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Method for analyzing and detecting alkaline flavor components by using direct solvent extraction gas chromatography-mass spectrometry

A gas chromatography-mass spectrometry and alkaline aroma technology, which is applied in the field of tobacco aroma components detection, can solve problems such as no distillation of alkaline aroma components, error in analysis results, high distillation temperature, etc., to achieve true and reliable analysis results, accurate and reliable analysis results, The effect of mild pretreatment conditions

Inactive Publication Date: 2016-03-30
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Although SDE is a commonly used sample pretreatment technology in the analysis of tobacco flavor components, SDE also inevitably has the following problems: (1) Simultaneous distillation extraction is an open system, which is heated and distilled at high temperature for a long time under air environment and atmospheric pressure. , some highly active basic fragrance components will undergo chemical reactions such as oxidation and thermal degradation
On the one hand, components that were not in the original sample were produced, and on the other hand, some of the original components were lost, which caused errors in the analysis results; (2) The distillation temperature was high, and the basic aroma components with a low boiling point would be lost, but the aqueous solution system caused the distillation The temperature cannot be too high, and the alkaline aroma components with too high boiling point cannot be distilled; (3) the alkaline components with very low content are difficult to quantify

Method used

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  • Method for analyzing and detecting alkaline flavor components by using direct solvent extraction gas chromatography-mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) Accurately weigh 15g of flue-cured tobacco powder sample, add 100mL of 10% sodium hydroxide solution, add 10μg of internal standard solution, soak for 15min, ultrasonically extract for 60min, and centrifuge to obtain the supernatant.

[0024] 2) Pour the supernatant into a separatory funnel, add 100mL of dichloromethane extraction solvent, shake well, let stand to separate layers, and release the lower dichloromethane phase. The extraction was repeated three times and the dichloromethane phase was collected. Add 20 g of anhydrous sodium sulfate, shake and let stand for 3 hours. Evaporate to 1 mL by rotary evaporation, filter with a 0.45 micron filter membrane and add to a chromatographic vial to obtain the sample to be tested.

[0025] 3) Use GC-MS instrument to detect the sample obtained in step 2). After the detection is completed, the spectral data are processed to obtain the analysis and test results of the basic aroma components.

Embodiment 2

[0027] 1) Accurately weigh 25g of flue-cured tobacco powder sample, add 200mL of 15% sodium hydroxide solution, add 10μg of internal standard solution, soak for 15min, ultrasonically extract for 60min, and centrifuge to obtain the supernatant.

[0028] 2) Pour the supernatant into a separatory funnel, add 100mL of dichloromethane extraction solvent, shake well, let stand to separate layers, and release the lower dichloromethane phase. The extraction was repeated three times and the dichloromethane phase was collected. Add 20 g of anhydrous sodium sulfate, shake and let stand for 3 hours. Evaporate to 1 mL by rotary evaporation, filter with a 0.45 micron filter membrane and add to a chromatographic vial to obtain the sample to be tested.

[0029] 3) Use GC-MS instrument to detect the sample obtained in step 2). After the detection is completed, the spectral data are processed to obtain the analysis and test results of the basic aroma components.

Embodiment 3

[0031] 1) Accurately weigh 20g of Burley tobacco powder sample, add 300mL of 20% sodium hydroxide solution, add 10μg of internal standard solution, soak for 15min, ultrasonically extract for 60min, and centrifuge to obtain the supernatant.

[0032] 2) Pour the supernatant into a separatory funnel, add 100mL of dichloromethane extraction solvent, shake well, let stand to separate layers, and release the lower dichloromethane phase. The extraction was repeated three times and the dichloromethane phase was collected. Add 20 g of anhydrous sodium sulfate, shake and let stand for 3 hours. Evaporate to 1 mL by rotary evaporation, filter with a 0.45 micron filter membrane and add to a chromatographic vial to obtain the sample to be tested.

[0033] 3) Use GC-MS instrument to detect the sample obtained in step 2). After the detection is completed, the spectral data are processed to obtain the analysis and test results of the basic aroma components.

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Abstract

The invention discloses a method for analyzing and detecting alkaline flavor components by using direct solvent extraction gas chromatography-mass spectrometry. The method is characterized by comprising the following specific steps: 1) accurately weighing a tobacco waste sample, adding a sodium hydroxide solution and an internal standard solution, soaking and performing ultrasonic extraction; 2) adding a dichloromethane extraction solvent into the supernate, repeatedly extracting for three times and collecting and merging the dichloromethane phase; adding anhydrous sodium sulfate, vibrating and then standing; performing rotary evaporation to 1mL; and filtering with a 0.45-micron filter membrane to obtain a to-be-detected sample; and 3) detecting the sample with a GC-MS instrument; and after the detection, treating the atlas data to obtain an analysis test result of alkaline flavor components. The method disclosed by the invention has the following advantages: the pretreatment process is simple, mild and fast; the alkaline flavor components in tobacco can be accurately tested; and the method is of important theoretical significance and application value in directing the scientific cigarette formula and improving the cigarette flavor and taste.

Description

technical field [0001] The invention belongs to the technical field of detection of tobacco flavor components, and in particular relates to a method for analyzing and detecting basic flavor components in tobacco by direct solvent extraction gas chromatography mass spectrometry. Background technique [0002] Tobacco aroma components are one of the main factors affecting the quality of tobacco and cigarettes, and an important indicator for evaluating the sensory quality of tobacco products. Tobacco flavor components can be roughly divided into acidic flavor components, neutral flavor components, and basic flavor components. The basic aroma components in tobacco mainly include heterocyclic compounds such as pyridine, pyrazine, pyrrole, quinoline, etc., which are an important class of aroma substances in tobacco, although their content in tobacco is very small, but because of their strong The odor and lower threshold make them play an important role in enhancing the aroma chara...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N27/62
CPCG01N27/62G01N30/02G01N2030/025
Inventor 贾云祯聂聪王宜鹏孙学辉秦亚琼王晓瑜孙培健杨松刘惠民陈黎崔华鹏潘立宁
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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