CN113834894A - Tobacco essence extraction and separation device with sampler and method - Google Patents
Tobacco essence extraction and separation device with sampler and method Download PDFInfo
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- 238000000605 extraction Methods 0.000 title claims abstract description 133
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 49
- 238000000926 separation method Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims description 19
- 244000061176 Nicotiana tabacum Species 0.000 title 1
- 238000007789 sealing Methods 0.000 claims abstract description 68
- 239000007788 liquid Substances 0.000 claims abstract description 51
- 241000208125 Nicotiana Species 0.000 claims abstract description 48
- 238000004458 analytical method Methods 0.000 claims abstract description 43
- 238000005070 sampling Methods 0.000 claims abstract description 25
- 239000000126 substance Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 17
- 239000011521 glass Substances 0.000 claims description 12
- 230000001105 regulatory effect Effects 0.000 claims description 12
- 235000019504 cigarettes Nutrition 0.000 claims description 10
- 239000004033 plastic Substances 0.000 claims description 10
- 229920003023 plastic Polymers 0.000 claims description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- 238000004811 liquid chromatography Methods 0.000 claims description 8
- 238000004817 gas chromatography Methods 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000000796 flavoring agent Substances 0.000 claims description 5
- 235000019634 flavors Nutrition 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 238000001819 mass spectrum Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 3
- 239000005695 Ammonium acetate Substances 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 229940043376 ammonium acetate Drugs 0.000 claims description 3
- 235000019257 ammonium acetate Nutrition 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 230000001276 controlling effect Effects 0.000 claims description 3
- 238000010828 elution Methods 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 2
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 2
- 239000005060 rubber Substances 0.000 claims description 2
- 238000007865 diluting Methods 0.000 claims 1
- 230000008569 process Effects 0.000 description 5
- 239000003205 fragrance Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000002304 perfume Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 235000013599 spices Nutrition 0.000 description 3
- 238000007599 discharging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 235000019505 tobacco product Nutrition 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000004454 trace mineral analysis Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a tobacco essence extraction and separation device with a sampler, which comprises an extraction bottle (5), a first sealing cover (2), a controller (1), a movable plate (6), a connecting strip (4), an isolating valve (7), a second sealing cover (9), a first sampler (10) and a second sampler (11); a first sealing cover (2) and a second sealing cover (9) are arranged at the two ends of the extraction bottle (5); the movable plate (6) can move up and down in the extraction flask (5); an openable and closable isolating valve (7) is arranged on the movable plate (6); the controller (1) is connected with the movable plate (6) through the connecting strip (4). The first sampler (10) extends into the extraction liquid; the second sampler (11) extends into the raffinate. The invention can realize effective separation of the upper solution and the lower solution of essence extraction, and the extraction liquid and the raffinate layer solution can be directly used for chemical component analysis, and has the advantages of rapidness, accuracy, simple operation and the like. The invention has the sampler, and the sampling is more convenient.
Description
Technical Field
The invention belongs to the field of analytical chemistry, and particularly relates to a device and a method for extracting and separating tobacco essence with a sampler.
Background
The aroma chemical substances released by the combustion and the pyrolysis of the tobacco are the main sources of the aroma and the taste of the cigarettes, but the quality of the tobacco as a crop is often influenced by the cultivation conditions and the later processing process, so that the quality of the tobacco is fluctuated. In order to meet the processing quality requirements of tobacco products and coordinate the miscellaneous gas of the tobacco, essence and spices are usually added to make up the deficiency of the fragrance of the tobacco and coordinate and improve the fragrance and the taste of the tobacco. The tobacco essence and spice has important functions of improving the taste of cigarettes, compensating and enhancing the fragrance of the cigarettes and highlighting the brand style of the cigarettes, so that the fragrance is the soul of the cigarettes, and the tobacco essence and spice technology is extremely important in the cigarette industry as an important content in the processing of tobacco products.
The tobacco essence has complex and various components, is usually a multi-component perfume raw material mixing system, and also has extremely low threshold concentration of certain perfume components, which belongs to trace analysis range, thereby providing extremely high requirements for the analysis of the tobacco essence perfume. Extraction and separation are an important pretreatment means and are often applied to essence analysis. Because the tobacco essence is more in variety, complex in components and some samples are still extremely viscous, the problems that a liquid outlet is blocked, an upper layer and a lower layer are difficult to separate and the like often occur when the conventional extracting device is used, the taking out and the component analysis of an upper layer solution are particularly not facilitated, and the accurate analysis of chemical components in the next step is difficult to guarantee. In addition, the sampling is complicated and requires opening the extraction bottle cap to complete the sampling process.
