Gallated Epicatechin Separation via Isonicotinic Acid Complex

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Solution Overview

Problem

Current methods for separating gallated epicatechins (EGCG & ECG) from green tea extract or green tea dust are not efficient in achieving high purity and yield, as they do not utilize isonicotinic acid to form a hydrated complex, which is essential for effective liberation and purification of these compounds.

Innovation Solution

The process involves forming a hydrated gallated epicatechins (EGCG & ECG)-isonicotinic acid complex using isonicotinic acid, followed by the use of water miscible and immiscible solvents, and treatment with a brine solution to remove insoluble materials, including steps like dissolving, concentrating, precipitating, filtering, slurrying, washing, extracting, and freeze drying to achieve high purity.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional separation methods are used for gallated epicatechins, then the process is simpler, but the purity and yield are insufficient

Engineering Contradiction:
Improvepurity of gallated epicatechinsVSAvoidcomplexity of separation process
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent introduces isonicotinic acid as an intermediary substance that forms a hydrated complex with gallated epicatechins. This complex acts as a mediator that enables selective precipitation and separation of EGCG and ECG from the green tea extract, achieving high purity (>97%) that conventional methods cannot attain. The intermediary compound facilitates the separation process by creating a distinct chemical form that can be selectively isolated.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent employs parameter changes by adjusting pH levels and using specific solvents (water-miscible and water-immiscible) to control the formation and dissolution of the hydrated complex. By changing the chemical environment parameters, the gallated epicatechins are transformed into a separable complex form, then recovered in high purity through controlled parameter adjustments during the separation process.

Inventive Principle:
Principle #35Parameter changes

2Productivity

If conventional separation methods are used, then the process is faster, but the yield of gallated epicatechins is low

Engineering Contradiction:
Improveyield of gallated epicatechinsVSAvoidtime for separation process
Core Design Contradiction:
ProductivityVSLoss of time

Solution Approach 1:

The patent applies preliminary action by first forming the hydrated complex with isonicotinic acid before performing the separation. This preliminary complexation step prepares the gallated epicatechins in a form that is optimized for subsequent separation and recovery, ensuring maximum yield. The preliminary formation of the complex prevents loss of target compounds during the separation process.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent uses extraction with water-immiscible solvents to take out the hydrated complex from the aqueous phase. This extraction step efficiently transfers the complex into the organic phase, separating it from impurities and enabling high-yield recovery of gallated epicatechins after solvent removal and decomposition of the complex.

Inventive Principle:
Principle #2Taking out (Extraction)

3Manufacturing precision

If isonicotinic acid complex formation is used, then purity is improved, but the process complexity increases

Engineering Contradiction:
Improvepurity of gallated epicatechinsVSAvoidease of separation process
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The patent introduces isonicotinic acid as an intermediary substance that forms a hydrated complex with gallated epicatechins. This complex acts as a mediator that enables selective precipitation and separation of EGCG and ECG from the green tea extract, achieving high purity (>97%) that conventional methods cannot attain. The intermediary compound facilitates the separation process by creating a distinct chemical form that can be selectively isolated.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent employs parameter changes by adjusting pH levels and using specific solvents (water-miscible and water-immiscible) to control the formation and dissolution of the hydrated complex. By changing the chemical environment parameters, the gallated epicatechins are transformed into a separable complex form, then recovered in high purity through controlled parameter adjustments during the separation process.

Inventive Principle:
Principle #35Parameter changes

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This method results in a high-yielding process that achieves >97% purity of gallated epicatechins, with >75% EGCG and >20% ECG, as confirmed by XRPD and HPLC analysis, providing a more effective separation and purification of these valuable compounds.

Implementation Method 1

forming a hydrated gallated epicatechins (EGCG & ECG)-isonicotinic acid complex using isonicotinic acid

Methodology Applied
Scientific EffectComplex formation: Chemical Bonding

Implementation Method 2

concentrating by centrifugation

Methodology Applied
Scientific EffectCentrifugal separation: Centrifugal Separation

Implementation Method 3

freeze drying to obtain >97% purity of gallated epicatechins

Methodology Applied
Scientific EffectFreeze drying: Freeze Drying

Data Source

PatentUS11420954B2Process for the separation of gallated epicatechins (EGCG and ECG) from green tea extract or green tea dust
Publication Date: 2022.08.23 CRYSTALMORPHIX TECH PVT LTD
  • US11420954B2 patent drawing
  • US11420954B2 patent drawing
  • US11420954B2 patent drawing

AI summary

The present invention relates to an improved process for the separation of gallated epicatechins (EGCG & ECG) from green tea extract or green tea dust. The present invention specifically relates to an improved process for the separation of gallated epicatechins (EGCG & ECG) from green tea extract or green tea dust by forming hydrated gallated epicatechins (EGCG & ECG)-isonicotinic acid complex using isonicotinic acid as acid, organic solvents for liberating gallated epicatechins. The present invention more specifically relates to the process for the separation of gallated epicatechins (EGCG & ECG) from green tea extract or green tea dust, wherein processes comprises steps of dissolving, concentrating by centrifugation, adding, precipitating, filtering, slurrying, removing supernatant liquid, washing, extracting and freeze drying. The present invention also relates to hydrated gallated epicatechins (EGCG & ECG)-isonicotinic acid complex.