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Method for analyzing and detecting alkaline aroma constituents in tobacco through ultrasound-assisted cloud-point extraction gas chromatography-mass spectrometry technology

A gas chromatography-mass spectrometry and alkaline aroma technology, which is applied in the field of tobacco aroma components detection, can solve the problems of no distillation of alkaline aroma components, high distillation temperature, low alkaline components, etc., and achieve accurate and reliable analysis results and pre-treatment conditions Gentle, gentle treatment conditions

Inactive Publication Date: 2016-01-13
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

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 aroma constituents in tobacco through ultrasound-assisted cloud-point extraction gas chromatography-mass spectrometry technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Accurately weigh 15g of tobacco dust sample, add 100mL of 10% sodium hydroxide solution, add 10μg of internal standard solution, soak for 15min, extract with power 40w ultrasonic for 60min, and centrifuge to obtain the supernatant. Add 10mL GenapolX-080 and stir evenly to form a 10% surfactant solution, heat to 55°C and keep this temperature for 20min. After static separation, the lower aqueous phase was discarded.

[0029] 2) Add 10mL of stripping solvent and conduct ultrasonic extraction for 10min. Centrifuge and separate the layers to take the upper layer back extraction solvent phase, add 2g of anhydrous sodium sulfate, shake and let stand for 2h. Concentrate to 1 mL, filter through a 0.45 micron filter membrane and add to a chromatographic vial to obtain the sample to be tested.

[0030] 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...

Embodiment 2

[0032] 1) Accurately weigh 25g of tobacco dust sample, add 200mL of 5% sodium hydroxide solution, add 10μg of internal standard solution, soak for 15min, extract with 60w ultrasonic power for 30min, and centrifuge to obtain the supernatant. Add 20mL TritonX-100 and stir evenly to form a 10% surfactant solution, heat to 85°C, and keep this temperature for 30min. After static separation, the lower aqueous phase was discarded.

[0033] 2) Add back extraction solvent 30mL, ultrasonic extraction for 10min. Centrifuge and separate the layers to take the upper layer back extraction solvent phase, add 3g of anhydrous sodium sulfate, shake and let stand for 2h. Concentrate to 1 mL, filter through a 0.45 micron filter membrane and add to a chromatographic vial to obtain the sample to be tested.

[0034] 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 basi...

Embodiment 3

[0036] 1) Accurately weigh 20g of tobacco dust sample, add 150mL of 20% sodium hydroxide solution, add 10μg of internal standard solution, soak for 15min, extract with 80w ultrasonic for 10min, and centrifuge to obtain the supernatant. Add 7.5mL PONPE10 and stir evenly to form a 5% solution, heat to 45°C higher than the cloud point temperature, and keep this temperature for 30min. After centrifugation, the lower aqueous phase was discarded.

[0037] 2) Add 50mL of stripping solvent and conduct ultrasonic extraction for 10min. Centrifuge and separate layers to take the upper layer back extraction solvent phase, add 5g of anhydrous sodium sulfate, shake and let stand for 2h. Concentrate to 1 mL, filter through a 0.45 micron filter membrane and add to a chromatographic vial to obtain the sample to be tested.

[0038] 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 ...

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Abstract

The invention discloses a method for analyzing and detecting alkaline aroma constituents in tobacco through an ultrasound-assisted cloud-point extraction gas chromatography-mass spectrometry technology. The method includes the steps that 1, a tobacco powder sample is accurately weighed, a sodium hydroxide solution and an internal standard solution are added, soaking and ultrasonic extraction are performed, centrifugation is performed to obtain supernate, a surfactant is added, the mixture is evenly stirred to form a 5%-15% solution, the 5%-15% solution is heated to a temperature higher than the cloud point temperature, and an aqueous phase is removed after standing layering or centrifugal layering; 2, reextraction solvent is added, ultrasonic extraction is performed, a reextraction solvent phase on the upper layer is taken, anhydrous sodium sulfate is added, the mixture is oscillated and then subjected to standing concentration, and the product is filtered through a filtration membrane to obtain a sample to be detected; 3, the sample is detected through a GC-MS, and graph spectrum data are processed to obtain an analysis and test result of the alkaline aroma constituents. The method has the advantages that the pretreatment process is simple, mild and fast, the alkaline aroma constituents in the tobacco can be accurately determined, and the method has great theoretical significance and application value for guiding a scientific formula of cigarettes and improving the aroma and taste quality of the cigarettes.

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 ultrasonic-assisted cloud point 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 enhancin...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 贾云祯聂聪王宜鹏孙学辉秦亚琼王晓瑜孙培健杨松陈黎崔华鹏潘立宁谢复炜
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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