阅读说明：本技术 一种烟用香精萃取分离装置和方法 (Tobacco essence extraction and separation device and method ) 是由 张凤梅 钱颖颖 韩敬美 刘志华 唐石云 蒋薇 司晓喜 朱瑞芝 李振杰 蒋昆明 刘 于 2021-08-25 设计创作，主要内容包括：本发明公开一种烟用香精萃取分离装置,其包括萃取瓶(5)、第一密封盖(2)、控制器(1)、活动板(6)、连接条(4)、隔断阀(7)、第二密封盖(9)；萃取瓶(5)两端设有第一密封盖(2)和第二密封盖(9)；活动板(6)可在萃取瓶(5)内部上下移动；用于萃取过程中萃取液和萃余液的隔断和分离,还可搅拌让萃取剂和待萃取样品充分混合均匀；活动板(6)上有可开启与闭合的隔断阀(7)；控制器(1)通过连接条(4)与活动板(6)相连,用于控制活动板(6)位置及隔断阀(7)的开启与闭合。本发明能对香精萃取上层和下层溶液实现有效分离,萃取液和萃余液两层溶液均可直接用于化学成分分析,具有快速、准确、操作简单等优点。(The invention discloses an essence extraction and separation device for cigarettes, 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) and a second sealing cover (9); 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); the device is used for separating and separating the extraction liquid and the raffinate in the extraction process, and can also be stirred to fully and uniformly mix the extractant and the sample to be extracted; an isolating valve (7) which can be opened and closed is arranged on the movable plate (6); 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) and the opening and closing of the isolating valve (7). The invention can realize effective separation of the upper solution and the lower solution of essence extraction, and the two solutions of the extraction liquid and the raffinate can be directly used for chemical component analysis, and has the advantages of rapidness, accuracy, simple operation and the like.)

1. The utility model provides an essence extraction separator for cigarette which characterized in that: the extraction 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) and a second sealing cover (9);

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 and taking out an extraction liquid and a raffinate;

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 bottle (5) and the opening and closing of the isolating valve (7) on the movable plate (6).

2. The tobacco essence extraction and separation device 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.

3. The tobacco essence extraction and separation device 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.

4. The tobacco essence extraction and separation device 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.

5. The tobacco essence extraction and separation device 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).

6. The tobacco essence extraction and separation device 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.

7. The tobacco essence extraction and separation device according to claim 1, characterized in that: 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 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 0.5-50 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, the 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 to the layered position of the liquid level, the second adjusting valve of the controller (1) is rotated to 180 degrees, namely, the closing valve (7) is closed, the first sealing cover (2) or the second sealing cover (9) is opened, and the extraction liquid or the raffinate is taken out to carry out chemical component 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 (250mm × 4.6mm × 5 μm) or equivalent column; column temperature: 30-60 ℃; sample introduction amount: 5-10 mu L; the mobile phase A is water, the mobile phase B is acetonitrile, and the flow rate is 0.6-1.2 mL/min; gradient elution conditions were 0min, 15% a; 18min, 25% A; 30min, 45% A; 32min, 45% A; 34min, 15% A; 34min, 15% A;

detector conditions: temperature of the drift tube: 60-90 ℃; flow rate of atomizing gas: 1 to 3L/min.

Technical Field

The invention belongs to the field of analytical chemistry, and particularly relates to an extraction and separation device and method for tobacco essence.

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 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 an extraction and separation device and method for tobacco essence, which 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 an essence extraction and separation device for cigarettes, 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 and a second sealing cover 9;

the two ends of the extraction bottle 5 are provided with a first sealing cover 2 and a second sealing cover 9 which are used for adding an extracting agent and a sample to be extracted and taking out an extraction liquid and a raffinate;

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.

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 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 second aspect of the invention discloses an extraction and separation method of tobacco essence, which uses the extraction and separation device of the tobacco essence 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 0.5-50 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, the 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 to the liquid level layering position, the second adjusting valve of the controller 1 is rotated to 180 degrees, the isolating valve 7 is closed, the first sealing cover 2 or the second sealing cover 9 is opened, and the extraction liquid or the raffinate is taken out for chemical component 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 (250mm × 4.6mm × 5 μm) or equivalent column; column temperature: 30-60 ℃; sample introduction amount: 5-10 mu L; the mobile phase A is water, the mobile phase B is acetonitrile, and the flow rate is 0.6-1.2 mL/min; gradient elution conditions were 0min, 15% a; 18min, 25% A; 30min, 45% A; 32min, 45% A; 34min, 15% A; 34min, 15% A;

detector conditions: temperature of the drift tube: 60-90 ℃; flow rate of atomizing gas: 1 to 3L/min.

Compared with the prior art, the invention has the following beneficial effects:

compared with the prior art, the invention has the following beneficial effects:

1. the tobacco essence extraction and separation device 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, after extraction is finished, the first sealing cover 2 or the second sealing cover 9 is opened, and extraction liquid or raffinate is taken out to carry out chemical component analysis. The problem of liquid port blockage in the prior art can not occur.

