CN109387590B - Extraction device and extraction and analysis method for chemical components in cigarette core material - Google Patents
Extraction device and extraction and analysis method for chemical components in cigarette core material Download PDFInfo
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- CN109387590B CN109387590B CN201811156138.5A CN201811156138A CN109387590B CN 109387590 B CN109387590 B CN 109387590B CN 201811156138 A CN201811156138 A CN 201811156138A CN 109387590 B CN109387590 B CN 109387590B
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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
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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
- G01N30/12—Preparation by evaporation
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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
- G01N2030/062—Preparation extracting sample from raw material
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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
- G01N30/12—Preparation by evaporation
- G01N2030/126—Preparation by evaporation evaporating sample
Abstract
The invention discloses an extraction device and an extraction and analysis method of chemical components in a cigarette core material, which comprises the steps of extracting the chemical components of the cigarette core material and analyzing by a sample instrument to be tested, and specifically comprises the following steps: (1) wrapping the tobacco core material with filter paper, and placing in a liquid storage tube of an extraction device; the distillation end of the extraction device is inorganic salt water solution, the extraction end of the extraction device is medium-polarity organic solvent, and the cigarette core material is extracted and separated. (2) After extraction, the extract is rapidly dehydrated and filtered by anhydrous sodium sulfate. (3) And concentrating the filtrate. (4) The liquid to be detected is used for the analysis and the measurement of an instrument. The invention can obtain the information of the chemical components in the cigarette core material as much as possible, and can effectively avoid the influence of the glycerol in the cigarette core material on the detection of other chemical components. The method can be effectively used for analyzing, measuring and evaluating the chemical components in the cigarette core material of the heating non-combustible cigarette, and has practical guiding significance for developing novel tobacco products.
Description
Technical Field
The invention relates to an extraction device and an extraction and analysis method for chemical components in a cigarette core material, in particular to an extraction device and an extraction and analysis method for chemical components in a cigarette core material of a heating non-combustible cigarette, and belongs to the technical field of cigarettes.
Background
The cigarette which is not burnt after being heated releases smoke through heating the tobacco material, certain tobacco characteristic feeling can be provided for consumers, and the release amount of harmful ingredients is low. The cigarette core material of the cigarette which is not burnt by heating is only heated but not burnt, so that most of chemical components in smoke are generated by heating and volatilizing the chemical components in the cigarette core material. In order to analyze the chemical components in the cigarette core material, a series of pre-treatments such as extraction, purification, concentration and the like are required to be carried out on the cigarette core material. Different from the traditional cigarette, the cigarette core material of the heating non-combustible cigarette contains additional fiber, tobacco material, additional glycerol and essence and spice, and the glycerol content is very high. Experimental research shows that if the tobacco core material extracting solution contains high-concentration glycerol, the glycerol can affect the analysis of other chemical components.
How to obtain rich chemical composition information under the condition of reducing the content of glycerol in the liquid to be detected is the key for analyzing the chemical compositions of the cigarette core material of the heating non-combustible cigarette. Therefore, it is of practical significance to develop an extraction device and an extraction and analysis method for chemical components in the core material of the cigarette which is not combusted by heating.
Disclosure of Invention
The invention solves the technical problem of providing the device for extracting the chemical components in the tobacco core material, which can prevent the tobacco core material from being burnt due to being stuck on the wall of a glass flask in the heating and boiling process and the chemical components from being damaged, and the device realizes the simultaneous extraction and extraction separation, can efficiently and temporarily separate glycerol in an extracting solution to a distillation end flask, and can separate the chemical components in the tobacco core material to an extraction end flask, so that the content of the chemical components in the tobacco core material in the extraction end flask is high, and the device is favorable for carrying out chemical analysis and detection on the tobacco core material.
Meanwhile, the invention provides a method for extracting chemical components from the tobacco core material, and the extracting solution obtained by the method only contains a small amount of glycerol, so that the interference of the glycerol on the detection of other chemical components is reduced.
