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Helichrysum italicum D.C. Essential Oil from Balkans

Contact Author Laure Saint-Lary, Francis Hadji Minaglou, Christian Escriva, Anne-Sophie Beyls, Frédéric Badie
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BY LAURE SAINT-LARYa, Francis Hadji Minagloub, Christian Escrivac, Anne-Sophie Beylsa, Frédéric Badiea

a Payan Bertrand, Grasse, France
b Botanicert, Grasse, France
c Le Gattilier, Valderoure, France

 

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Helichrysum italicum D.C. is becoming a well-known plant by consumers. The Corsican origin has been promoted for a few years now, particularly in the cosmetic world. Its Balkan origins is another quality to push its popularity forward in the industry. Payan Bertrand established a respectful and ethical supply chain with a local partner for the last eight years in Bosnia and Herzegovina, in which the essential oil quality differs from the popular Corsican variety. The goal of the following article is to present this specific quality based on a wide spectrum of scientific aspects. Chemical composition, aromatherapy activities and activities through olfaction were investigated. Perfumers, chemists and pharmacists/aromatherapists worked and discussed the properties of Helichrysum italicum D.C. essential oil. Different approaches were discussed to create an overview of this product, using an original method called a “sensorial approach” developed by one producer.

The name of this little gold flower Helichrysum italicum D.C. comes from ancient Greek “helios” for sun, “chrysos” for the color and “italicum” for Italy – the area where the plant was described for the first time. The plant is commonly known as the everlasting plant or curry plant in reference to exhibiting a similar odor as the spice. Its essential oil is traditionally recognized for its anti-inflammatory, cold, sleep-inducing and anti-microbial properties1. The odor is described as exhibiting terpenic, fruity, green and hay notes.

An overview of this plant’s complex market is difficult to represent as it is grown in different geographical origins around the Mediterranean Sea: Corsica in France, Italy, Bosnia and Herzegovina, Croatia, Macedonia – all containing different organoleptic qualities. Known for its high level of active compounds, Helichrysum is coveted, particularly in aromatherapy, cosmetics, fragrances and flavors: creating an exponential demand. An inescapable pressure on this wild resource in the last decade resulted in a shift from wild harvest to cultivation of Helichrysum.

Since 2010, Payan Bertrand has been partnering with a local distiller to sustainably obtain a supply of Helichrysum oil through its specific network of harvesters who are aware of its environmental issue. The last several years have shown a rising demand, price increase and thus the development of new opportunistic producers of this plant which led then to a drastic price decrease after 2017 (see F-1 and F-2). So, a regulation of the number of producers and market stabilization could be expected. Our partnership consists of protecting our supply chain at several levels: social, environmental and economical, for the interest of all the actors linked to this project.

Study

Samples

Essential oils were supplied by our partner in Bosnia and Herzegovina. Gas chromatography coupled with mass spectrometry (GC/MS) and gas chromatography equipped with a flame-ionization detector (GC-FID) analyses were performed on three samples (10% (w/w) in pure ethanol) representing three years of production: 2014, 2015 and 2016. Each sample is representing the average of approximately ten batches chosen for supply conformity to Payan Bertrand.

Gas chromatography coupled with olfactometry and mass spectrometer (GC-O/MS) study was performed on the 2016 sample (5% (w/w) in pure ethanol). Sensorial analysis and sensorial approach were also organized with the 2016 sample (pure).

GC/MS Analyses

The GC/MS analyses were carried out with an Agilent 7890A apparatusa coupled to an Agilent 5975C mass-selective detector (MSD) and equipped with a VF-1MS cap. columnb and with a VF-WAX-MS cap. column.c Injection of 1 μl was in split mode 200:1. The oven temp. was programmed isothermal at 60°C for 1 min, then rose from 60 to 250 °C at 10 °C/min, and finally held isothermal at 250 °C for 11 min; ion-source temp., 230 °C; transfer-line temp., 240 °C; carrier gas, He (0.8 ml/min); ionization energy, 70 eV; EI-MS spectra acquired over the mass range 40–400 amu.

