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Detecting Essential Oil Adulteration

  • Young Living Essential Oils
Volume 2 • Issue 2 • 1000132
J Environ Anal Chem
ISSN: JREAC, an open access journal
Environmental Analytical Chemistry
Boren et al., J Environ Anal Chem 2015, 2:2
Review Article Open Access
Detecting Essential Oil Adulteration
Boren KE, Young DG, Woolley CL, Smith BL, Carlson RE
Young Living Essential Oils, 3125 Executive Parkway, Lehi, UT 84043, USA
*Corresponding author: Carlson RE, Young Living Essential Oils, 3125
Executive Parkway, Lehi, UT 84043, USA, Tel: 801-418-8900; E-mail:
Received September 09, 2014; Accepted February 13, 2015; Published February
16, 2015
Citation: Boren KE, Young DG, Woolley CL, Smith BL, Carlson RE (2015) Detecting
Essential Oil Adulteration. J Environ Anal Chem 2: 132. doi:10.4172jreac.1000132
Copyright: © 2015 Boren KE, et al. This is an open-access article distributed under
the terms of the Creative Commons Attribution License, which permits unrestricted
use, distribution, and reproduction in any medium, provided the original author and
source are credited.
Nearly two millennia ago, Pliny the Elder wrote, “It is the natural
propensity of man to falsify and corrupt everything.” His words referred
to such practices as the then-common adulteration of wine with gypsum,
pitch, lime, rosin, wood ashes, salt, sulphur, articial pigments, etc [1].
While wine fraud is still with us, the more common food adulteration is
the topic of over 60,000 studies on PubMed, where this contamination
is termed Economically Motivated Adulteration (EMA) [2].
Riding a popular natural health trend, the aromatherapy market in
the United States enjoyed retail sales of nearly $32 million in 2012, a
17.7% increase over 2011 totals [3]. e United States is home to a large
direct-sale essential oil industry as well. More impressive gains were
posted for world trade in essential oils: sales rose from just over U.S.
$706 million in 1990 to slightly over U.S. $1.7 billion in 2005 [4].
Unfortunately, this burgeoning market has encouraged the
adulteration of essential oils. A brief Medline search revealed 30 studies
dealing with this topic. A study conducted at the University of Messina in
Italy reports that “Unscrupulous producers have begun to fraudulently
increase prots while keeping down raw material costs mainly through
the addition of cheaper oils or oil constituents” [5]. While Pliny was
undoubtedly at the forefront of rst-century chemistry, his simple
balsam purity test—“Moreover a drop of pure balsam thickens in warm
water, settling to the bottom of the vessel, whereas when adulterated it
oats on the top like oil” [6], would hardly pass muster today.
Some oil adulterations are easily red-agged with routine testing;
e.g., adulterated cinnamon bark (Cinnamomum verum) essential oil
that has been diluted with cheaper cinnamon leaf oil can be detected
because leaf oil has a higher content of eugenol, which is handily
ascertained with GC analysis. Other adulterations require more
advanced technology. A 1997 study in the Journal of Essential Oil
Research states that “as the latest progress in origin specic analysis of
essential oils and avors, an integral authenticity evaluation, including
isotopic data, enantiomeric distributions, as well as quantication of
compounds analyzed, has been established” [7].
However, a worldwide consensus for essential oil constituent
standards has not yet been established. e International Organization
for Standardization (ISO) and Association Française de Normalisation
(AFNOR) have set constituent levels for certain essential oils. However,
hundreds of oils lack international standards, creating uncertainty.
International standards are critical for essential oil trade and commerce.
An upsurge in worldwide essential oil sales seems to have intensied corrupt practices by unscrupulous cost-
cutters and adulterators with varying levels of expertise. From outright misrepresentation of botanical species to the
addition of cheaper oils to create additional prot for the oil producer, adulteration is unfortunately a common place
occurrence in essential oil trade.
The most adulterated essential oils fall into two categories: high-value oils like sandalwood and rose and the best-
selling oils such as lavender, peppermint, citrus oils, wintergreen, oregano, and thyme. While some adulterations can
be detected simply by routine GC-MS testing, with technology such as GC-IRMS and SNIF-NMR, analysts are able to
spot adulteration with synthetic compounds or the natural compounds and/or oil fractions taken from cheaper essential
oils. Today’s cutting-edge technology for essential oil adulteration detection encompasses many analytical techniques
from HPLC and fast GC to GC × GC, IRMS to MS, 1H, and 13C NMR.
This paper is a review of 30 studies dating up to May 2014 that detail the analytical procedures used to uncover
essential oil adulteration in order to ensure that essential oils are authentic and genuine.
Meeting Essential Oil Standards
For the oils that do have ISO standards, natural variations resulting
from climate, geography, and altitude must be considered.