The invention also provides an analysis method of the chemical components in the cigarette core material, and the method realizes effective and comprehensive analysis of the chemical components in the cigarette core material of the cigarette which is not combusted by heating.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the extraction device for the chemical components in the cigarette core material comprises a liquid storage pipe for placing the cigarette core material, wherein an opening at the top end of the liquid storage pipe is connected with the bottom end of a condensing pipe, the top end of the condensing pipe is closed, a left connecting pipe and a right connecting pipe are arranged on the side wall of the top end of the condensing pipe in a bilateral symmetry mode, the left connecting pipe is connected with the top end of a left steam mixing pipe, the bottom end of the left steam mixing pipe is connected with the top end of a left liquid return pipe, the bottom end of the left liquid return pipe is connected with a distillation end flask, and the side wall of the left liquid return pipe is communicated with the side wall of the middle upper part of the liquid storage pipe through a first connecting pipe; the right connecting pipe is connected with the top end of the right steam mixing pipe, the bottom end of the right steam mixing pipe is connected with the top end of the right liquid return pipe, the bottom end of the right liquid return pipe is connected with the flask at the extraction end, and the side wall of the right liquid return pipe is connected with the bottom end of the liquid storage pipe through a second connecting pipe; the condenser pipe is provided with a condenser pipe cooling water inlet and a condenser pipe cooling water outlet, and the liquid storage pipe is provided with a liquid storage pipe cooling water inlet and a liquid storage pipe cooling water outlet.
The method for extracting chemical components from the cigarette core material comprises the following steps:
s01, extracting the tobacco core material by adopting the device, wrapping the tobacco core material with filter paper and placing the wrapped tobacco core material in the liquid storage tube; an inorganic salt aqueous solution is filled in the distillation end flask, a medium-polarity organic solvent is filled in the extraction end flask, the specific gravity of the medium-polarity organic solvent is greater than that of the inorganic salt aqueous solution, and the Soxhlet extraction and the simultaneous distillation extraction are carried out by utilizing the device;
s02, after extraction is finished, quickly dehydrating and filtering the extracting solution in the extraction end flask to obtain filtrate;
s03, concentrating the filtrate to obtain concentrated extract for later use.
The inorganic salt aqueous solution comprises water, a sodium chloride aqueous solution, a sodium sulfate aqueous solution, a magnesium chloride aqueous solution or a magnesium sulfate aqueous solution; the distillation end keeps the aqueous solution of inorganic salt boiling.
The medium-polarity organic solvent comprises dichloromethane or carbon tetrachloride, and the temperature in the extraction end flask is 50-80 ℃.
The time for simultaneous distillation and extraction is 3-6 h.
The method for quickly dehydrating the extracting solution adopts an anhydrous sodium sulfate small column method for dehydration.
The anhydrous sodium sulfate small column method comprises the following operation steps: taking a syringe injector, taking down the syringe, installing an organic phase needle type filter at the front end of the syringe injector, and then installing a certain amount of anhydrous sodium sulfate in the syringe; pouring the extract into the syringe, pushing the piston to make the extract flow through the anhydrous sodium sulfate and the organic phase needle type filter, and realizing the rapid dehydration and filtration of the extract.
The organic phase needle type filter comprises a microporous filter membrane with the pore diameter of 0.45um or 0.22 um.
Concentrating the filtrate by using a rotary evaporator.
The method for analyzing chemical components in the cigarette core material comprises the following steps of carrying out gas chromatography-mass spectrometry on the extracted concentrated solution.
The determination conditions of the gas chromatography-mass spectrometry are as follows: gas chromatography parameters: the chromatographic column is a DB-35 quartz capillary column (30m multiplied by 0.25mm multiplied by 0.25um), the carrier gas is nitrogen, the flow rate is 1mL/min, the sample injection amount is 1ul, the sample injection port temperature is 280 ℃, the split ratio is 10:1, and the column temperature adopts a programmed temperature rising mode: the initial temperature is 50 ℃, the temperature is increased to 260 ℃ at the speed of 10 ℃/min, the temperature is increased to 280 ℃ at the speed of 20 ℃/min, and the temperature is maintained for 20 min; the mass spectrum parameters are as follows: transmission line temperature is 280 ℃, ionization mode: electron bombardment source EI; the monitoring mode is as follows: full scanning; the scanning range is 29-450amu, the ionization energy is 70eV, the ion source temperature is 230 ℃, the quadrupole rod temperature is 150 ℃, and the solvent delay is 5 min; standard library of charts: NIST.
The invention has the beneficial effects that:
1. the method adopts a mode of combining Soxhlet extraction and simultaneous distillation extraction to extract chemical components in the heating non-combustible cigarette core material, can realize the extraction of volatile chemical components in water extraction steam by an organic solvent and the direct extraction of the chemical components in the cigarette core material, can obtain as much information about the chemical components in the cigarette core material as possible, can be effectively used for the analysis, determination and evaluation of the chemical components in the heating non-combustible cigarette core material, and has practical guiding significance for developing novel tobacco products.