The identification of the constituents was based on the comparison of its mass spectra with those of internal and commerciald mass-spectral libraries. Retention indices (RIs) were determined relative to the retention times of a series of n-alkanes (C7–C40).

GC-FID Analyses

The GC-FID analyses were carried out with an Agilent 7890 apparatus equipped with a flame-ionization detector (FID), an automatic liquid sampler, and the same VF-1MS cap. column and VF-WAX-MS cap. column described above. The oven temp. was programmed isothermal at 60°C for ١ min, then rose from 60 to 250 °C at 12 °C/min and then held isothermal at 250 °C for 9 min; injector temp., 250 °C; detector temp., 250 °C; carrier gas, H2 (1.0 ml/min); split ratio, 1:200; injection volume, 1 ml. The air and H2 flows of the FID were 350 and 35 ml/min., respectively.

Quantification was based on internal normalization, a method classically used by the perfume industry to evaluate essential oil quality.

DHS-TDU-PTV-GC-O/MS analyses

Analyses were carried out with an Agilent 7890B apparatus hyphenated to an Agilent 5977A mass-selective detector (MSD) and equipped with an olfactive port ODP 3 from Gerstel. HP-5MS Ultra Inert cap. columne was used. Sample extraction was done thanks to an automatic sampler MPS-2 from Gerstel with a Dynamic Headspace (DHS), a Thermal Desorption Unit (TDU) and a Programmed Temperature Vaporizer (PTV or called CIS by Gerstel).

The sample was incubated at 80 °C for 10 min. Then, headspace of the sample was purged with 400 ml of helium at 40 ml/min, and volatile components were trapped on a Tenaxf TA (Gerstel) adsorbent. The Tenax trap was then desorbed in TDUg in splitless mode. Components were cryofocalized during desorption at -10 °C, heated to 270 °C at 12 °C/s and held for 5 min at 270 °C in solvent vent mode to inject on the column. The oven temp. was programmed isothermal at 50 °C for 1 min, then rose from 50 to 250 °C at 8 °C/min, and finally held isothermal at 250 °C for 4 min; Carrier gas (He): 1.8 ml/min in cap.column and then flow was divided in 1.2 ml/min from splitter to ODP 3 and from splitter to MSD.

Eight trained panelists participated in the olfactometric experiment. They were asked to push a button when they perceived an odor stimulation and had to describe the perception in a microphone linked to Gerstel-olfactory recorder software. The frequency method was applied to treat results and only frequencies from 3/8 were considered significant in T-1.2

Sensorial Analyses

Perfumers Evaluation

Essential oil was evaluated by four perfumers and three trained panelists who were assigned to smell paper strips. For 15 minutes, each individual provided olfactive descriptors and followed by perceived emotions while smelling the product. Thus, top notes and heart notes were evaluated.

Sensorial Approach

This experiment worked with 35 participants from various professions (29 women and 6 men), individually or in small groups from a variety of adjacent professional backgrounds, most notably medical and unconventional therapy, biology and cosmetic science.

The study observed olfaction effects from the essential oil that was placed on a paper strip, as well as participants’ reported physical and mental levels. Participants did not know the name of the essential oil observed. Olfaction went from 30 minutes to two hours. Experimenters were all trained for this kind of exercise. Observations were written during or at the end of the olfaction. The various reported effects were those that were the most frequently quoted by the participants.

Results

Aromatherapy Properties Through Structure – Activity Relation

Helichrysum italicum D.C.essential oil is commonly described as an anti-inflammatory, analgesic, antibacterial, antistress, anti-depressant sedative and is used for the treatment of scars, liver, cough, colds, etc. and to regulate cholesterol. This oil is often called “the super arnica of aromatherapy.” Its properties are often cited from a general Helichrysum italicum D.C.without noting its geographical origins.3-9

Properties of essential oils are first explained by composition in our occidental scientific mind. This is logically the starting point of this study. In fragrances, we refer to odor families, which correspond to chemical groups. Regarding activities in cosmetics, pharmaceutics, etc., we refer to pharmacological activity, which are related to one or more chemical groups.