In order to accurately analyze the chemical components of the tobacco essence, a device needs to be developed to effectively extract and separate the essence. Especially, it is important to develop a special tobacco essence extraction and separation device and a component analysis method for tobacco essence samples with complex and extremely viscous components.
The present invention has been made to solve the above problems.
Disclosure of Invention
In order to solve the problems, the invention provides the device and the method for extracting and separating the tobacco essence with the sampler, and the device and the method have the advantages of rapidness, accuracy, simplicity in operation and the like.
The technical scheme adopted by the invention is as follows:
the invention provides a tobacco essence extraction and separation device with a sampler, which comprises an extraction bottle 5, a first sealing cover 2, a controller 1, a movable plate 6, a connecting bar 4, a closing valve 7, a second sealing cover 9, a first sampler 10 and a second sampler 11;
the two ends of the extraction bottle 5 are provided with a first sealing cover 2 and a second sealing cover 9 for adding an extracting agent and a sample to be extracted;
the movable plate 6 is positioned inside the extraction flask 5 and can move up and down inside the extraction flask 5; the device is used for separating and separating the extraction liquid and the raffinate in the extraction process, and can also play a role in stirring to fully and uniformly mix the extractant and the sample to be extracted;
the movable plate 6 is provided with the isolating valve 7, and the isolating valve 7 can be opened and closed;
the controller 1 is connected with the movable plate 6 through the connecting strip 4 and is used for controlling the position of the movable plate 6 inside the extraction flask 5 and the opening and closing of the isolating valve 7 on the movable plate 6;
the first sampler 10 is positioned on the first sealing cover 2, and is provided with a first sampler piston 12, a first sampler needle cylinder 13, a sampler water remover 14 and a first sampling needle 15, and the first sampling needle 15 of the first sampler extends into the extraction liquid; the second sampler 11 is located on the second sealing cover 9, and is provided with a second sampler piston 18, a second sampler syringe 17, and a second sampling needle 16, and the second sampling needle 16 of the second sampler extends into the raffinate. The effect of the water removal agent 14 of the sampler is to remove water, if there is water in the essence sample to be extracted, a small amount of water may enter the extraction liquid during the extraction process, and the water entering the gas chromatography along with the extraction liquid will affect the chromatographic column and the mass spectrum, affecting the analysis result. The water removing agent is used for removing a small amount of water in the extraction liquid, protecting a gas chromatographic column and a mass spectrum, keeping a good chromatographic peak shape and ensuring the accuracy and effectiveness of an analysis result.
In the drawings, reference numeral 3 denotes both the extractant and the extraction liquid, and reference numeral 8 denotes both the raffinate of the sample to be extracted, the extractant and the sample to be extracted before the extraction separation, and the extraction liquid and the raffinate after the extraction separation.
Preferably, the diameter of the sampler 10 and the sampler 11 is 0.5-2 cm, and the volume is 1 muL-5 mL; scales are arranged on the first sampler syringe 13 and the second sampler syringe 17, and the measuring range is 1 mu L-5 mL; the first sampling needle 15 and the second sampling needle 16 respectively extend into the extraction liquid and the raffinate, the length is 0.1-50 cm, and the diameter is 0.05-3 mm; the sampler dehydrator 14 is anhydrous sodium sulfate, anhydrous calcium chloride or anhydrous magnesium sulfate, is uniformly distributed on the inner wall of the sampler needle cylinder, has the weight of 0.05-5 g, and is used for removing a small amount of water in the extraction liquid; the first sampler 10 and the second sampler 11 are suitable for direct sample analysis of gas chromatography and liquid chromatography.
Preferably, the controller 1 is provided with a first adjusting valve (not shown in the figure) of the movable plate 6, and the movable plate 6 is adjusted to move up and down inside the extraction flask 5 by pressing the first adjusting valve up and down;
the controller 1 is provided with a second regulating valve (not shown in the figure) of the isolating valve 7, and the opening and closing of the isolating valve 7 are regulated by rotating the second regulating valve left and right.
Preferably, the extraction flask 5 is made of glass or plastic, is cylindrical, has a volume of 5-1000 mL, a height of 2-50 cm and a diameter of 0.5-30 cm.