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, the isolating valve 7 is arranged on the movable plate 6, 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 the cigarettes shows that the relative standard deviation of the integral area sum of volatile semi-volatile components in the essence is between 0.20 and 2.24 percent, and the relative standard deviation of the integral area sum of water-soluble or alcohol-soluble components in the essence is between 0.18 and 2.17 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 which 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, fat-soluble or alcohol-soluble substances in the tobacco essence, and has the advantages of rapidness, accuracy, simple operation and the like.

Drawings

FIG. 1 is a schematic structural diagram of an essence extraction and separation device for tobacco;

FIG. 2 is a schematic structural diagram of a movable plate in the tobacco flavor extraction and separation device;

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-sample to be extracted/raffinate and 9-second sealing cover.

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 of the embodiment includes an extraction bottle 5, a first sealing cover 2, a controller 1, a movable plate 6, a connecting bar 4, an isolating valve 7, and a second sealing cover 9; the two ends of the extraction bottle 5 are provided with a first sealing cover 2 and a second sealing cover 9 which are used for adding an extracting agent and a sample to be extracted and taking out an extraction liquid and a raffinate; 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 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 100mL, the height of the extraction flask is 10cm, and the diameter of the extraction flask is 4 cm.

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 of the sealing system is 0.5cm, and the diameter of the sealing system is 4 cm.

The connecting strip 4 material is the metal, and scalable length is 0 ~ 10cm, and is not 0, and the diameter is 0.5cm, 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 4 cm.

The isolating valve 7 is made of glass, is circular, has the diameter of 0.3cm and 15 quantity, is 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 left and right rotation angles are 180 degrees.

The tobacco essence extraction and separation method uses the tobacco essence extraction and separation device; 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 20g of a sample 8 to be extracted into the extraction flask 5, and continuously adding 50g of the extracting agent 3;

2. closing the first sealing cover 2 and the second sealing cover 9, extracting for 20min, and standing for 10 min;

3. after the extraction liquid 3 and the raffinate 8 are layered, the 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 liquid level layering position, the second adjusting valve of the controller 1 is rotated to 180 degrees, the isolating valve 7 is closed, the first sealing cover 2 or the second sealing cover 9 is opened, and the extraction liquid 3 or the raffinate 8 is taken out to perform chemical component analysis.

The instrumental analysis conditions of the volatile semi-volatile components were:

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 5 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 2 ℃/min, and the temperature is kept for 5 min; carrier gas: high-purity helium gas, a constant flow mode, and a column flow rate of 1 mL/min; and (3) sample introduction mode: split-flow sample injection, split-flow ratio 5: 1;

mass spectrum conditions: an ion source: an EI source; ionization energy: 70 eV; ion source temperature: 220 ℃; transmission line temperature: 230 ℃; detection mode: full scan monitoring mode, quality scan range: 30amu to 500 amu; solvent retardation: for 1 min.

The device is used for extracting and separating the essence for cigarettes, and fig. 3 is an analysis chromatogram of volatile semi-volatile components of the essence for cigarettes in example 1, and an analysis result shows that the relative standard deviation of the sum of the integral areas of the volatile semi-volatile components in the same essence for cigarettes is 0.20-2.24%.

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 (250mm × 4.6mm × 5 μm) or equivalent column; column temperature: 40 ℃; sample introduction amount: 10 mu L of the solution; the mobile phase A is water, the mobile phase B is acetonitrile, and the flow rate is 1.0 mL/min; gradient elution conditions were 0min, 15% a; 18min, 25% A; 30min, 45% A; 32min, 45% A; 34min, 15% A; 34min, 15% A;

detector conditions: temperature of the drift tube: 70 ℃; flow rate of atomizing gas: 2L/min.

The device is used for extracting and separating the essence for cigarettes, and figure 4 is an analysis chromatogram of water-soluble or alcohol-soluble components of the essence for cigarettes in example 1 of the invention, and an analysis result shows that the relative standard deviation of the total integral area of the water-soluble or alcohol-soluble components in the same essence for cigarettes is 0.18-2.17%.

Example 2

Selecting a common extraction separation device (shown in figure 5), fixing the extraction separation device on an extraction frame, closing a liquid outlet at the lower end, opening a bottle cap, adding 20g of a sample 8 to be extracted, and continuously adding 50g of an extracting agent 3; extracting for 20min, 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 integral areas of the volatile semi-volatile components in the same tobacco essence sample is between 8.23 and 14.35 percent.

Instrumental analysis conditions for water-soluble or alcohol-soluble components: the same as in example 1. The analysis result shows that the relative standard deviation of the total integral area of the water-soluble or alcohol-soluble components in the same tobacco essence sample is 7.35-13.17%.

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.