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Extraction and column chromatography group composition separation method of tobacco lipoid

A separation method and a technology of family composition, which are applied in the field of tobacco chemistry, can solve the problems of inability to fully and correctly reflect the quality of tobacco leaves, many interferences in spectrum analysis, and complex injection components, so as to reduce the sensitivity of equipment, reduce pollution, and simplify the detection of components. the effect of

Inactive Publication Date: 2018-06-22
CHINA TOBACCO SHAANXI IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods generally have shortcomings such as complex injection components, large equipment pollution, and many interferences in spectral analysis, and cannot fully and correctly reflect the quality of tobacco leaves.

Method used

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  • Extraction and column chromatography group composition separation method of tobacco lipoid
  • Extraction and column chromatography group composition separation method of tobacco lipoid
  • Extraction and column chromatography group composition separation method of tobacco lipoid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Take the Shaanxi B3L tobacco sample as an example to describe in detail:

[0046] 1. Sample Extraction

[0047] Accurately weigh 6.0084g of crushed tobacco powder, pack it in 2 parts with dry filter paper extracted with chloroform (no smoke powder leaking out), add 300mL chromatographically pure chloroform into a 500mL flat-bottomed flask, and carry out Soxhlet extraction at 78°C for 24h (circulating cooling water at 8°C), concentrated to 10-15mL by a rotary evaporator, transferred to a 200mL beaker, dried in an oven at 40°C for 2 hours, and cooled to room temperature in a drying dish. Weigh to obtain 0.4791g extract, set aside.

[0048] 2. Asphaltene separation

[0049] Add 3 mL of dichloromethane to the extract in 1, heat and shake to dissolve completely. Then add 30mL of n-hexane, let it stand for 12h, transfer the supernatant to a 200mL beaker for use, then add 30mL of n-hexane to the extract and let it stand, take the supernatant and merge it into the first supern...

Embodiment 2

[0070] Take the Yunnan B3F tobacco leaf sample as an example to describe in detail:

[0071] 1. Sample Extraction

[0072] Accurately weigh the pulverized smoke powder 6.0073, pack it in 2 parts with dry filter paper extracted with chloroform (no smoke powder leaks out), add 300 mL of chromatographically pure chloroform into a 500 mL flat-bottomed flask, and carry out Soxhlet extraction at 75 °C for 24 hours ( circulating cooling water (8°C), concentrated to 10-15mL by a rotary evaporator, transferred to a 200mL beaker, dried in an oven at 40°C for 2 hours, and cooled to room temperature in a drying dish. Weigh to obtain 0.5121g extract, set aside.

[0073] 2. Asphaltene separation

[0074] Add 3 mL of dichloromethane to the extract in 1, heat and shake to dissolve completely. Then add 30mL of n-hexane, let it stand for 18h, transfer the supernatant to a 200mL beaker for use, then add 30mL of n-hexane to the extract and let it stand, take the supernatant and merge it into t...

Embodiment 3

[0082] Take the Hubei S6-H tobacco sample as an example to describe in detail:

[0083] 1. Sample Extraction

[0084] Accurately weigh 5.0002g of crushed tobacco powder, pack it in 2 parts with dry filter paper extracted with chloroform (no smoke powder leaking out), add 320mL chromatographically pure chloroform into a 500mL flat-bottomed flask, and carry out Soxhlet extraction at 70°C for 22 hours (circulating cooling water at 5°C), concentrated to 10-15mL by a rotary evaporator, transferred to a 200mL beaker, dried in an oven at 30°C for 4 hours, and cooled to room temperature in a drying dish. Weigh to obtain 0.4918g extract, set aside.

[0085] 2. Asphaltene separation

[0086] Add 2 mL of dichloromethane to the extract in 1, heat and shake to dissolve completely. Then add 25mL of n-hexane, let it stand for 4h, transfer the supernatant to a 200mL beaker, stand by, then add 25mL of n-hexane to the extract and let it stand, take the supernatant and merge it into the first...

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Abstract

The invention relates to an extraction and column chromatography group composition separation method of tobacco lipoid. Firstly, crushed tobacco powder is taken and subjected to Soxhlet extraction with chloroform, and an extracting solution is obtained; the extracting solution is concentrated and dried, and an extract is obtained; the extract is dissolved with dichloromethane, a mixed liquid is obtained, n-hexane is added to the mixed liquid, still standing is performed, and a liquid supernatant and insoluble asphaltene at the bottom are separated; the liquid supernatant passes through a wellfilled chromatographic column, washing is performed sequentially with n-hexane, dichloromethane and methanol, non-polar fractions, weak-polar fractions and strong-polar fractions are obtained respectively, and extraction and column chromatography group composition separation of the tobacco lipoid are completed. With the adoption of a column chromatography separation technology, the extract is divided into three fractions including non-polar fractions, weak-polar fractions and strong-polar fractions, so that detection ingredients are simplified, pollution of complicated samples to equipment isreduced, the defect that a lot of micro components in conventional analysis methods cannot be detected due to coverage by main components is overcome, and interference in spectrum interpretation is reduced.

Description

technical field [0001] The invention belongs to the technical field of tobacco chemistry, and in particular relates to a method for extracting tobacco lipids and separating components of column chromatography. Background technique [0002] Tobacco lipid is an important part of the surface substances of tobacco leaves, with complex chemical components, and the characteristic chemical components are closely related to the unique aroma and taste quality of tobacco. Therefore, research on the effective separation of characteristic chemical components in tobacco lipids is of great significance for tobacco leaf quality evaluation, formulation research, and process production. [0003] At present, the pretreatment methods for the analysis of tobacco lipids include: direct sampling of samples, direct sampling of extracts and other methods. These methods generally have disadvantages such as complex injection components, large equipment pollution, and many interferences in spectral a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/14
CPCG01N30/06G01N30/14
Inventor 王瑶彭军仓邓宝安康世平张萌萌张凤侠樊亚玲吕娟付瑜
Owner CHINA TOBACCO SHAANXI IND
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