According to gas chromatography analysis, the compositions of three batches of essential oil from Payan Bertrand were studied (see T-1). In this study, 82% of the essential oil was identified. It was composed of 62.9% of terpenes, 10.6% of esters, 4.6% of ketones, 3.2% of terpenic alcohols, 0.9% of oxides and 0.1% of aldehydes.

Activity depends on the more abundant molecular groups, as well as the specific activities and concentrations of one or several main metabolites (see F-3).

To conclude, the use of this essential oil in aromatherapy would be for traumatic pain with or without oedema, articular or muscular inflammation, deep or superficial bruise, and after surgical operation.

The well-known Helichrysum italicum D.C. essential oil composition from Corsica in France was compared to the samples in this study. Corsica samples from local producers close to Calvi and Cargese (samples A, B and C from this reference) were studied.11 The compound’s concentrations are found in both origins (see T-2). Large amount of differences are noticed in the Balkans with alpha pinene (+ 102%), neryl acetate (- 91%), neryl propionate (- 86%), nerol oxide (- 86 %), nerol (- 76 %). The sum of the compounds listed in T-2 contain 74% for Corsica oil and only of 50 % for Balkans’ oil. Balkans’ essential oil is indeed characterized by other major compounds: 5.8% of beta selinene, 5.19% of beta caryophyllene, 3.49% of alpha cedrene and 2.53% of alpha selinene. Both essential oils then contain different compositions and thus different properties.

Comparative studies of the antitraumatic properties of different chemotypes of Helichrysum italicum ssp italicum are desirable, with production in many different countries.

With this article, we try to describe the properties of the essential oil from Balkans (Payan Bertrand quality) through different aspects, to be more comprehensive on this specific quality. Information about Helichrysum italicum ssp italicum from Corsica, France, can be found in the referenced study.12

New Aromatherapy Point of View Through Olfactometry Profile

Experimental data on psychopharmacological properties of essential oils are scarce; even if the study of one odorant compound seems to be easier, pharmacodynamics and pharmacokinetics phenomena for an essential oil or perfumed composition is difficult to apprehend.

In the following section, chemists and perfumers worked together to develop an olfactometry profile of the essential oil. Later, a pharmacist studied the collected data to find the aromatherapy profile linked to these odorant compounds.

Olfactometry profile

The olfactometry profile was obtained from eight panelists (F-4). Olfactive differences were calculated considering detection frequency values with their corresponding odor power. T-3 sums up the data with the participants’ confidence levels of identification and odor descriptions. Odor areas were classified in eight categories: terpenic, fruity, green, pyrazine, floral, spicy, animal and miscellaneous notes. Helichrysum italicum D.C. essential oil was mainly described as green, fruity and terpenic. Five odorant areas exhibited an intense odorant impact with a detection frequency from 6/8 to 8/8. The most intense characteristic was described as fruity, plum, lactone, peach, osmanthus, fruity damascenone, fruity apple, floral.

The first hypothesis of identification was done thanks to a retention index (RI) and odor description in which damascenone could be a good candidate. This potential compound would be at a very low level and probably coeluted which complicated mass spectrum extraction. The hypothesis was confirmed by another technique 2D-GC-GC (first dimension column was polar, and second dimension column was apolar); mass spectrum of damascenone was thus extracted. The second more odorant compound was linalool, exhibiting floral aqueous, floral, ozone, rose characteristics. Identification was complete with mass spectrum, retention index and odor similarity with databases. Three other areas had a significant odor impact with a detection frequency of 6/8. Nevertheless, identification levels were different. A correct hypothesis was achieved for alpha-terpineol with a retention index, mass spectrum and partial odor description of spicy, mushroom, fresh, aldehyde orange. Paracresyl acetate was identified according to the same level of confidence as damascenone in the first hypothesis. The zone was described as leather, styrax, fruity, dry, cresol, animal, ylang. Identification of the last zone with 6/8 frequency remained unknown, with green, floral aqueous, bourgeonal, greasy, milky, rose and floral characteristics.

Aromatherapy Through Olfaction

The chemical content of olfactive families were studied to discover their properties coupled to odors (see T-4). Different chemical groups are responsible for activities through olfaction in this essential oil: oxides, aldehydes and terpenes (green family); ketones (fruity family); terpenes (terpenic family); and alcohol (floral family). No specific activities were related to pyrazine, animal and spicy families.

