Technology for jointly extracting synephrine, hesperidin and PMFs (polymethoxy latednavones) from fructus aurantii immaturus

A technology of combined extraction and hesperidin, applied in the field of bioseparation engineering, can solve the problems of difficult separation and extraction, no simultaneous extraction and separation, waste of auxiliary materials and heat energy during separation and extraction, and achieve energy consumption reduction, heat energy reduction, and high-efficiency Good results

Active Publication Date: 2014-10-15
SICHUAN XINHUAKANG BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] However, there is no report on the simultaneous extraction and separation of three medicinal active ingredients in the above-mentioned open documents, which shows how difficult it is to separate and extract, and the separation and extraction process needs to waste a lot of auxiliary materials and heat energy

Method used

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  • Technology for jointly extracting synephrine, hesperidin and PMFs (polymethoxy latednavones) from fructus aurantii immaturus
  • Technology for jointly extracting synephrine, hesperidin and PMFs (polymethoxy latednavones) from fructus aurantii immaturus
  • Technology for jointly extracting synephrine, hesperidin and PMFs (polymethoxy latednavones) from fructus aurantii immaturus

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: The technology that extracts synephrine, hesperidin and PMFs jointly in the citrus aurantium described in the present embodiment is characterized in that comprising the following steps:

[0038] a. Extraction and separation of synephrine

[0039] (1) Sieve 10kg of Citrus aurantium to remove stones, iron nails and other sundries, wash away the sediment, air-dry until soaked, and crush. Equally distributed in two percolation tanks, coded as No. 1 and No. 2.

[0040] (2) First add 100L 0.08% dilute H to No. 1 tank 2 SO 4 The solution is soaked, stirred, and percolated, and the effluent is added to No. 2 tank for the same operation. Add 100L 0.08% dilute H to No. 1 tank 2 SO 4 solution, repeat once, and combine the leachate.

[0041] (3) Concentrate the leachate in (2) to 180L at a vacuum degree of 0.08Mpa and a temperature of 70°C for later use.

[0042] (4) Pretreatment of D001 macroporous resin: Soak 200g of resin in distilled water overnight, drain,...

Embodiment 2

[0053] a. Extraction and separation of synephrine

[0054] (1) Perform step a (1) in Example 1 with 100kg Citrus aurantium.

[0055] (2) First add 1000L 0.08% dilute HCl solution to No. 1 tank for soaking, stirring and diafiltration, then add the effluent to No. 2 tank for the same operation. Then add 1000L 0.08% dilute HCl solution to No. 1 tank, repeat once, and combine the leachate.

[0056] (3) Concentrate the leachate in (2) to 1600L at a vacuum degree of 0.08Mpa and a temperature of 65°C for later use.

[0057] (4) Pretreatment of D061 macroporous resin: Soak 2kg of resin in distilled water overnight, drain, wash with 3% HCl, distilled water, 3% NaOH, distilled water, 3% HCl, and distilled water until neutral, and wet-pack the column .

[0058](5) Pass the leachate in (2) through the chromatographic column to absorb synephrine for 8 hours, then wash with water until the effluent is neutral, desorb with 8% ammonia solution at a rate of 6L / h, and desorb until the efflue...

Embodiment 3

[0068] a. Extraction and separation of synephrine

[0069] (1) Perform step a (1) in Example 1 with 1000kg Citrus aurantium.

[0070] (2) First add 10000L 0.2% dilute HCl solution to No. 1 tank for soaking, stirring, and percolation, and then add the effluent to No. 2 tank for the same operation. Then add 10000L 0.2% dilute HCl solution to No. 1 tank, repeat once, and combine the leachate.

[0071] (3) Concentrate the leachate in (2) to 14,000L at a vacuum degree of 0.08Mpa and a temperature of 70°C for later use.

[0072] (4) Pretreatment of D152 macroporous resin: 20kg of resin was treated the same as step (4) of step a in Example 2.

[0073] (5) Pass the leachate in (2) through the chromatographic column to adsorb synephrine for 14 hours, then wash with water until the effluent is neutral, desorb with 10% ammonia solution at a rate of 6L / h, and desorb until the effluent is nearly free up to color. The desorption solution was concentrated at a vacuum degree of 0.085Mpa a...

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PUM

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Abstract

The invention relates to a technology for jointly extracting synephrine, hesperidin and PMFs (polymethoxy latednavones) from fructus aurantii immaturus. The technology comprises the following steps: a, smashing fructus aurantii immaturus, and subpackaging equal quantity of the smashed fructus aurantii immaturus in a percolation tank I and a percolation tank II respectively; adding a dilute acid solution in the percolation tank I, soaking, stirring and percolating; adding effluent liquid into the percolation tank II, soaking, stirring and percolating; mixing the leachate, performing vacuum concentration, adsorbing synephrine by a resin column, desorbing and collecting a desorption solution by using weak aqua ammonia, and performing vacuum drying to obtain dried synephrine; b, washing fructus aurantii immaturus dregs to be neutral with clear water, soaking with a dilute strong base solution, stirring, percolating, performing vacuum concentration, adding absolute methanol or absolute ethyl alcohol, performing still standing, filtering, performing vacuum concentration on the filtrate, and recycling alcohol to obtain a mother solution; c, adsorbing PMFs from the mother solution through the resin column and a chromatographic column, enabling methyl alcohol or ethyl alcohol to pass through the columns for desorbing under static pressure, collecting the stripping liquid, performing vacuum concentration, and recycling an eluent to obtain PMFs; acidizing the effluent liquid passing through resin, standing, and performing devitrification to obtain dried hesperidin.

Description

technical field [0001] The invention relates to a production process for jointly extracting synephrine, hesperidin and polymethoxyflavones (PMFs), in particular to a low-efficiency method for jointly extracting synephrine, hesperidin and PMFs from Citrus aurantium citrus A cost-efficient production process belongs to the field of biological separation engineering. Background technique [0002] Citrus aurantium is the dried young fruit of Rutaceae plant lime (Citrus aurantium L.) and its cultivars or sweet orange (Citrus sinensis Osbeck). Citrus aurantium, as a traditional Chinese medicine, is widely used in chest knots, gastroptosis, prolapse of the anus, and stagnation due to its warm nature, bitter taste, pungent, sour, spleen and stomach meridian, and the effect of dispelling qi and eliminating stagnation, resolving phlegm and dissipating swelling. Internal stagnation, fullness and pain, heavy diarrhea after diarrhea, obstructed stool, phlegm stagnation and qi obstructio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08C07C215/60C07C213/10C07D311/30C07D311/40
Inventor 夏雯徐培东蒋国彬陈华英
Owner SICHUAN XINHUAKANG BIO TECH
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