Preferably, the first sealing cover 2 and the second sealing cover 9 are made of glass, plastic or rubber, are cylindrical, and form a sealing system with the extraction bottle 5, the height is 0.1-2 cm, and the diameter is 0.5-30 cm.
Preferably, the connecting strip 4 is made of metal or plastic, the telescopic length is 0-50 cm and is not 0, the diameter is 0.05-1 cm, the telescopic length of the connecting strip 4 is adjusted by the pressing force of a first adjusting valve on the controller 1, so that the movable plate 6 moves up and down in the extraction flask 5, and the position of the movable plate 6 in the extraction flask 5 is controlled.
Preferably, the movable plate 6 is made of glass, metal or plastic, is circular in shape, and has a diameter of 0.5-30 cm.
Preferably, the isolating valve 7 is made of glass, metal or plastic, is circular, has a diameter of 0.1-5 cm, is 0-50 in number and is not 0, and is adjusted to be opened or closed by the rotation angle of a second adjusting valve on the controller 1, wherein the rotation angle is 0-180 degrees.
The invention discloses a tobacco essence extraction and separation method, which uses the tobacco essence extraction and separation device with a sampler in the first aspect of the invention;
the method comprises the following steps:
1. opening the first sealing cover 2 or the second sealing cover 9, opening the isolating valve 7, adding 0.5-50 g of a sample to be extracted or 0.5-50 g of a solid sample and 0.5-50 g of a diluted solution into the extraction flask 5, wherein the diluted solution is water, and continuously adding 0.5-900 g of an extracting agent;
2. closing the first sealing cover 2 and the second sealing cover 9, extracting for 5-60 min, and standing for 5-30 min;
3. after the extraction liquid and the raffinate are layered, pressing a first adjusting valve of a controller 1, adjusting the length of a connecting strip 4 to control a movable plate 6 to stay at a liquid level layering position, rotating a second adjusting valve of the controller 1 to 180 degrees, namely closing an isolating valve 7, pulling a piston of a first sampler 10 or a second sampler 11 outwards, taking 1-2 mL of the extraction liquid or the raffinate after extraction separation into a sampler cylinder, pulling out the sampler without opening a first sealing cover 2 or a second sealing cover 9, and transferring a sample into a chromatographic bottle to perform chemical component analysis; or 1-10 mu L of extraction liquid or raffinate liquid separated by extraction is extracted into the needle cylinder of the sampler without opening the first sealing cover 2 or the second sealing cover 9, the sampler is pulled out, and the sampler is directly manually put into an instrument for on-line analysis.
Preferably, the analysis method of the volatile semi-volatile components is GC/MS (gas chromatography-mass spectrometry), and the analysis conditions are as follows:
gas chromatography conditions: the chromatographic column is DB-5MS capillary chromatographic column (60m × 0.25mm × 0.25 μm) or equivalent column; the sample injection amount is 1-10 mu L; sample inlet temperature: 230 ℃; temperature programming: the initial temperature is 40 ℃, the temperature is kept for 1min, the temperature is increased to 240 ℃ at the speed of 1-4 ℃/min, and the temperature is kept for 5-10 min; carrier gas: high-purity helium gas is adopted, the constant flow mode is adopted, and the column flow is 1-2 mL/min; and (3) sample introduction mode: split-flow sample introduction, wherein the split-flow ratio is 2-10: 1;
mass spectrum conditions: an ion source: an EI source; ionization energy: 70 eV; ion source temperature: 210-230 ℃; transmission line temperature: 220-250 ℃; detection mode: full scan monitoring mode, quality scan range: 30amu to 500 amu; solvent retardation: 0.2-2 min.
Preferably, the method for analyzing the water-soluble or alcohol-soluble components is liquid chromatography (HPLC), and the analysis conditions are as follows:
liquid chromatography conditions: the chromatographic column is C18 high performance liquid chromatographic column (150mm × 4.6mm × 5 μm) or equivalent column; column temperature: 30-60 ℃; sample introduction amount: 5-15 muL; the mobile phase A is 0.02mol/L ammonium acetate water solution, the mobile phase B is acetonitrile, and the flow rate is 0.6-1.2 mL/min; gradient elution conditions were 0min, 95% a; 10min, 55% A; 11.1min, 5% A; 13min, 5% A; 13.1min, 95% A; 16min, 95% A;
detector conditions: the detection wavelength is 420 nm-620 nm.