According to this olfactometry profile, this essential oil would have properties to decrease stress, anxiety, fears with psychostimulant effect and attention preservation.

Both previous studies were considering the composition of the essential oil, which lets us correlate chemistry and aromatherapy. The last part focuses on the whole essential oil. Conventional sensory analysis was done with perfumers. Then, experiments according to the “sensorial approach” were conducted on Helichrysum italicum D.C. essential oil from Balkans by its author C. Escriva13.

From Perfumes to the Sensorial Approach

Perfumers' Point of View

Top notes and heart notes are described in T-5. Heart notes were qualified 15 min after the first smell for top notes. The terpenic aspect decreased as well as liquorice and freshness. Dry aspect was then reinforced.

To move on to the sensorial approach explained in the next part, perfumers tried to express their feelings (physical and psychological) about this essential oil during olfaction. Seven reported feelings/activity on the spirit or body that developed from this experiment: activity in respiratory tract, muscular pain, well-being/relaxation but also a comforting feeling with solid bases, heat sensation, connection with nature, and finally some negative emotions for two people among the six panelists. This approach was more deeply investigated in the following part with a panel well experienced to this kind of exercise, requiring people able to listen to their deeper instinct.

Reports from the Sensorial Approach

The sensorial approach can be qualified as “phenomenological” and asks many epistemological issues, the major one being: what do we project from our personalities? A discussion with this delicate question would be out of the scope of this article. However, the general intention was to add another dimension of understanding to the essential oil beyond olfactive descriptions.

Experimenters perceived a soft light, pastel and austere, a link with an aerial principle; a relation with a water element and with heat. This odor did not provoke rich metaphors or vivid imagery.

Effects on circulatory venous or arterial toning were perceived with more or less intensity according to subjects. Brain micro-circulation was activated (hyperacousia: increasing of auditory acuteness, as well as an increase of visual acuteness). Some subjects experienced headaches in forehead-temporal (classical symptoms for ketones). Heart tropism of this essential oil was important, where subjects expressed painful compression or a heat sensation, a stimulation and a rhythm regulation (acceleration or slowing down).

Affinity with skin is strong. Regenerating, nourishing and protection effects are sensed and seemed to affect different cutaneous stratums.

Upper and lower gastrointestinal tracks were stimulated with a warming sensation. The effect on hepatobiliary (liver) sphere was well noticed and subjects expressed feelings of nausea. Subjects expressed the diaphragm to be relaxed and breath was amplified. Mucolytic and anti-inflammatory effects (otitis for example) were strong. Peculiar sensations on surgical operation zones, even old, were observed (tonsils removal, for example).

Long olfaction of this essential oil regulated neurovegetative system and experienced slight effects which consisted in a relaxation state (muscular, diaphragm, articular), a narcohypnia (heavy body sensation), a sensation of comfort and finally a feeling of stimulation.

During this kind of olfaction, a particular state of concentration was experimented. However, this state was not as important as an interior elevation of the spirit. Pains on body parts subjected to trauma, even very old, can be awakened.

Memories of some traumatic situations can return. An inner work is done on these painful parts of ourselves: some anger, some injuries, difficult situations, memory on menstruation pain, etc. The emergence of these memories is not violent, or cathartic, but rather calms the subject’s emotional sphere.

Discussion and Conclusion

The structure-activity relation in regards to studying aromatherapy is the most common approach and accepted by chemists and pharmacists educated in our occidental schools and universities.

Aromatherapy by olfactive study appeals to complex phenomena and requires an understanding of the level of each compound that reaches the olfactive epithelium of the panelist. As a reminder, one compound in low quantity in an essential oil can have a powerful odor. In this way, damascenone was described for the first time in Helichrysum italicum essential oil to our knowledge. Inversely, major compounds are not necessarily the most active odorants. It seems then to be obvious, that activity through olfaction can be different than the one studied thanks to the structure-activity relation (considering the concentration levels in essential oil). This second approach can be used as a new tool for perfumers to offer “active odorant composition.” Aromatherapy and fragrances can then be deeply linked.

