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Method for determining Cembrane diterpene alcoholate in tobacco and tobacco product by gas chromatography-mass spectrometry

A technology of Chinese cedarane diterpene alcohol and tobacco products, which is applied in the field of cetahane diterpene alcohol, can solve problems such as the difficulty of accurate quantitative analysis, the inability to achieve separation, and the difficulty in realizing accurate quantification of derivatization conditions, achieving high extraction efficiency , the effect of easy operation

Inactive Publication Date: 2011-06-22
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because if the derivatization treatment is not carried out in the gas phase and GC analysis, the separation of the two substances cannot be achieved. When the derivatization treatment is performed, the mastery of the derivatization conditions will make it difficult to achieve accurate quantification.
For liquid phase and liquid chromatography conditions, it is very difficult to achieve baseline separation and accurate quantitative analysis of these two substances due to the limitation of extraction solvent and injection solvent

Method used

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  • Method for determining Cembrane diterpene alcoholate in tobacco and tobacco product by gas chromatography-mass spectrometry
  • Method for determining Cembrane diterpene alcoholate in tobacco and tobacco product by gas chromatography-mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] a, take by weighing 0.2-0.5g of the tobacco sample of 40 mesh sieves in the glass flask, add the dichloromethane of 20-50ml (contain the content of the sucrose octaacetate of 16mg / ml n-heptadecanol and 6mg / ml Standard), at room temperature, ultrasonic extraction frequency of 50KHz and ultrasonic power of 350w ultrasonic 10min, after cooling to room temperature, with 5g of anhydrous sodium sulfate filter paper to filter out the smoke.

[0022] b. Concentrating the resulting filtrate to dryness at 10-13kpa. The residue was dilute to 5-10ml with chloroform. Take 1 ml and concentrate to dryness under the protection of inert gas. Add 500ul of 1:1 DMF:BSTFA and react at 60-80°C for 0.5-1.5 hours.

[0023] c. GC-MS analysis is performed on the obtained sample.

Embodiment 2

[0025] a, get two flue-cured tobacco green tobacco leaves, add 2000ml of 1,2-ethylene dichloride in a glass beaker of 5000ml, (containing 16mg / ml n-heptadecanol and 6mg / ml sucrose octaacetate), The tobacco leaves were dipped three times in the beaker for six seconds each time. After dipping, the solution was filtered with filter paper filled with 50 g of anhydrous sodium sulfate.

[0026] b. Concentrating the resulting filtrate to dryness at 10-13kpa. The residue was adjusted to 50ml with dichloromethane. Take 1 ml and concentrate to dryness under the protection of inert gas. Add 500ul of 1:1 DMSO:TMCS and react at 60-80°C for 0.5-1.5 hours.

[0027] c. GC-MS analysis is performed on the obtained sample.

Embodiment 3

[0029] a, get five oriental tobacco green tobacco leaves, add 500ml of chloroform (containing 16mg / ml n-heptadecanol and 6mg / ml sucrose octaacetate) in a 2000ml glass beaker, dip the tobacco leaves in the beaker Dip five times for three seconds each time. After dipping, the solution was filtered with filter paper containing 15 g of anhydrous sodium sulfate.

[0030] b. Concentrating the resulting filtrate to dryness at 10-13kpa. The residue was made up to 10ml with 1,2-dichloroethane. Take 1 ml and concentrate to dryness under the protection of inert gas. Add 500ul of 1:1 DMF:TMCS and react at 60-80°C for 0.5-1.5 hours.

[0031] c. GC-MS analysis is performed on the obtained sample.

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Abstract

The invention relates to a method of making use of gas chromatography-mass spectrometry for the measurement of cembrane diterpene alcohol in the tobacco and the tobacco products, which is characterized in that: the invention includes the following steps: a. firstly, a certain amount of tobacco products are taken, a certain amount of extraction solvent halohydrocarbon is added; after that, ultrasonic waves are used for vibration extraction of the diterpene alcohol; b. the extraction solvent is evaporated till the dryness under certain condition and another halohydrocarbon is added, appropriateamount is taken after the dissolution and volume control; c. the taken solvent is evaporated under certain condition, a certain volume of another solvent which is difficult to volatilize and the sameproportion of certain silicon derivatization reagent are added, so as to carry out the derivatization under the certain temperature condition. The cembrane diterpene alcohol in which can be measured directly by gas chromatography-mass spectrometry after the full derivatization. Compared with the prior art, the method of the invention can not only carry out the extraction analysis of cembrane diterpene alcohol of the tobacco and other complicated systems, but also has high extraction efficiency, simple and rapid operation.

Description

technical field [0001] The present invention relates to a method for measuring tobacco, in particular to a method for measuring cembradane diterpene alcohols in tobacco and tobacco products by gas chromatography-mass spectrometry. analysis to achieve rapid and accurate determination. Background technique [0002] The chemical constituents in tobacco are diverse and very complex. Cembradane diterpene alcohol is a widely distributed important chemical constituent in tobacco, and they are considered to be important precursors of aroma substances. However, due to the difficulty in the extraction and separation and purification of cembradin diterpene alcohols, they are considered to be one of the chemical components of tobacco that are difficult to accurately determine. At present, there are many analysis methods for tobacco cembradane diterpene alcohols, including gas chromatography, gas chromatography-mass chromatography, liquid chromatography-mass chromatography, and even thi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/78G01N30/88G01N27/62
Inventor 谢复炜刘克建丁丽赵乐
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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