Compared with the prior art, the invention has the following beneficial effects:
1. the tobacco essence extraction and separation device with the sampler has the advantages that layering is more accurate after extraction is finished, the movable plate 6 capable of moving up and down is arranged in the extraction bottle 5, the extraction bottle can be used for separating and separating extraction liquid and raffinate in the extraction process, and the stirring effect can be achieved to fully and uniformly mix an extractant and a sample to be extracted; after the extraction liquid and the raffinate are layered, the first regulating valve of the controller 1 is pressed, the length of the connecting strip 4 is regulated to control the movable plate 6 to stay to the layered position of the liquid level, the second regulating valve of the controller 1 is rotated to 180 degrees, namely, the closing valve 7 is closed, the layered position is accurately layered by virtue of physical action after extraction is finished, and the problems that the upper layer and the lower layer are difficult to separate in the prior art are solved.
2. The two ends of the extraction bottle 5 are provided with a first sealing cover 2 and a second sealing cover 9, and the first sampler 10 and the second sampler 11 are arranged on the covers. After extraction is finished, pulling a piston of the first sampler 10 or the second sampler 11 outwards, extracting 1-2 mL of extraction liquid or raffinate after extraction separation into a sampler cylinder, pulling out the sampler without opening the first sealing cover 2 or the second sealing cover 9, and transferring a sample into a chromatographic bottle to perform chemical component analysis; or 1-10 mu L of extraction liquid or raffinate liquid separated by extraction is extracted into the needle cylinder of the sampler without opening the first sealing cover 2 or the second sealing cover 9, the sampler is pulled out, and the sampler is directly manually put into an instrument for on-line analysis.
3. The extraction bottle has high accuracy, the first sealing cover 2 and the second sealing cover 9 are arranged at the two ends of the extraction bottle 5, extraction is completed in a closed system with a fixed volume, and loss of volatile semi-volatile components in tobacco essence in the transfer process is greatly reduced. Meanwhile, the movable plate 6 capable of moving up and down is arranged in the tobacco essence extraction and separation device with the sampler, the movable plate 6 is provided with the isolating valve 7, the movable plate 6 and the isolating valve 7 can also play a role in stirring to fully and uniformly mix the solution, so that the reduction of extraction efficiency caused by the nonuniform mixing of the solution in the extraction process is reduced, and the accuracy of the analysis process is improved. The analysis result of the essence for extracting cigarettes shows that the relative standard deviation of the integral area sum of volatile semi-volatile components in the essence is between 0.19 and 2.43 percent, and the relative standard deviation of the integral area sum of water-soluble or alcohol-soluble components in the essence is between 0.21 and 2.57 percent.
4. The invention has simple analysis steps, can carry out sample injection analysis only after solvent extraction, has simple steps, and simultaneously provides the one-stop tobacco essence extraction and separation device with the sampler, and is easy to popularize.
5. The extraction bottle, the sealing cover, the controller, the movable plate, the connecting strip, the isolating valve and the like are prepared from materials which are easily available in a laboratory, and the cost is low.
6. The device and the method are wide in applicability, are suitable for different types of tobacco essence samples such as solid and liquid, and are particularly suitable for viscous samples which are easy to block a common extraction device; meanwhile, due to the existence of the movable plate, the upper layer solution and the lower layer solution can be poured and analyzed at will through up-down inversion. The method is used for detecting volatile semi-volatile substances, water-soluble or alcohol-soluble substances in the tobacco essence, and has the advantages of rapidness, accuracy, simple operation and the like.
7. The invention also has a first sampler 10 and a second sampler 11, so that the sampling is more convenient, and the samplers are directly used for sample introduction and analysis of the instrument without sample transfer; the sealing cover does not need to be opened in the sampling step, the water removal and sample introduction analysis steps are simple, and no sample is lost.