Complementarity between both approaches is observed with different activities (F-5): traumatic pain, muscular and articular inflammation are observed in the classical way; and decreasing stress and stimulant are observed by olfaction.

The sensorial approach experimented by C. Escriva is shedding new light on studying perfumery and aromatherapy. Concordance with elements from the first two studies related to chemical composition was highlighted, which was also in agreeance with the third study by perfumers who are inexperienced with this kind of sensorial exercise. A blind study (no knowledge of essential oil type) is preferred in order to avoid influencing people during the study. Despite being unconventional to new non-scientifically explained domains, this methodology seems well accepted by people coming from diverse backgrounds outside of the scientific arena. This approach needs training, concentration and an openness to a spiritual mindset, like meditation. This comparative work would deserve to be repeated on other essential oils.

Acknowledgments

The panel of 35 experimenters working with Christian Escriva for many years are kindly thanked for their willingness and enthusiastic involvement in this study!

We thank Research Institute for Chromatography (Belgium) and Christophe Devos for their participation to confirm elucidation of the damascenone compound.

The Elmar and Mariç family are thanked for their deep collaboration on fields and technical aspects.

Sophie Trestour and Geoffrey Balme are thanked for their help in the final stages!

 

Caption:

The sensitive approach takes a phenomenological approach to olfactive description where the oil’s perceived effects on consciousness and the subject’s experience are taken into account.

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References

References

  1. Separation of phytochemicals from Helichrysum italicum: an analysis of different isolation techniques and biological activity of prepared extracts, S. Maksimovic, V. Tadic, D. Skala, I. Zizovic, Phytochemistry, 138, 2017, 9-28
  2. Methods for gas chromatography-olfactometry: a review, S.M van Ruth, Biomolecular Engineering, 17, 2001, 121-128
  3. Les huiles essentielles, Vertus et applications, X. Fernandez, F. Chemat, TKT. Do, Vuibert, Paris, 2012
  4. The aromatherapy encyclopedia, a concise guide to over 385 plant oils, C. Schiller, D. Schiller, Basic Health Publications, Laguna Beach, CA, 2013
  5. La bible Larousse des huiles essentielles, T. Folliard, Larousse, Paris, 2016
  6. Ma bible des huiles essentielles, guide complet d’aromathérapie, D. Festy, Leduc S, Paris, 2008
  7. Essential oils, a handbook for aromatherapy practices, J. Peace Rhind, 2nd Ed, Singing Dragon, 2012
  8. Medical aromatherapy, healing with essential oils, K. Schnaubelt, North Atlantic Books, 1999
  9. The essential oils, complete reference guide, KG Stiles, Page Street Publishing, 2017
  10. Huile essentielle d’Hélichryse, A. Lobstein, F. Couic Marinier, Actualités Pharmaceutiques 56(567) : 51-54 · June 2017
  11. Composition of Helichrysum italicum (Roth) G. Don fil. Subsp. Italicum essential oils from Corsica, A. Bianchini, P. Tomi, J. Costa, A. F. Bernardini, Flavour and Fragrance Journal, 16, 2001, 30-34
  12. Les Huiles Essentielles Corses, Les Plantes aromatiques Corses et leurs propriétés thérapeutiques, C. Escriva, Amyris, Bruxelles, 2012
  13. Les Alcoolatures, une nouvelle approche des Teintures mères, C. Escriva, Amyris, Bruxelles, 2015

Footnotes

 Author Footnotes:

a Payan Bertrand, Grasse, France
b Botanicert, Grasse, France
c Le Gattilier, Valderoure, France

Footnotes:

Agilent Technologies

100% dimethylpolysiloxane, 20 m x 0.15 mm i.d., film thickness 0.15 μm; Agilent Technologies

100% polyethylene glycol, 20 m x 0.15 mm i.d., film thickness 0.15 μm; Agilent Technologies

NIST 2014

5% phenyl)-methylpolysiloxane, 30 m x 0.25 mm i.d., film thickness 0.25 μm; Agilent Technologies

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