2. According to the invention, the extract to be extracted is wrapped by the filter paper and placed in the liquid storage tube of the extraction device, and the chemical components in the extract to be extracted are extracted by the Soxhlet extraction principle, so that the extraction efficiency of the chemical components is effectively improved, the chemical reaction of the object to be detected which is heated and boiled in water is avoided, and the authenticity of the detection result is improved.
3. The method adopts a mode of combining Soxhlet extraction and simultaneous distillation extraction to extract the cigarette core material of the heating non-combustible cigarette, so that the extracting solution only contains trace glycerol, thereby avoiding the influence of the glycerol in the extracting solution on the detection of other chemical components.
4. The invention adopts the anhydrous sodium sulfate small column method to carry out rapid dehydration and filtration, improves the dehydration efficiency of the extract liquor and shortens the treatment time of the extract liquor.
Drawings
FIG. 1 is a schematic view of an extraction apparatus according to the present invention;
FIG. 2 is a mass spectrum of a sample detected in the present invention.
Detailed Description
For a more clear description of the objects, aspects and advantages of the present invention, reference is now made to the accompanying drawings, which illustrate some, but not all embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
As shown in fig. 1-2, the device for extracting chemical components from a tobacco core material comprises a liquid storage pipe 3 for placing the tobacco core material, wherein an opening at the top end of the liquid storage pipe 3 is connected with the bottom end of a condensation pipe, the top end of the condensation pipe is closed, a left connecting pipe and a right connecting pipe are symmetrically arranged on the side wall of the top end of the condensation pipe in a left-right manner, the left connecting pipe is connected with the top end of a left steam mixing pipe 1, the bottom end of the left steam mixing pipe 1 is connected with the top end of a left liquid return pipe 2, the bottom end of the left liquid return pipe 2 is connected with a distillation end flask 4, and the side wall of the left liquid return pipe 2 is communicated with the side wall of the middle upper part of the liquid storage pipe 3 through a first connecting pipe; the right connecting pipe is connected with the top end of the right steam mixing pipe, the bottom end of the right steam mixing pipe is connected with the top end of the right liquid return pipe, the bottom end of the right liquid return pipe is connected with the flask 5 at the extraction end, and the side wall of the right liquid return pipe is connected with the bottom end of the liquid storage pipe 3 through a second connecting pipe; the condenser pipe is provided with a condenser pipe cooling water inlet 6 and a condenser pipe cooling water outlet 7, and the liquid storage pipe 3 is provided with a liquid storage pipe cooling water inlet 8 and a liquid storage pipe cooling water outlet 9.
The method for extracting chemical components from the cigarette core material comprises the following steps: 2.00g of the cigarette core material of the cigarette which is not combusted by heating is weighed, cut into small pieces, wrapped by filter paper and placed in the liquid storage tube 3. The left steam mixing pipe 1, the left liquid reflux pipe 2 and the liquid storage pipe 3 of the extraction device are connected and assembled. A500 ml distillation end flask 4 was taken, 100ml of water and 20g of sodium chloride were added, and a small amount of zeolite was added, and attached to the distillation end of an extraction apparatus. A100 ml extraction end flask 5 was taken, 60ml dichloromethane was added, and a small amount of zeolite was added, attached to the extraction end of the extraction apparatus. The condenser pipe cooling water inlet 6 and the condenser pipe cooling water outlet 7 on the condenser pipe and the liquid storage pipe cooling water inlet 8 and the liquid storage pipe cooling water outlet 9 on the liquid storage pipe 3 are connected by hoses, and the cooling water is opened. The distillation end flask 4 is heated by an electric heating jacket to keep the water solution at the distillation end boiling. The extraction end flask 5 was heated in a water bath at 60 ℃. The extraction time is 4 h. After extraction, the extract is dehydrated quickly by adopting an anhydrous sodium sulfate small column method and filtered. Transferring the filtrate into a concentration bottle, and concentrating the filtrate to about 1.0ml by using a rotary evaporator to obtain a solution to be detected.
Wherein, the extraction solution is quickly dehydrated by adopting an anhydrous sodium sulfate small column method, and the operation is as follows: taking a 100ml syringe injector, taking down an injection needle, installing a 0.22um organic phase needle type filter at the front end of the syringe injector, and then installing 10ml anhydrous sodium sulfate in the syringe; pouring the extractive solution into syringe, pushing piston to make the extractive solution flow through anhydrous sodium sulfate and filter for rapid dehydration and filtration.
The method for analyzing the chemical components in the cigarette core material comprises the following steps: and (4) carrying out gas chromatography-mass spectrometry on the liquid to be detected.