Drawings
FIG. 1 is a schematic structural diagram of an essence extraction and separation device for tobacco with a sampler;
FIG. 2 is a schematic structural diagram of a movable plate in the tobacco flavor extraction and separation device with a sampler;
FIG. 3 is an analysis chromatogram of volatile and semi-volatile components of the tobacco flavor of example 1;
FIG. 4 is an analysis chromatogram of fat-soluble or alcohol-soluble components of the tobacco flavor of example 1;
FIG. 5 is a diagram of a conventional prior art extractive separation apparatus;
in the figure: 1-controller, 2-first sealing cover, 3-extractant/extract, 4-connecting strip, 5-extraction bottle, 6-movable plate, 7-isolating valve, 8-to-be-extracted sample/raffinate, 9-second sealing cover, 10-first sampler, 11-second sampler, 12-first sampler piston, 13-first sampler syringe, 14-sampler dehydrator, 15-first sampling needle, 16-second sampling needle, 17-second sampler syringe and 18-second sampler piston.
Detailed Description
The present invention will be described in further detail with reference to examples.
It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The materials or equipment used are not indicated by manufacturers, and all are conventional products available by purchase.
As used herein, the singular forms "a", "an", "the" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. It will be understood that when an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. Further, "connected" as used herein may include wirelessly connected.
In the description of the present invention, "a plurality" means two or more unless otherwise specified. The terms "inner," "upper," "lower," and the like, refer to an orientation or a state relationship based on that shown in the drawings, which is for convenience in describing and simplifying the description, and do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the invention.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "provided" are to be construed broadly, e.g., as being fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; may be directly connected or indirectly connected through an intermediate. To those of ordinary skill in the art, the specific meanings of the above terms in the present invention are understood according to specific situations.
It will be understood by those skilled in the art that, unless otherwise defined, all terms including technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
Example 1
As shown in fig. 1, the tobacco essence extraction and separation device with a sampler of this embodiment includes an extraction bottle 5, a first sealing cover 2, a controller 1, a movable plate 6, a connecting bar 4, a closing valve 7, a second sealing cover 9, a first sampler 10, and a second sampler 11; the two ends of the extraction bottle 5 are provided with a first sealing cover 2 and a second sealing cover 9 for adding an extracting agent and a sample to be extracted; the movable plate 6 is positioned inside the extraction flask 5 and can move up and down inside the extraction flask 5; the device is used for separating and separating the extraction liquid and the raffinate in the extraction process, and can also play a role in stirring to fully and uniformly mix the extractant and the sample to be extracted; the movable plate 6 is provided with the isolating valve 7, and the isolating valve 7 can be opened and closed; the controller 1 is connected with the movable plate 6 through the connecting strip 4, and is used for controlling the position of the movable plate 6 inside the extraction flask 5 and the opening and closing of the closing valve 7 on the movable plate 6. The first sampler 10 is positioned in the first sealing cover 2, and the first sampler 10 extends into the extraction liquid; the first sampler 10 is positioned on the first sealing cover 2, and is provided with a first sampler piston 12, a first sampler needle cylinder 13, a sampler water remover 14 and a first sampling needle 15, and the first sampling needle 15 of the first sampler extends into the extraction liquid; the second sampler 11 is located on the second sealing cover 9, and is provided with a second sampler piston 18, a second sampler syringe 17, and a second sampling needle 16, and the second sampling needle 16 of the second sampler extends into the raffinate.
The diameter of the sampler 10 and the sampler 11 is 1cm, and the volume is 1 mL; scales are arranged on the first sampler syringe 13 and the second sampler syringe 17, and the measuring range is 2 mL; the first sampling needle 15 and the second sampling needle 16 respectively extend into the extraction liquid and the raffinate, the length is 8cm, and the diameter is 1 mm; the sampler water remover 14 is anhydrous sodium sulfate, is uniformly distributed on the inner wall of the sampler needle cylinder, has the weight of 2g and is used for removing a small amount of water in the extraction liquid; the sampler 10 and the sampler 11 are suitable for direct sample analysis of gas chromatography and liquid chromatography.
The controller 1 is provided with a first adjusting valve (not shown in the figure) of the movable plate 6, and the movable plate 6 is adjusted to move up and down in the extraction flask 5 by pressing the first adjusting valve up and down; the controller 1 is provided with a second regulating valve (not shown in the figure) of the isolating valve 7, and the opening and closing of the isolating valve 7 are regulated by rotating the second regulating valve left and right.
The extraction flask 5 is made of glass and is cylindrical, the volume of the extraction flask is 500mL, the height of the extraction flask is 20cm, and the diameter of the extraction flask is 6 cm.
The first sealing cover 2 and the second sealing cover 9 are made of glass and are cylindrical, and form a sealing system with the extraction bottle 5, the height of the sealing system is 0.5cm, and the diameter of the sealing system is 6 cm.
