Purification method of antioxidant rosmarinic acid for tobacco

A technology of rosmarinic acid and antioxidant, which is applied in the field of tobacco additives, can solve the problems of health threats to operators, large amount of organic solvents, and numerous elution steps, and reduce threats and pollution of the surrounding environment. The method is simple, The effect of eliminating hidden dangers in production safety

Active Publication Date: 2013-03-06
HUBEI CHINA TOBACCO IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that there are following three problems in the prior art: (1) the elution steps are numerous and complicated to operate; (2) the amount of organic solvent used is relatively large, which not only increases the cost, but also pollutes the environment; (3) organic reagents— - Use of petroleum ether
Therefore, during production, it will not only threaten the health of operators, but also pose a greater safety hazard.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Primary purification: using water as a solvent, extract perilla leaves by steam distillation to obtain extract A containing rosmarinic acid. First pass the extract A through a 30nm inorganic membrane, and then pass the obtained filtrate through an organic roll-type membrane with a molecular weight cut-off of 3000 to obtain filtrate B.

[0020] (2) Sample loading preparation: Concentrate the filtrate B through a reverse osmosis membrane to obtain a concentrated sample C.

[0021] (3), fine purification: the concentrated sample C is chromatographically separated with a gel column, and then eluted with deionized water of 1.2 times the column volume and 50% volume concentration ethanol of 1.2 times the column volume, and the rosemary is collected acid fraction.

[0022] (4), then use underpressure distillation in the prior art (temperature is 45 ℃) and ethanol recrystallization method (pH is 2.2; temperature is-5 ℃; time is 14 hours) to the rosmarinic acid flow that co...

Embodiment 2

[0024] (1) Primary purification: using 20% ​​ethanol as a solvent, extract perilla leaves by steam distillation to obtain extract A containing rosmarinic acid. First pass the extract A through a 30nm inorganic membrane, and then pass the obtained filtrate through an organic roll-type membrane with a molecular weight cut-off of 3000 to obtain filtrate B.

[0025] (2) Sample loading preparation: Concentrate the filtrate B through a reverse osmosis membrane to obtain a concentrated sample C.

[0026] (3), fine purification: the concentrated sample C is chromatographically separated with a gel column, and then eluted with deionized water of 2 times the column volume and 50% ethanol with a volume concentration of 2.5 times the column volume, and the rosemary is collected acid fraction.

[0027] (4), then use the underpressure distillation method (temperature is 35 ℃) and ethanol recrystallization method (pH is 1.8; temperature is 0 ℃; time is 18 hours) to the rosmarinic acid strea...

Embodiment 3

[0029] (1), primary purification: using water as a solvent, extract rosemary by steam distillation to obtain extract A containing rosmarinic acid. First pass the extract A through a 30nm inorganic membrane, and then pass the obtained filtrate through an organic roll-type membrane with a molecular weight cut-off of 3000 to obtain filtrate B.

[0030] (2) Sample loading preparation: Concentrate the filtrate B through a reverse osmosis membrane to obtain a concentrated sample C.

[0031] (3), fine purification: the concentrated sample C is chromatographically separated with a gel column, eluted with deionized water of 2.5 times the column volume and 50% ethanol with a volume concentration of 2 times the column volume successively, and rosemary is collected acid fraction.

[0032] (4), then use the underpressure distillation method (temperature is 48 ℃) and ethanol recrystallization method (pH is 2.5; temperature is 4 ℃; time is 22 hours) to the rosmarinic acid stream of collecti...

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Abstract

Belonging to the technical field of tobacco additives, the invention discloses a purification method of an antioxidant rosmarinic acid for tobacco. The purification method is carried out according to the steps of: (1) performing primary purification: first passing a rosmarinic acid-containing extraction solution A through a 30nm inorganic membrane, then passing it through an organic spiral-wound membrane with molecular weight cut-off of 3000, thus obtaining the filtrate B; (2) making sample loading preparation: subjecting the filtrate B to reverse osmosis membrane concentration to obtain a concentrated sample C; (3) conducting fine purification: carrying out chromatographic separation on the concentrated sample C by a gel column and collecting rosmarinic acid fraction; and (4) further concentrating and purifying the collected rosmarinic acid fraction by a pressure reduction distillation method and a recrystallization method in the prior art so as to make the rosmarinic acid content reach 80%-95%. The method provided in the invention is simple, safe, pollution-free, and is easy to implement.

Description

technical field [0001] The invention belongs to the technical field of cigarette additives, and specifically relates to a method for improving the existing rosmarinic acid purification by using membrane technology coupled with column separation technology. Background technique [0002] Rosmarinic acid is a polyphenolic compound with strong antioxidant activity existing in many plants, and its antioxidant activity is stronger than that of vitamin E. Adding rosmarinic acid to cigarettes can significantly reduce the content of free radicals in mainstream smoke and prevent cell damage caused by smoke free radicals in the human body, thereby reducing the risk of cancer and arteriosclerosis caused by smoking. The purity of rosmarinic acid extract directly affects the smoking quality of cigarettes. When the purity of the rosmarinic acid extract is low and contains more impurities, it will bring negative effects such as increased irritation to cigarettes and serious oral cavity res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/732C07C67/48
Inventor 王娟陈义坤郭国宁张华
Owner HUBEI CHINA TOBACCO IND
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