Chios Mastic Terpene Fraction Purification via Chromatography

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Solution Overview

Problem

Existing methods for processing Chios mastic gum do not effectively isolate and purify terpene monomers and oligomers, as they often include detrimental poly-terpene polymers, which can hinder biological activities in cosmetic, nutraceutical, and pharmaceutical applications.

Innovation Solution

A reverse-phase chromatography process is used to extract and purify a fraction of terpene monomers and oligomers from Chios mastic gum, removing poly-terpene polymers with a degree of polymerization greater than 8, resulting in a composition with a purity higher than 98%, comprising hemiterpenes, monoterpenes, sesquiterpenes, and triterpenes.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If conventional extraction methods are used to obtain Chios mastic gum fractions, then the extraction process is simple, but the fraction contains poly-terpene polymers that reduce biological activity and therapeutic effectiveness

Engineering Contradiction:
Improveextraction process simplicityVSAvoidbiological activity effectiveness
Core Design Contradiction:
Ease of manufactureVSReliability

Solution Approach 1:

The patent applies segmentation by dividing the terpene fraction into distinct molecular weight components using size-exclusion chromatography. The process separates terpenes into monomers (molecular weight <500), oligomers (500-2000), and polymers (>2000), allowing selective isolation of biologically active lower molecular weight fractions while removing detrimental poly-terpene polymers. This segmentation resolves the contradiction by maintaining manufacturing feasibility through established chromatographic techniques while significantly improving biological activity through polymer removal.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The patent applies the extraction principle by specifically removing poly-terpene polymers from the crude terpene fraction using size-exclusion chromatography. The process extracts and isolates the beneficial monomeric and oligomeric terpenes while leaving the harmful high molecular weight polymers behind. This selective extraction resolves the contradiction by eliminating the source of reduced biological activity while preserving the therapeutic compounds.

Inventive Principle:
Principle #2Taking out (Extraction)

2Quantity of substance

If crude mastic gum extract is used directly, then the composition contains all natural components including terpenes, but the presence of poly-terpene polymers hinders biological activities

Engineering Contradiction:
Improvetotal terpene contentVSAvoidpolymer interference with biological activity
Core Design Contradiction:
Quantity of substanceVSObject-affected harmful factors

Solution Approach 1:

The patent applies the 'blessing in disguise' principle by converting the harmful effect of poly-terpene polymers into a beneficial separation process. Size-exclusion chromatography uses the size difference between polymers and monomers/oligomers to achieve separation, transforming what was previously a harmful contaminant into a separable component. The process converts the harmful polymer fraction into a removable byproduct while enriching the desired biologically active fraction, thus resolving the contradiction between maintaining total terpene content and eliminating harmful polymers.

Inventive Principle:
Principle #22Blessing in disguise (Convert harm into benefit)

Solution Approach 2:

The patent applies parameter changes by separating components based on molecular weight parameters. Using size-exclusion chromatography, the process exploits differences in hydrodynamic volume and molecular weight to separate terpenes into distinct fractions. This parameter-based separation allows retention of total terpene content while selectively removing the harmful high molecular weight polymer fraction, resolving the contradiction between quantity and quality of terpene components.

Inventive Principle:
Principle #35Parameter changes

3Manufacturing precision

If size-exclusion chromatography is used to separate terpenes by molecular weight, then polymer removal is effective, but the process complexity increases

Engineering Contradiction:
Improvepolymer removal efficiencyVSAvoidchromatography process complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent applies local quality by using different chromatography media for different separation needs. Size-exclusion chromatography media with specific pore sizes are selected to match the molecular weight range of target separation. This localized optimization of media properties enables effective polymer removal while maintaining process simplicity, resolving the contradiction between manufacturing precision and device complexity.

Inventive Principle:
Principle #3Local quality

Solution Approach 2:

The patent applies parameter changes by optimizing chromatography conditions including mobile phase composition, flow rate, and column dimensions to achieve effective separation with minimal process complexity. By adjusting these parameters, the process achieves high polymer removal efficiency using standard chromatographic equipment rather than complex specialized systems, resolving the contradiction between precision and complexity.

Inventive Principle:
Principle #35Parameter changes

4Reliability

If polymer-free terpene fraction is produced, then biological activity is enhanced, but the purification process time increases

Engineering Contradiction:
Improvetherapeutic effectivenessVSAvoidpurification process duration
Core Design Contradiction:
ReliabilityVSLoss of time

Solution Approach 1:

The patent applies preliminary action by performing size-exclusion chromatography separation early in the processing workflow, before subsequent formulation or application steps. This preliminary removal of polymers prevents downstream processing issues and eliminates the need for additional purification steps later, reducing total process time while ensuring therapeutic effectiveness. The separation is performed once at the beginning rather than requiring repeated treatments.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent applies continuity of useful action by using a continuous size-exclusion chromatography process that maintains constant separation efficiency throughout the purification. The continuous flow system ensures consistent polymer removal without interruptions or repeated batch processing, reducing overall purification time while maintaining high therapeutic effectiveness. The process operates continuously to separate and collect the active fraction in a single streamlined operation.

Inventive Principle:
Principle #20Continuity of useful action

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

The process efficiently isolates terpene monomers and oligomers, enhancing their biological activities and therapeutic effects, such as antimicrobial and anticancer properties, while eliminating the detrimental effects of poly-terpene polymers, resulting in a highly effective composition for various therapeutic applications.

Implementation Method 1

A reverse-phase chromatography process is used to extract and purify a fraction of terpene monomers and oligomers from Chios mastic gum, removing poly-terpene polymers

Methodology Applied
Scientific EffectChromatography: Chromatography

Implementation Method 2

A reverse-phase chromatography process is used to extract and purify a fraction of terpene monomers and oligomers from Chios mastic gum

Methodology Applied
Scientific EffectExtraction:

Data Source

PatentEP3363448A1Terpene enriched fractions free from polyterpenes extracted from chios mastic gum and cosmetic, nutraceutical, medical devices and pharmaceutical compositions containing them
Publication Date: 2018.08.22 PHYTOITAL SRL
  • EP3363448A1 patent drawingFigure 1
  • EP3363448A1 patent drawingFigure 2
  • EP3363448A1 patent drawingFigure 3

AI summary

The invention relates to isolated fractions of Chios mastic gum enriched in terpene monomers and oligomers and substantially free of poly-terpene polymers with a degree of polymerization greater than 8 and a molecular weight in the range from about 1,000 to about 100,000 as well as to a process for their preparation. The invention also relates to compositions comprising an isolated fraction of monomeric and oligomeric terpenes extracted and purified by reverse-phase chromatography and essentially free of polymers. The monomeric and oligomeric enriched terpenes fraction obtained from Chios mastic gum exhibits biological activities in cosmetic, nutraceutical, medical devices and pharmaceutical applications.