The connecting strip 4 material is the metal, and scalable length is 0 ~ 50cm, and is not 0, and the diameter is 0.1cm, through the pressing force degree of first governing valve on the controller 1 is adjusted the flexible length of connecting strip 4 makes fly leaf 6 is in reciprocate in extraction flask 5, thereby control fly leaf 6 is in position in the extraction flask 5.
The movable plate 6 is made of glass, is circular and has a diameter of 6 cm.
The isolating valves 7 are made of glass, are circular, have the diameter of 0.3cm and the number of 25, and are adjusted to be opened or closed through the rotation angle of the second adjusting valve on the controller 1, and the left and right rotation angles are 180 degrees.
The tobacco essence extraction and separation method uses the tobacco essence extraction and separation device with the sampler; the method comprises the following steps:
1. opening the first sealing cover 2 or the second sealing cover 9, opening the isolating valve 7, adding 40g of the solid sample and 40g of the diluted solution into the extraction flask 5, and continuously adding 400g of the extracting agent 3;
2. closing the first sealing cover 2 and the second sealing cover 9, extracting for 10min, and standing for 10 min;
3. after the extraction liquid and the raffinate are layered, a first adjusting valve of the controller 1 is pressed, the length of the connecting strip 4 is adjusted to control the movable plate 6 to stay at the layered position of the liquid level, a second adjusting valve of the controller 1 is rotated to 180 degrees, namely, the closing valve 7 is closed, the piston of the first sampler 10 or the second sampler 11 is pulled outwards, 5 mu L of extraction liquid or 10 mu L of raffinate which is extracted and separated is taken into a sampler cylinder, the sampler is taken down, and the extraction liquid and the raffinate are directly manually fed into an instrument for on-line analysis.
The instrumental analysis conditions of the volatile semi-volatile components were:
gas chromatography conditions: the chromatographic column is DB-5MS capillary chromatographic column (30m × 0.25mm × 0.25 μm) or equivalent column; the sample injection amount is 5 mu L; sample inlet temperature: 200 ℃; temperature programming: the initial temperature is 40 ℃, the temperature is kept for 2min, the temperature is increased to 230 ℃ at the speed of 3 ℃/min, and the temperature is kept for 5 min; carrier gas: high-purity helium gas, a constant flow mode, and a column flow of 1.5 mL/min; and (3) sample introduction mode: split-flow sample injection, split-flow ratio 6: 1;
mass spectrum conditions: an ion source: an EI source; ionization energy: 70 eV; ion source temperature: 200 ℃; transmission line temperature: 200 ℃; detection mode: full scan monitoring mode, quality scan range: 30amu to 400 amu; solvent retardation: 0.3 min.
The device is used for extracting and separating the essence for cigarettes, and the analysis result shows that the relative standard deviation of the total integral area of volatile semi-volatile components in the same essence sample for cigarettes is between 0.19 and 2.43 percent.
The instrumental analysis conditions of the water-soluble or alcohol-soluble components were:
liquid chromatography conditions: the chromatographic column is C18 high performance liquid chromatographic column (150mm × 4.6mm × 5 μm) or equivalent column; column temperature: 30 ℃; sample introduction amount: 10 mu L of the solution; the mobile phase A is 0.02mol/L ammonium acetate water solution, the mobile phase B is acetonitrile, and the flow rate is 0.8 mL/min; gradient elution conditions were 0min, 95% a; 10min, 55% A; 11.1min, 5% A; 13min, 5% A; 13.1min, 95% A; 16min, 95% A;
detector conditions: the detection wavelength is 420 nm-620 nm.
The device is used for extracting and separating the tobacco essence, and the analysis result shows that the relative standard deviation of the total integral area of water-soluble or alcohol-soluble components in the same tobacco essence sample is 0.21-2.57%.
Example 2
Selecting a common extraction separation device, fixing the common extraction separation device on an extraction frame, closing a liquid outlet at the lower end, opening a bottle cap, adding 40g of a solid sample and 50g of a diluent, and continuously adding 400g of an extracting agent 3; extracting for 10min, and standing for 10 min; opening a lower-end liquid outlet, discharging the lower-layer solution for analysis, discharging the upper-layer solution from the lower-end liquid outlet for analysis after the lower-layer solution is discharged, and taking out the two layers of solutions from the lower-end liquid outlet; for a sticky or indissolvable solid sample, the lower end liquid outlet hole is blocked, and the extraction liquid and the raffinate cannot be taken out, and the sample is recommended to be subjected to dispersion pretreatment and then to extraction separation; the extraction separation device is kept vertical to the ground during the sample taking process.
