organic matters, does not damage the sample, and has simple structure, good stability, wide linear range and relatively low sensitivity, but has little influence on the detection result because the content of the solvent in the detection liquid is high. Therefore, the present invention uses thermal conductivity to measure the separated liquid flowing out from the second outlet 223 of the column splitter 22 to determine the solvent content in the measured liquid. In addition, the reason for adopting the above two methods is also that: because the mass spectrometer scanning mode is selective ion detection (SIM), which only detects selected ions, and other ions are not recorded, the presence of solvent does not affect the detection of organic acids by MS (mass spectrometry); because the organic acid and solvent have been effectively separated as they pass through the column, the presence of the organic acid does not affect the detection of the solvent by the TCD (thermal conductivity detector).
From the above, the detection device for the content of organic acid and solvent in the essence for tobacco provided by the embodiment of the application has the following advantages:
the detection device adopts gas chromatography for sample introduction and separation, and has good separation effect on a detected object; after the separation, the separating liquid is also divided by arranging the chromatographic column splitter, and the separating liquid is divided into two parts, so that the same separating liquid is simultaneously detected by two methods, the operation is simplified, and the detection efficiency is improved. The mass spectrum detection is adopted for the organic acid, the detection sensitivity is high, and the detection of the organic acid cannot be influenced by the existence of the solvent; the solvent is detected by thermal conductivity, and the organic acid and the solvent are effectively separated when the liquid to be detected passes through the chromatographic column, so that the detection of the solvent cannot be influenced by the presence of the organic acid. To sum up, the detection device of organic acid and solvent content has synthesized gas chromatography's a kind separation function in the essence for cigarette that this application provided, and mass spectrometry detects function and thermal conductivity detection function, combines above-mentioned function together through the chromatographic column shunt, adopts this detection device to detect simultaneously the organic acid and the solvent of essence for cigarette simultaneously, easy operation, detection efficiency is high to the testing result is accurate. The detection device is suitable for the condition that the content of organic acid and solvent has detection requirements, and provides technical reference for solving the internal quality of various essences and designing essence formulas.
Another embodiment of this application still provides a detecting system that is arranged in tobacco essence organic acid and solvent content, and it includes: an extraction device, a filtering device and the detection device; wherein the content of the first and second substances,
the extraction device comprises an extraction bottle for placing tobacco essence and an extracting agent;
the filtering device is provided with an organic phase filtering membrane and is used for filtering the feed liquid treated by the extraction device to obtain liquid to be detected;
and the liquid to be detected enters the detection device through the gas chromatography sample introduction unit of the detection device.
The extraction device and the filter device are used for preprocessing the tobacco essence to provide detection liquid suitable for on-machine detection, and the content of a detection object in the detection liquid is improved. Above-mentioned extraction device is used for realizing the extraction to the essence for cigarette, in order to improve the extraction effect, preferredly adopts the mode of shaking the extraction, and is specific, above-mentioned extraction device is still preferred including shaking the shaking table, the extraction bottle set up in shake on the shaking table.
The filtering device is used for filtering the extracted feed liquid to remove macromolecular impurities, and preferably, the filtering pore diameter of the organic phase filtering membrane is 0.22 mu m.
The working process of the detection system for the content of the organic acid and the solvent in the tobacco essence is as follows:
adding tobacco essence and an extracting agent into the extraction bottle, and then placing the extraction bottle into a shaking table for shaking;
after shaking, the feed liquid in the extraction bottle passes through an organic phase filtering membrane to obtain liquid to be detected;
and adding the liquid to be detected into the detection device through a liquid inlet of the gas chromatography sample injection unit, then carrying out analysis and detection, and determining the content of the organic acid and the solvent.
The detection system is provided with the detection device, and accordingly has the advantages of being simple in operation, high in detection efficiency and accurate in detection result.
Having described embodiments of the present application, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The terminology used herein was chosen in order to best explain the principles of the embodiments, the practical application, or improvements to the technology in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
Claims (10)
1. The utility model provides a detection apparatus for be arranged in essence for cigarette organic acid and solvent content which characterized in that includes: the system comprises a gas chromatography sample introduction unit, a gas chromatography separation and shunt unit, a mass spectrometry detection unit and a thermal conductivity detection unit; wherein, the first and the second end of the pipe are connected with each other,
the gas chromatography separation split-flow unit comprises: capillary gas chromatography columns and column splitters;
the inlet of the capillary gas chromatographic column is connected with a gas chromatographic sample introduction unit;
the chromatography column splitter comprises: the liquid outlet pipe comprises a liquid inlet pipe, a first liquid outlet pipe and a second liquid outlet pipe, wherein the first liquid outlet pipe and the second liquid outlet pipe are communicated with the liquid inlet pipe; the outlet of the capillary gas chromatographic column is connected with the liquid inlet pipe of the chromatographic column splitter; the tail end of a first liquid outlet pipe of the chromatographic column splitter is connected with a sample inlet of the mass spectrum detection unit; and the tail end of a second liquid outlet pipe of the chromatographic column splitter is connected with a sample inlet of the thermal conductivity detection unit.
2. The detection apparatus according to claim 1, wherein the capillary gas chromatography column has dimensions of: the length is 60m, the diameter is 0.25mm, and the thickness of the coating is 0.25 mu m; the capillary gas chromatographic column is an inertly treated polyethylene glycol polymer chromatographic column.
3. The test device of claim 1, wherein the chromatographic column diverter has a split ratio of 1.
4. The test device of claim 3, wherein the chromatography column splitter is a Y-quartz splitter.
5. The testing device of claim 4, wherein a damping post is disposed in each of the first and second outlet conduits.
6. The test device of claim 5, wherein the damping cylinder has an inner diameter of 0.22mm.
7. The detection apparatus according to claim 1, wherein the gas chromatography sample introduction unit comprises: a sample introduction box and a gasification chamber; the sample introduction box comprises a liquid inlet; the gasification chamber is connected with the liquid inlet and is used for gasifying the liquid to be tested flowing in from the liquid inlet; the outlet of the gasification chamber is connected with the inlet of the capillary gas chromatographic column;
the gas chromatography separation and distribution unit further comprises a gas chromatography column box, and the capillary gas chromatography column and the chromatography column splitter are arranged in the gas chromatography column box.
8. A detecting system for organic acid and solvent content in tobacco essence is characterized by comprising: an extraction device, a filtration device and a detection device according to any one of claims 1 to 7; wherein, the first and the second end of the pipe are connected with each other,
the extraction device comprises an extraction bottle for placing tobacco essence and an extracting agent;
the filtering device is provided with an organic phase filtering membrane and is used for filtering the feed liquid treated by the extraction device to obtain liquid to be detected;
and the liquid to be detected enters the detection device through the gas chromatography sample introduction unit of the detection device.
9. The detection system according to claim 8, wherein the extraction apparatus further comprises a shaker, and the extraction flask is disposed on the shaker.
10. The detection system according to claim 8, wherein the filtration pore size of the organic phase filtration membrane is 0.22 μm.
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| CN202221945622.8U CN218298148U (en) | 2022-07-26 | 2022-07-26 | Detection device and detection system for content of organic acid and solvent in tobacco essence |
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| CN202221945622.8U CN218298148U (en) | 2022-07-26 | 2022-07-26 | Detection device and detection system for content of organic acid and solvent in tobacco essence |
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