Peppermint (Mentha piperita) oil is the perfect example. e
U.S. produces nearly 80% of global peppermint essential oil, most of
which is grown specically for avoring gum, candy, food, toothpaste,
mouthwash, pharmaceuticals, and confectionaries. It is estimated that
less than 1% of the U.S.-grown peppermint essential oil is available to
the aromatherapy/alternative health care industry. is makes India the
largest supplier of peppermint essential oil for aromatherapy markets
and introduces geographically unique oil when analyzing for possible
adulteration. Because of geographical dierences, ISO standards are
dierent for U.S.-grown peppermint and the peppermint grown in
India also produces cornmint (Mentha arvensis), a less-expensive
mint plant that is frequently used as a peppermint adulterant. is
can be avoided by carefully considering analytical analyses. Cornmint
is higher in menthol, while peppermint contains unique marker
compounds that identify it as genuine. Menthofuran is found in
peppermint in levels from 0.4 to 14.6%, while this compound is either
not detected or is detected only in levels up to 0.01% in cornmint. e
biomarker viridioral is found in peppermint up to 0.9%, while it is not
detected in cornmint.
Enantiomeric Analyses
Mosandl reports that “the systematic evaluation of natural
enantiomeric ratios has been proven to be a valuable criterion for
Volume 2 • Issue 2 • 1000132
J Environ Anal Chem
ISSN: JREAC, an open access journal
Citation: Boren KE, Young DG, Woolley CL, Smith BL, Carlson RE (2015) Detecting Essential Oil Adulteration. J Environ Anal Chem 2: 132.
Page 2 of 3
dierentiating natural compounds from those of synthetic origin
and that “under good manufacturing practice (GMP) the chirality
evaluation of linalool has been proven to be a reliable indicator in the
authenticity assessment of bergamot, sweet orange, or lavender oils”
[8]. Chanotiya et al. employed enantiomeric composition studies as
indicators of origin authenticity and quality of essential oils of Indian
origin: Citrus sinensis, basil, bergamot, rose, geranium, Lippia alba,
Zingiber roseum, lemongrass, and oregano [9].
Researchers at Service Central d’Analyse in France tested for
adulteration in the essential oils of lemon, lemongrass, citronella,
Litsea cubeba, Lippia citriodora, and lemon balm (Melissa ocinalis).
ey report: “Our results indicate the utility of combined chiral and
isotope analysis and use of the statistical method PCA for analysis of
composition for detecting the adulteration and for determining the
botanic origin of essential oils” [10].
Orthogonal Methodology
Swiss researchers note in a May 2014 study, “Since a control of
authenticity by standard analytical techniques can be bypassed using
elaborated adulterated oils to pretend a higher quality, a combination
of advanced orthogonal methods has been developed” [11]. One such
method was employed by French researchers using 2H-ERETIC-NMR
technology on 19 samples of methyl salicylate (natural/synthetic and
commercial/extracted). ey found that deuterium site-specic natural
isotope abundance “allows discrimination between synthetic and
natural samples. [12] Wintergreen remains one of the most commonly
adulterated essential oils, with the ease of synthetic methyl salicylate
substitution or dilution. In fact, synthetic methyl salicylate is also
known as “oil of wintergreen.
Cold-pressed citrus oils are found in multiple products relating
to human health. Because of their high cost, synthetic chemicals and
cheaper essential oils are common adulterants.
An Italian study using fast-GC/MS and HPLC analysis shows that
a lemon essential oil was found to contain herniarin, isopimpinellin,
and 5-heranyloxy-8-methoxypsoralen, normally present only in lime
oil. is study concludes, “e experimental results shown in this
study demonstrate that fast-GC/MS and HPLC remain one of the most
eective means to detect these illegal modications” [13]. HPLC and
GCxGC were the technologies used to determine genuineness of two
citrus oils, bergamot and sweet orange, in a recent Italian study [14].
A study conducted at Shiraz University of Medical Sciences in Iran
reports that many of 19 tested samples of rose water did not contain
rose essential oil but instead had the cheaper essential oil of palmarosa
(Cymbopogon martinii), as determined by unusual δ (13)C values using
GC/IRMS analysis. It states, “e increase in market demand has led
to production of inferior products for hydrosol that contain synthetic
essences or essential oils of other plants. Dibutyl phthalate was also
detected in most samples” [15]. e latter plasticizing chemical is
known as a reproductive and developmental toxicant and endocrine
Hervé Casabianca on yme Adulteration
In a communication [16] from Hervé Casabianca, French expert
in natural product analysis, he reiterates that using classical analysis,
a person is not able to dierentiate a natural from a synthetic avoring
molecule. He explained that by using IRMS, we can easily compare
natural versus synthetic thymol because natural thymol must be
deuterium depleted and 18O enriched. Casabianca’s research using
deuterium/hydrogen ratio analysis of the essential oil constituent’s
thymol, carvacrol, gamma-terpinene, and p-cymene is published in the
Journal of Chromatography A [17].
Rose and Sandalwood Adulteration
We close with research on adulteration of high-value essential oils.