Instrumental analysis conditions for volatile semi-volatile components: the same as in example 1. Analysis results show that the relative standard deviation of the sum of the integrated areas of the volatile semi-volatile components in the same tobacco essence sample is between 9.54 and 15.54 percent.
Instrumental analysis conditions for water-soluble or alcohol-soluble components: the same as in example 1. Analysis results show that the relative standard deviation of the sum of the integral areas of the water-soluble or alcohol-soluble components in the same tobacco essence sample is 8.45-14.37%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The utility model provides an essence extraction separator for cigarette with sampler which characterized in that: the device comprises an extraction bottle (5), a first sealing cover (2), a controller (1), a movable plate (6), a connecting strip (4), a closing valve (7), a second sealing cover (9), a first sampler (10) and a second sampler (11);
a first sealing cover (2) and a second sealing cover (9) are arranged at two ends of the extraction bottle (5) and are used for adding an extracting agent and a sample to be extracted;
the movable plate (6) is positioned inside the extraction flask (5) and can move up and down inside the extraction flask (5); the device is used for separating and separating the extraction liquid and the raffinate in the extraction process, and can also play a role in stirring to fully and uniformly mix the extractant and the sample to be extracted;
the movable plate (6) is provided with the isolating valve (7), and the isolating valve (7) can be opened and closed;
the controller (1) is connected with the movable plate (6) through the connecting strip (4) and is used for controlling the position of the movable plate (6) in the extraction flask (5) and the opening and closing of the isolating valve (7) on the movable plate (6);
the first sampler (10) is positioned on the first sealing cover (2), and is provided with a first sampler piston (12), a first sampler needle cylinder (13), a sampler water remover (14) and a first sampling needle (15), and the first sampling needle (15) of the first sampler extends into the extraction liquid; the second sampler (11) is positioned on the second sealing cover (9) and is provided with a second sampler piston (18), a second sampler needle cylinder (17) and a second sampling needle (16), and the second sampling needle (16) of the second sampler extends into the raffinate.
2. The tobacco essence extraction and separation device with the sampler according to claim 1, characterized in that: the diameter of the sampler (10) and the diameter of the sampler (11) are 0.5-2 cm, and the volume of the sampler is 1 mu L-5 mL; scales are arranged on the first sampler syringe (13) and the second sampler syringe (17), and the measuring range is 1 mu L-5 mL; the first sampling needle (15) and the second sampling needle (16) respectively extend into the extraction liquid and the raffinate, the length is 0.1-50 cm, and the diameter is 0.05-3 mm; the sampler water remover (14) is anhydrous sodium sulfate, anhydrous calcium chloride or anhydrous magnesium sulfate, is uniformly distributed on the inner wall of the sampler needle cylinder, has the weight of 0.05-5 g, and is used for removing a small amount of water in the extraction liquid; the first sampler (10) and the second sampler (11) are suitable for direct sample analysis of gas chromatography and liquid chromatography.
3. The tobacco essence extraction and separation device with the sampler according to claim 1, characterized in that: the controller (1) is provided with a first adjusting valve of the movable plate (6), and the movable plate (6) is adjusted to move up and down in the extraction bottle (5) by pressing the first adjusting valve up and down;
and the controller (1) is provided with a second regulating valve of the isolating valve (7), and the opening and closing of the isolating valve (7) are regulated by rotating the second regulating valve leftwards and rightwards.
4. The tobacco essence extraction and separation device with the sampler according to claim 1, characterized in that: the extraction bottle (5) is made of glass or plastic, is cylindrical, has a volume of 5-1000 mL, a height of 2-50 cm and a diameter of 0.5-30 cm.
5. The tobacco essence extraction and separation device with the sampler according to claim 1, characterized in that: the first sealing cover (2) and the second sealing cover (9) are made of glass, plastic or rubber, are cylindrical in shape, and form a sealing system with the extraction bottle (5), the height of the sealing system is 0.1-2 cm, and the diameter of the sealing system is 0.5-30 cm.