The determination conditions of the gas chromatography-mass spectrometry are as follows: gas chromatography parameters: the chromatographic column is a DB-35 quartz capillary column (30m multiplied by 0.25mm multiplied by 0.25um), the carrier gas is nitrogen, the flow rate is 1mL/min, the sample injection amount is 1ul, the sample injection port temperature is 280 ℃, the split ratio is 10:1, and the column temperature adopts a programmed temperature rising mode: the initial temperature is 50 ℃, the temperature is increased to 260 ℃ at the speed of 10 ℃/min, the temperature is increased to 280 ℃ at the speed of 20 ℃/min, and the temperature is maintained for 20 min.
The mass spectrum parameters are as follows: transmission line temperature is 280 ℃, ionization mode: electron bombardment source EI; the monitoring mode is as follows: full scanning; the scanning range is 29-450amu, the ionization energy is 70eV, the ion source temperature is 230 ℃, the quadrupole rod temperature is 150 ℃, and the solvent delay is 5 min; standard library of charts: NIST.
Table 1 shows the results of analysis of chemical components in a heat-not-burn cigarette core material by the method of this example.
TABLE 1 analysis results of chemical components in a cigarette core material of a heat-not-burn cigarette
Example 2
This example differs from example 1 only in that: in the method for extracting chemical components in the cigarette core material, an inorganic salt aqueous solution is a sodium sulfate aqueous solution, a medium-polarity organic solvent is carbon tetrachloride, the temperature in an extraction end flask 5 is 80 ℃, the distillation extraction time is 3 hours, and an organic phase needle type filter is a microporous filter membrane with the aperture of 0.45 um.
Example 3
This example differs from example 1 only in that: in the method for extracting chemical components from the cigarette core material, the inorganic salt aqueous solution is a magnesium chloride aqueous solution, the temperature in the extraction end flask 5 is 50 ℃, and the distillation extraction time is 6 hours.
Example 4
This example differs from example 1 only in that: in the method for extracting chemical components from the cigarette core material, the inorganic salt aqueous solution is magnesium sulfate aqueous solution, the temperature in the extraction end flask 5 is 70 ℃, and the distillation extraction time is 5 hours.
Example 5
This example differs from example 1 only in that: in the method for extracting chemical components from the cigarette core material, the inorganic salt water solution is an aqueous solution, the temperature in the extraction end flask 5 is 65 ℃, and the distillation extraction time is 4.5 hours.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (6)
1. The method for extracting the chemical components in the cigarette core material is characterized by comprising the following steps: the method for extracting the chemical components in the cigarette core material adopts an extraction device for extracting the chemical components in the cigarette core material to extract the cigarette core material;
the extraction device for the chemical components in the cigarette core material comprises a liquid storage pipe (3) for placing the cigarette core material, wherein an opening at the top end of the liquid storage pipe (3) is connected with the bottom end of a condensing pipe, the top end of the condensing pipe is closed, a left connecting pipe and a right connecting pipe are symmetrically arranged on the side wall of the top end of the condensing pipe in a left-right mode, the left connecting pipe is connected with the top end of a left steam mixing pipe (1), the bottom end of the left steam mixing pipe (1) is connected with the top end of a left liquid return pipe (2), the bottom end of the left liquid return pipe (2) is connected with a distillation end flask (4), and the side wall of the left liquid return pipe (2) is communicated with the side wall of the middle upper part of the liquid storage pipe (3) through a first connecting pipe; the right connecting pipe is connected with the top end of the right steam mixing pipe, the bottom end of the right steam mixing pipe is connected with the top end of a right liquid return pipe, the bottom end of the right liquid return pipe is connected with an extraction end flask (5), and the side wall of the right liquid return pipe is connected with the bottom end of the liquid storage pipe (3) through a second connecting pipe; the condenser pipe is provided with a condenser pipe cooling water inlet (6) and a condenser pipe cooling water outlet (7), and the liquid storage pipe (3) is provided with a liquid storage pipe cooling water inlet (8) and a liquid storage pipe cooling water outlet (9);
the method for extracting chemical components from the cigarette core material comprises the following steps:
s01, extracting the tobacco core material by adopting the device, wrapping the tobacco core material with filter paper and placing the wrapped tobacco core material in the liquid storage tube (3); the distillation end flask (4) is filled with an inorganic salt aqueous solution, the extraction end flask (5) is filled with a medium polar organic solvent, the specific gravity of the medium polar organic solvent is greater than that of the inorganic salt aqueous solution, and the Soxhlet extraction and the simultaneous distillation extraction are carried out by utilizing the device;
s02, after extraction is finished, quickly dehydrating and filtering the extracting solution in the extraction end flask (5) to obtain filtrate;
s03, concentrating the filtrate to obtain concentrated extract for later use;
the inorganic salt aqueous solution comprises water, a sodium chloride aqueous solution, a sodium sulfate aqueous solution, a magnesium chloride aqueous solution or a magnesium sulfate aqueous solution; the distillation end keeps the inorganic salt water solution boiling;
the medium-polarity organic solvent comprises dichloromethane or carbon tetrachloride, and the temperature in the extraction end flask (5) is 50-80 ℃;
the time for simultaneous distillation and extraction is 3-6 h.
