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Analytical method for quantitatively measuring super-multi-target aroma components in tobacco

A technology for the quantitative determination of aroma components, applied in the direction of analysis materials, measuring devices, material separation, etc., can solve the problems of limited quantity of trace aroma components in tobacco leaves, incomplete disclosure of the material basis of tobacco leaves, loss of low boiling point substances, etc., and achieve low cost and environmental protection. The effect of being friendly and using less solvent

Active Publication Date: 2019-09-06
ZHENGZHOU TOBACCO RES INST OF CNTC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Constrained by analytical method problems such as sample matrix interference and insufficient sensitivity of GC / MS, the number of trace aroma components in tobacco leaves covered by previous studies is extremely limited
For example, there are more than 500 types of trace tobacco / smoke components with unique flavor and low sensory threshold used in tobacco additives at home and abroad, but the previous research was limited to dozens of types by analysis technology, so the style and characteristics of tobacco leaves Incomplete disclosure of the material basis
Moreover, the current method does not use the standard curve to quantify, and does not involve the standard of the target object in the whole analysis process, but uses a semi-quantitative method, that is, the ratio of the peak area of ​​each compound to the peak area of ​​the internal standard that is qualitatively retrieved from the spectral library calculate
In addition, the extraction methods of aroma components in tobacco reported in the literature mainly include simultaneous distillation extraction, steam distillation, solid phase microextraction, purge and trap, supercritical extraction, headspace extraction, etc. The distillation extraction method is the most widely used in practice and has become the most commonly used extraction method for the analysis of tobacco aroma components, but it has problems such as serious loss of low boiling point substances, many by-products, low extraction efficiency, and long time consumption.

Method used

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  • Analytical method for quantitatively measuring super-multi-target aroma components in tobacco
  • Analytical method for quantitatively measuring super-multi-target aroma components in tobacco
  • Analytical method for quantitatively measuring super-multi-target aroma components in tobacco

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0047] The matrix effect of 345 kinds of aroma components (361 chromatographic peaks in total) was investigated by the following formula: ME=B / A, wherein, A is the slope of the solvent standard working solution standard curve, and B is the slope of the matrix matching standard working solution standard curve . The concentrations of the standard working solutions were 0.01, 0.02, 0.05, 0.1, 0.2, 0.5 and 1 μg / mL, respectively.

[0048] GC-MS / MS analysis conditions are as follows:

[0049] Gas chromatography conditions: Chromatographic column: elastic quartz capillary column, stationary phase is 50% phenyl-methylpolysiloxane, size 60m×0.25mm×0.25μm, pre-column connected in series at the inlet port (5m×0.25mm) ; Inlet temperature: 280°C; Injection volume: 0.8μL; Injection method: splitless injection, splitless time 1min; Carrier gas: Helium, constant flow mode, flow rate 1.5mL / min; The temperature is 75°C, kept for 5 minutes, then raised to 150°C at 1°C / min, kept for 1min, then ...

example 2

[0055] Weigh 2g of tobacco powder sample into a 50mL stoppered centrifuge tube, add 10mL of phosphate buffer to adjust the pH to 3, vortex to completely infiltrate the sample, let it stand for 20min; add 10mL of acetonitrile and 80μL of 30.0mg / L d 8 -Acetophenone internal standard working solution, vortex at 2500r / min for 2min, then put it into the refrigerator at -18℃ for 10min; take it out, add 4g of anhydrous magnesium sulfate, 1g of sodium chloride and shake vigorously quickly, then refrigerate at 2500r / min Vortex 2min at 8000r / min, centrifuge at 8000r / min for 3min; take 1mL of supernatant in a 2mL centrifuge tube, add 150mg of anhydrous magnesium sulfate and 10mg of multi-walled carbon nanotubes, vortex at 2500r / min for 2min, and centrifuge at 8000r / min 3min; the supernatant was filtered through a 0.22μm organic phase filter and analyzed by GC-MS / MS;

[0056] GC-MS / MS analysis conditions are as follows:

[0057] Gas chromatography conditions: Chromatographic column: elas...

example 3

[0072] Weigh 2g of tobacco powder sample into a 50mL stoppered centrifuge tube, add the standard solution to make the addition level of the target substance 0.5μg / g, add 10mL of phosphate buffer to adjust the pH value to 3, vortex to completely infiltrate the sample, and statically Set aside for 20min; add 10mL acetonitrile and 80μL 30.0mg / L d 8 -Acetophenone internal standard working solution, vortex at 2500r / min for 2min, then put it into the refrigerator at -18℃ for 10min; take it out, add 4g of anhydrous magnesium sulfate, 1g of sodium chloride and shake vigorously quickly, then refrigerate at 2500r / min Vortex 2min at 8000r / min, centrifuge at 8000r / min for 3min; take 1mL of supernatant in a 2mL centrifuge tube, add 150mg of anhydrous magnesium sulfate and 10mg of multi-walled carbon nanotubes, vortex at 2500r / min for 2min, and centrifuge at 8000r / min 3min; the supernatant was filtered through a 0.22 μm organic phase filter and then analyzed by GC-MS / MS; the conditions for ...

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Abstract

The invention, which belongs to the technical field of tobacco component detection, relates to an analytical method for quantitatively measuring super-multi-target aroma components in tobacco. The method comprises the following steps that: a tobacco sample is immersed in an acidic buffer solution and extraction is performed by an organic solvent; a multi-walled carbon nanotube is used as a reversesolid phase-dispersed adsorbent and vortexing and centrifugation are performed to purify the sample; and then simultaneous detection of 345 kinds of aroma component in tobacco is realized by combining gas chromatography-tandem mass spectrometry. The method has advantages of simple and rapid operation, high flux, low cost, low solvent dosage, good environmental friendly effect, wide range of analytical compounds, high accuracy, high precision, high sensitivity and high repeatability and can satisfy the demand of rapid detection and analysis of aroma component in tobacco.

Description

technical field [0001] The invention belongs to the technical field of detection of tobacco aroma components, in particular to a method for simultaneous determination of 345 aroma components in tobacco by immersion in acidic conditions, extraction with organic solvents, purification of multi-walled carbon nanotubes, and gas chromatography-tandem mass spectrometry (GC-MS / MS). Analytical method. Background technique [0002] Tobacco aroma components include aldehydes, ketones, alcohols, phenols, acids, ethers, esters, lactones, alkenes, pyridines, pyrroles, pyrazines and other types of volatile and semi-volatile components. The content level and mutual ratio of these components have a key impact on the style and quality of tobacco leaves and cigarettes, and are important chemical components that affect the aroma, quantity and flavor of tobacco. With the advancement of analytical techniques, the influence of aroma components on the sensory quality of tobacco leaves has receive...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/86G01N30/8658G01N2030/025G01N2030/062
Inventor 陈黎赵嘉幸任宗灿刘惠民谢复炜王晓瑜崔华鹏赵晓东樊美娟刘绍锋
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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