CN110726791A - Pretreatment method for detecting sweetener in electronic cigarette liquid or tobacco essence - Google Patents
Pretreatment method for detecting sweetener in electronic cigarette liquid or tobacco essence Download PDFInfo
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- CN110726791A CN110726791A CN201911102766.XA CN201911102766A CN110726791A CN 110726791 A CN110726791 A CN 110726791A CN 201911102766 A CN201911102766 A CN 201911102766A CN 110726791 A CN110726791 A CN 110726791A
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- electronic cigarette
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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
- G01N30/14—Preparation by elimination of some components
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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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Abstract
The invention relates to a pretreatment method for detecting a sweetening agent in electronic cigarette liquid or tobacco essence, which comprises the steps of completing the extraction of a sample by ultrapure water pure mechanical ultrasonic oscillation of the sample to be detected, and then using C18The powder is centrifuged to purify a sample, and a proper amount of supernatant is filtered by a water-phase filter membrane at present for the liquid to be detected for chromatographic detection.
Description
Technical Field
The invention belongs to the technical field of tobacco chemical component detection, and particularly relates to a pretreatment method for detecting a sweetening agent in electronic cigarette liquid or tobacco essence.
Background
In the purification process of sample pretreatment, the adsorbent is added for adsorbing part of matrix in the sample, so that the matrix effect can be effectively reduced, and C18The purifying agent belongs to an inverse phase adsorbent and can effectively remove nonpolar impurities such as lipid, sterol and the like. Taking electronic cigarette liquid and tobacco essence as investigation objects, adding C with different amounts into the extract18As a scavenger, optimizing C18The amount of the compound is used. The purification sample is obtained to the maximum extent, and a favorable means is provided for supervision and determination of the sweetening agent in the electronic cigarette liquid and the tobacco essence.
Respectively extracting the electronic cigarette liquid and the tobacco essence by using ultrapure water as an extraction solvent, sucking a proper amount of extract liquor into a centrifugal tube, adding C18 powder, and centrifuging to complete the purification of the sample. However, in the prior art, no proper sample pretreatment method exists, so that the problem of obvious interference in sample detection is caused.
Disclosure of Invention
The invention aims to provide a pretreatment method for detecting a sweetening agent in electronic cigarette liquid or tobacco essence, which provides a basis for detecting and controlling the content of related substances in the electronic cigarette liquid or the tobacco essence.
The invention is realized by the following technical scheme:
a pretreatment method for detecting a sweetening agent in electronic cigarette liquid or tobacco essence comprises the following steps:
1) weighing a first set amount of sample to be detected and placing the sample in a triangular flask with a plug;
2) adding a proper amount of extract liquid into a triangular flask with a plug;
3) extracting in a constant-temperature ultrasonic water bath for a first set time, and standing for a second set time;
4) sucking the second set amount of supernatant into the centrifuge tube, and adding C into the centrifuge tube18Centrifuging the powder for a third set time, and standing for a fourth set time;
5) and (4) absorbing the supernatant obtained in the step 4), filtering the supernatant into a chromatographic bottle through an aqueous phase filter membrane, and using the filtrate as a to-be-detected liquid of a to-be-detected sample for chromatographic analysis.
The extraction liquid is ultrapure water.
The constant-temperature ultrasonic water bath in the step 3) is extracted in a constant-temperature ultrasonic water bath at the temperature of 30 ℃.
The filtration with the water phase filter membrane is 0.22 mu m.
The invention has the beneficial effects that:
the pretreatment method of the technical method is an efficient pretreatment method for measuring the sweetener in the electronic cigarette liquid and the tobacco essence, and C is added18The powder decontaminates the sample to the maximum extent possible.
The technical scheme aims at the extraction mode, the extraction time, the volume of an extracting agent, the extraction temperature and C18The usage amount of the powder and the like are optimized, and the extraction efficiency is improved.
The extraction solvent used in the technical scheme is ultrapure water, has no pollution to the environment, and accords with the green development concept.
Drawings
The following figures are used to illustrate different extraction modes, amounts of extraction solutions, extraction times, extraction temperatures and C during the pretreatment of samples to be tested18Graph of the effect of powder usage on the extraction of the samples to be tested.
FIG. 1 is a graph showing the effect of different extraction methods on the extraction effect;
FIG. 2 is a graph showing the effect of extraction volume on extraction efficiency;
FIG. 3 is a graph showing the effect of extraction time on the extraction effect;
FIG. 4 is a graph of the effect of extraction temperature on extraction performance;
FIG. 5 is C18A graph of the effect of the amount of powder used on the extraction effect;
FIG. 6 is a flow chart of the measurement method of the present invention.
