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Industrialized production method for synchronously producing stevioside, flavone and chlorogenic acid

A technology of steviol glycosides and production methods, applied in the field of natural product extraction, can solve the problems of stevia resource waste, unfavorable industrial production, flavonoid component loss, etc., and achieve the effect of improving comprehensive utilization value, low equipment requirements, and short process

Active Publication Date: 2015-10-28
CHENGUANG BIOTECH GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The molecules of stevia flavonoids mostly contain glycosyl fragments, which greatly increase their water solubility. During the extraction process of glycosides, about 80% of the flavonoids have been leached out together with the glycosides, and only a small amount of flavonoids remain in the liquid residue. A large amount of flavonoid components are lost, and re-extraction leads to increased energy consumption, which is not conducive to industrial production
In the article, the ultraviolet method is mostly used to detect the content of flavonoids at a wavelength of 358nm. The components such as chlorophyll and chlorogenic acid in the process of extracting leaf residues with ethanol are also proposed at the same time, and these components also have strong absorption at this wavelength, which has a relatively large impact on the detection results. big disturbance
[0004] Due to the lack of technology, stevioside manufacturers at home and abroad only use stevia as the raw material of stevioside, and there are no other by-products on the market, resulting in a great waste of stevia resources

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Weigh 100g of stevia leaves, add 15 times of water and extract under reflux at 100°C for 2.5 hours, filter to obtain the extract, repeat 3 times, combine the extract, add 1% flocculant ferrous sulfate under heat preservation conditions, and stir Add CaO to adjust the pH to 11.0, stand at 65°C for 60 minutes, and filter to obtain filter mud and filtrate. The filtrate is adsorbed by the macroporous adsorption resin ADS-4 at a flow rate of 1.5BV / h, analyzed with 50% ethanol aqueous solution, and passed through the desalination resin 001 ×6. After decolorization resin 330 is purified, a stevioside product is obtained with a glycoside content of 90%.

[0039](2) Extract the filter mud with a mixed solution of pH=5 ethanol and water with a volume ratio of 7:3 for 3 times, combine the extracts, and concentrate to a solid content of 45%;

[0040] (3) Dilute the concentrated solution with 5% ethanol aqueous solution to 1 / 5 of the original concentration, and apply macroporous...

Embodiment 2

[0045] (1) Weigh 500g of stevia leaves, add 10 times of water and ultrasonically extract at 50°C for 1 hour, filter to obtain the extract, repeat twice, combine the extract, add 0.8% flocculant ferrous sulfate under heat preservation conditions, and add Adjust the pH to 9.0 with CaO, let stand at 55°C for 45 minutes, and filter to obtain filter mud and filtrate. The filtrate is adsorbed by macroporous adsorption resin DM30 at a flow rate of 1.5BV / h, analyzed with 50% ethanol aqueous solution, and desalted resin 001×6, After the decolorization resin SQ338 is purified, a stevioside product is obtained with a glycoside content of 95%.

[0046] (2) Extract the filter mud with a mixed solution of pH=3.5 methanol and water with a volume ratio of 3:2 for 4 times, combine the extracts, and concentrate to a solid content of 35%;

[0047] (3) Dilute the concentrate with 5% methanol aqueous solution to 1 / 10 of the original concentration, and apply macroporous adsorption resin AB-8 at a f...

Embodiment 3

[0052] (1) Weigh 100g of stevia leaf, add 20 times of water and extract under microwave at 82°C for 3 hours, filter to obtain the extract, repeat 5 times, combine the extract, add 1.3% flocculant polyaluminium chloride and sulfurous acid under the condition of heat preservation Iron and other mass mixtures, add CaO to adjust the pH to 12.0 under stirring conditions, let stand at 75°C for 0 min, and filter directly to obtain filter mud and filtrate. The aqueous solution is analyzed and purified by desalting resin 001×8 and decolorizing resin 330 to obtain stevioside products with a glycoside content of 90%.

[0053] (2) The filter mud is extracted once with a mixed solution of equal volumes of ethanol and isopropanol at pH=0.1, and the extract is concentrated to a solid content of 100%;

[0054] (3) Dilute the concentrated solution with 10% ethanol aqueous solution to 1 / 2 of the original concentration, and apply macroporous adsorption resin LX-5 at a flow rate of 0.5BV / h;

[0...

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Abstract

The invention provides an industrialized production method for synchronously producing stevioside, flavone and chlorogenic acid. The method includes the following steps that step1, stevia rebaudiana leaves are weighed, extracted by adding water and filtered to obtain an extracting solution, flocculating agents are added under the condition of heat preservation, the pH is adjusted to 7-12, standing is performed for 0-120 minutes at the temperature of 30 DEG C-75 DEG C, then filtering is performed to obtain filter mud and filter liquid, and resin purification is performed on the filter liquid so as to obtain the stevioside product; step2, the filter mud is extracted through acid solvent, and extracting solutions are merged and concentrated; step3, solvent is added into a concentrated solution for dilution, and macroporous adsorption resin is added for adsorption; step4, gradient resolution is performed on the macroporous adsorption resin in the step3, a low-concentration resolution liquid is concentrated and dried to obtain the chlorogenic acid product, and high-concentration resolution liquid is concentrated to be standby; step5, after water is added into the high-concentration resolution liquid for dilution, organic solvent the same as the high-concentration resolution liquid in volume is used for extraction, and organic phases are merged, concentrated and dried to obtain the flavone product. By the adoption of the method, the stevioside, flavone and chlorogenic acid are extracted at the same time, the production cost is lowered, and the comprehensive utilization value of the stevioside is increased.

Description

technical field [0001] The invention belongs to the technical field of natural product extraction, and in particular relates to an industrialized production method for synchronously producing steviol glycosides, flavonoids and chlorogenic acid. Background technique [0002] Stevioside is a natural product of terpene glycosides. It is a low-calorie high-intensity sweetener extracted from the leaves of Stevia rebaudiana. Its sweetness is 150-300 times that of sucrose, but its calories are only 1 / 300 of sucrose. As people pay more and more attention to health issues, steviol glycosides have been widely used in food, beverage and daily chemical industries due to their advantages of low energy and high sweetness. the third largest sugar source. [0003] Stevia rebaudiana is a perennial herb of the Asteraceae Stevia family. It has been used as sweet tea and medicinal tea for more than 100 years in its birthplace. In addition to steviol glycosides, stevia also contains flavonoids...

Claims

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Application Information

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IPC IPC(8): C07H15/256C07H1/08C07D311/30C07D311/40C07C69/732C07C67/48
Inventor 徐美利牛志平田洪王立志李乾丽
Owner CHENGUANG BIOTECH GRP CO LTD
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