6. The tobacco essence extraction and separation device with the sampler according to claim 1, characterized in that: the connecting strip (4) material is metal or plastics, and scalable length is 0 ~ 50cm, and is not 0, and the diameter is 0.05 ~ 1cm, through the pressing force degree of first governing valve on controller (1) is adjusted the flexible length of connecting strip (4), makes fly leaf (6) are in reciprocate in extraction bottle (5), thereby control fly leaf (6) are in position in extraction bottle (5).
7. The tobacco essence extraction and separation device with the sampler according to claim 1, characterized in that: the movable plate (6) is made of glass, metal or plastic, is circular and has a diameter of 0.5-30 cm; the isolating valve (7) is made of glass, metal or plastic, is circular in shape, 0.1-5 cm in diameter, 0-50 in number and not 0, and is adjusted to be opened or closed by the rotation angle of the second adjusting valve on the controller (1), and the rotation angle is 0-180 degrees.
8. A method for extracting and separating tobacco essence is characterized by comprising the following steps: the tobacco essence extraction and separation device with the sampler based on any one of claims 1 to 7;
the method comprises the following steps:
(1) opening the first sealing cover (2) or the second sealing cover (9), opening the isolating valve (7), adding 0.5-50 g of a sample to be extracted or 0.5-50 g of a solid sample and 0.5-50 g of a diluting solution into the extraction bottle (5), and continuously adding 0.5-900 g of an extracting agent;
(2) closing the first sealing cover (2) and the second sealing cover (9), extracting for 5-60 min, and standing for 5-30 min;
(3) after the extraction liquid and the raffinate are layered, pressing a first adjusting valve of a controller (1), adjusting the length of a connecting strip (4) to control a movable plate (6) to stay at a liquid level layering position, rotating a second adjusting valve of the controller (1) to 180 degrees, namely closing an isolating valve (7), pulling a piston of a first sampler (10) or a second sampler (11) outwards, extracting 1-2 mL of extraction liquid or raffinate after extraction separation into a sampler cylinder, pulling out the sampler without opening a first sealing cover (2) or a second sealing cover (9), and transferring a sample into a chromatographic bottle to perform chemical component analysis; or 1-10 mu L of extraction liquid or raffinate liquid separated by extraction is extracted into the needle cylinder of the sampler without opening the first sealing cover (2) or the second sealing cover (9), the sampler is pulled out, and the sampler is directly manually operated to perform online analysis.
9. The tobacco flavor extraction and separation method according to claim 8, characterized in that: the analysis method of the volatile semi-volatile components is GC/MS (gas chromatography-mass spectrometry), and the analysis conditions are as follows:
gas chromatography conditions: the chromatographic column is DB-5MS capillary chromatographic column (60m × 0.25mm × 0.25 μm) or equivalent column; the sample injection amount is 1-10 mu L; sample inlet temperature: 230 ℃; temperature programming: the initial temperature is 40 ℃, the temperature is kept for 1min, the temperature is increased to 240 ℃ at the speed of 1-4 ℃/min, and the temperature is kept for 5-10 min; carrier gas: high-purity helium gas is adopted, the constant flow mode is adopted, and the column flow is 1-2 mL/min; and (3) sample introduction mode: split-flow sample introduction, wherein the split-flow ratio is 2-10: 1;
mass spectrum conditions: an ion source: an EI source; ionization energy: 70 eV; ion source temperature: 210-230 ℃; transmission line temperature: 220-250 ℃; detection mode: full scan monitoring mode, quality scan range: 30amu to 500 amu; solvent retardation: 0.2-2 min.
10. The tobacco flavor extraction and separation method according to claim 8, characterized in that: the analysis method of the water-soluble or alcohol-soluble components is liquid chromatography HPLC, and the analysis conditions are as follows:
liquid chromatography conditions: the chromatographic column is C18 high performance liquid chromatographic column (150mm × 4.6mm × 5 μm) or equivalent column; column temperature: 30-60 ℃; sample introduction amount: 5-15 muL; the mobile phase A is 0.02mol/L ammonium acetate water solution, the mobile phase B is acetonitrile, and the flow rate is 0.6-1.2 mL/min; gradient elution conditions were 0min, 95% a; 10min, 55% A; 11.1min, 5% A; 13min, 5% A; 13.1min, 95% A; 16min, 95% A;
detector conditions: the detection wavelength is 420 nm-620 nm.
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Application publication date: 20211224 |