Detailed Description
The technical solutions of the present invention are described in detail below by examples, and the following examples are only exemplary and can be used only for explaining and explaining the technical solutions of the present invention, but not construed as limiting the technical solutions of the present invention.
Example 1
1) 0.5g of E-liquid was weighed into a 50mL triangular flask with a stopper.
2) Exactly 10mL of extract, in this case ultrapure water, was added.
3) Extracting in 30 deg.C constant temperature ultrasonic water bath for 15 min.
4) Sucking appropriate amount of supernatant into a centrifuge tube, and adding 20mg of C into the centrifuge tube18Pulverizing, centrifuging for 10min, and standing for 5 min.
5) And (4) sucking a proper amount of supernatant, filtering the supernatant into a chromatographic bottle through a 0.22-micron water-phase filter membrane, and performing high performance liquid chromatography analysis as a sample to be detected.
Example 2
1) 0.5g of tobacco flavor is weighed into a 50mL triangular flask with a plug.
2) Accurately adding 10mL of extraction liquid, wherein the extraction liquid is ultrapure water in the embodiment;
3) extracting in 30 deg.C constant temperature ultrasonic water bath for 15 min.
4) Sucking appropriate amount of supernatant into a centrifuge tube, and adding 20mg of C into the centrifuge tube18Pulverizing, centrifuging for 10min, and standing for 5 min.
5) And (4) sucking a proper amount of supernatant, filtering the supernatant into a chromatographic bottle through a 0.22-micron water-phase filter membrane, and performing high performance liquid chromatography analysis as a sample to be detected.
The technical scheme finishes the extraction of the sample by the pure mechanical ultrasonic oscillation of ultrapure water of the sample to be detected, and then uses C18The powder is centrifuged to purify a sample, and a proper amount of supernatant is filtered by a water-phase filter membrane at present for the liquid to be detected for chromatographic detection.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. A pretreatment method for detecting a sweetening agent in electronic cigarette liquid or tobacco essence is characterized by comprising the following steps:
1) weighing a first set amount of sample to be detected and placing the sample in a triangular flask with a plug;
2) adding a proper amount of extract liquid into a triangular flask with a plug;
3) extracting in a constant-temperature ultrasonic water bath for a first set time, and standing for a second set time;
4) sucking the second set amount of supernatant into the centrifuge tube, and adding C into the centrifuge tube18Centrifuging the powder for a third set time, and standing for a fourth set time;
5) and (4) absorbing the supernatant obtained in the step 4), filtering the supernatant into a chromatographic bottle through an aqueous phase filter membrane, and using the filtrate as a to-be-detected liquid of a to-be-detected sample for chromatographic analysis.
2. The pretreatment method for detecting the sweetener in the electronic cigarette liquid or the tobacco essence according to claim 1, wherein the extract is ultrapure water.
3. The pretreatment method for detecting the sweetener in the electronic cigarette liquid or the tobacco flavor according to claim 1, wherein the constant-temperature ultrasonic water bath in the step 3) is a 30 ℃ constant-temperature ultrasonic water bath for extraction.
4. The pretreatment method for detecting the sweetener in the electronic cigarette liquid or the tobacco flavor according to claim 1, wherein the water-phase filter membrane filtration is 0.22 μm water-phase filter membrane filtration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201911102766.XA CN110726791A (en) | 2019-11-12 | 2019-11-12 | Pretreatment method for detecting sweetener in electronic cigarette liquid or tobacco essence |
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| CN201911102766.XA CN110726791A (en) | 2019-11-12 | 2019-11-12 | Pretreatment method for detecting sweetener in electronic cigarette liquid or tobacco essence |
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| CN110726791A true CN110726791A (en) | 2020-01-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115015453A (en) * | 2022-06-15 | 2022-09-06 | 河南中烟工业有限责任公司 | Pretreatment method for detecting sweetener in oral smokeless tobacco product |
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| CN106324150A (en) * | 2016-11-25 | 2017-01-11 | 四川省食品药品检验检测院 | Method for determining eight sweetening agents in Baijiu by high-performance liquid chromatography-low-temperature evaporative light scattering detector method |
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| KR101662498B1 (en) * | 2015-11-24 | 2016-10-05 | 세종대학교산학협력단 | Method for production of high natural sweetner, phyllodulcin from leaf of Hydrangea tea |
| CN106324150A (en) * | 2016-11-25 | 2017-01-11 | 四川省食品药品检验检测院 | Method for determining eight sweetening agents in Baijiu by high-performance liquid chromatography-low-temperature evaporative light scattering detector method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115015453A (en) * | 2022-06-15 | 2022-09-06 | 河南中烟工业有限责任公司 | Pretreatment method for detecting sweetener in oral smokeless tobacco product |
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Application publication date: 20200124 |