2. The method of claim 1, wherein the extraction of chemical components from the core material comprises: the method for quickly dehydrating the extracting solution adopts an anhydrous sodium sulfate small column method for dehydration.
3. The method of claim 2, wherein the extraction of chemical components from the core material comprises: the anhydrous sodium sulfate small column method comprises the following operation steps: taking a syringe injector, taking down the syringe, installing an organic phase needle type filter at the front end of the syringe injector, and then installing a certain amount of anhydrous sodium sulfate in the syringe; pouring the extract into the syringe, pushing the piston to make the extract flow through the anhydrous sodium sulfate and the organic phase needle type filter, and realizing the rapid dehydration and filtration of the extract.
4. The method of claim 3, wherein the extraction of chemical components from the core material comprises: the organic phase needle type filter comprises a microporous filter membrane with the pore diameter of 0.45um or 0.22 um.
5. The method of claim 1, wherein the extraction of chemical components from the core material comprises: concentrating the filtrate by using a rotary evaporator.
6. A method for analyzing chemical components in a cigarette core material is characterized by comprising the following steps: the method comprises the following steps:
extracting a concentrated solution of the tobacco core material by adopting the method for extracting the chemical components in the tobacco core material according to any one of claims 1 to 5;
carrying out gas chromatography-mass spectrometry on the concentrated solution of the extracted tobacco core material;
the determination conditions of the gas chromatography-mass spectrometry are as follows:
gas chromatography parameters: the chromatographic column is a DB-35 quartz capillary column, the carrier gas is nitrogen, the flow rate is 1ml/min, the sample injection amount is 1ul, the temperature of a sample injection port is 280 ℃, and the split ratio is 10: 1;
column temperature adopts a programmed heating mode: the initial temperature is 50 ℃, the temperature is increased to 260 ℃ at the speed of 10 ℃/min, the temperature is increased to 280 ℃ at the speed of 20 ℃/min, and the temperature is maintained for 20 min;
the mass spectrum parameters are as follows: the temperature of the transmission line is 280 ℃;
an ionization mode: electron bombardment source EI;
the monitoring mode is as follows: full scanning, wherein the scanning range is 29-450amu, the ionization energy is 70eV, the ion source temperature is 230 ℃, the quadrupole rod temperature is 150 ℃, and the solvent delay time is 5 min;
standard library of charts: NIST.
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| CN101439234A (en) * | 2007-11-21 | 2009-05-27 | 深圳波顿香料有限公司 | Improved device for simultaneous distillation and extraction |
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| CN203629941U (en) * | 2013-12-05 | 2014-06-04 | 广东中烟工业有限责任公司 | Device capable of simultaneously distilling and extracting |
| CN204034306U (en) * | 2014-07-30 | 2014-12-24 | 河南中烟工业有限责任公司 | A kind of modified SDE method increasing Liquid-liquid Extraction Processes |
| CN104621708A (en) * | 2015-01-29 | 2015-05-20 | 湖南中烟工业有限责任公司 | Burley tobacco extractive, electronic tobacco juice and tobacco extraction method |
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- 2018-09-30 CN CN201811156138.5A patent/CN109387590B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101439234A (en) * | 2007-11-21 | 2009-05-27 | 深圳波顿香料有限公司 | Improved device for simultaneous distillation and extraction |
| CN103235060A (en) * | 2012-10-15 | 2013-08-07 | 红塔烟草(集团)有限责任公司 | Optimized extraction detection method for tobacco aroma substance simultaneous distillation extraction (SDE) |
| CN203629941U (en) * | 2013-12-05 | 2014-06-04 | 广东中烟工业有限责任公司 | Device capable of simultaneously distilling and extracting |
| CN204034306U (en) * | 2014-07-30 | 2014-12-24 | 河南中烟工业有限责任公司 | A kind of modified SDE method increasing Liquid-liquid Extraction Processes |
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