Rose oil (Rosa damascena) sells for as much as U.S. $240 for a
5-milliliter bottle. It is, therefore, no surprise that university scientists
from Italy used GC/C/IRMS in combination with GC/MS and GC/FID
analysis on 19 commercial samples and found unusual δ (13)C values
in most of the oils, indicating that a natural, cheaper palmarosa oil
(Cymbopogon martinii) had been added [18].
Vankar reports the rose oil adulterator “now has to his disposal a
number of natural isolates of lower-priced oils. e most important of
these are geraniol and rhodinol (l-citronellol). If added in moderate
quantities, these compounds cannot be detected in rose oil by mere
routine analysis” [19]. Chanotiya, as previously mentioned, used
enantioselective capillary gas chromatograph-ame ionization and
mass spectrometry to determine the authenticity and quality of Indian
essential oils, including rose [20]. Moein notes Iranian rose water
samples were adulterated with less expensive essential oils (Pelargonium
and Dianthus) and synthetic essences [21].
Because of shortages related to sustainability issues, sandalwood
is an attractive target for adulteration. Distilled from the heartwood
of the tree, sandalwood essential oil international standards require
90% total santalol content. Testing in 2004 revealed all tested samples
failed to comply with the santalol content requirement, and only
about half of the samples met the ISO standard [22]. Kuriakose et al.
suggests that “NIR spectroscopy with chemometric techniques could
be successfully used as a rapid, simple, instant and non-destructive
method for the detection of adulterants, even 1% of the low-grade oils,
in the high quality form of sandalwood oil” [23].Updating the previous
2010 research in November 2013, Kuriakose et al. focused on “the
application of near infrared spectroscopy to detect sample authenticity
and quantify economic adulteration of sandalwood oils. Several pre-
treatments are investigated for calibration and prediction using partial
square regression (PLSR)” [24].
In summation, illegal essential oil adulteration and contamination
scandals now require sophisticated and highly technical methods to
authenticate the oils. Analytical chemistry must be employed in all its
forms to thwart the escalating, economic adulteration of these valued
therapeutic agents.
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among the Ancients. Science 29: 455-458.
2. Everstine K, Spink J, Kennedy S (2013) Economically motivated adulteration
(EMA) of food: common characteristics of EMA incidents. J Food Prot 76: 723-
3. US Trends in Aromatherapy Essential Oil Choices, Dorene Petersen, American
College of Healthcare Choices.
4. Trade Information Brief Essential Oils. Accessed August 19, 2014.
5. Costa R, Dugo P, Dugo G, Mondello L (2015) GC and HPLC Detection of
Adulterations in Citrus Oils. J Sep Sci Featured Article accessed 8: 6-14.
6. Pliny (circa AD 23-79), Loeb Classical Library, Natural History, Books 12-16,
7. Mosandl A, Juchelka D (1997) Advances in the Authenticity Assessment of
Citrus Oils. J Ess Oil Res 9: 5-12.
Volume 2 • Issue 2 • 1000132
J Environ Anal Chem
ISSN: JREAC, an open access journal
Citation: Boren KE, Young DG, Woolley CL, Smith BL, Carlson RE (2015) Detecting Essential Oil Adulteration. J Environ Anal Chem 2: 132.
Page 3 of 3
8. Mosandl A (2004) Authenticity assessment: a permanent challenge in food
avor and essential oil analysis. J Chromatogr Sci 42: 440-449.
9. Chanotiya CS, Yadav A (2009) Enantiomeric composition of (3R)-(-)- and (3S)-
(+)-linalool in various essential oils of Indian origin by enantioselective capillary
gas chromatography-ame ionization and mass spectrometry detection
methods. Nat Prod Commun 4: 563-566.
10. Nhu-Trang TT, Casabianca H, Grenier-Loustalot MF (2006) Authenticity control
of essential oils containing citronellal and citral by chiral and stable-isotope gas-
chromatographic analysis. Anal Bioanal Chem 386: 2141-2152.
11. Marti G, Boccard J, Mehl F, Debrus B, Marcourt L, et al. (2014) Comprehensive
proling and marker identication in non-volatile citrus oil residues by mass
spectrometry and nuclear magnetic resonance. Food Chem 150: 235-245.
12. Le Grand F, George G, Akoka S (2005) Natural abundance 2H-ERETIC-NMR
authentication of the origin of methyl salicylate. J Agric Food Chem 53: 5125-
13. Costa R, op. cit.
14. Tranchida PQ, Zoccali M, Bonaccorsi I, Dugo P, Mondello L, et al. (2013)
The off-line combination of high performance liquid chromatography and
comprehensive two-dimensional gas chromatography-mass spectrometry: a
powerful approach for highly detailed essential oil analysis. J Chromatogr A
1305: 276-284.
15. Moein M, Zarshenas MM, Delnavaz S (2014) Chemical composition analysis of
rose water samples from Iran. Pharm Biol 52: 1358-1361.
16. Personal communication from Hervé Casabiana to Richard Carlson, June 11,
17. Nhu-Trang TT, Casabianca H, Grenier-Loustalot MF (2006) Deuterium/
hydrogen ratio analysis of thymol, carvacrol, gamma-terpinene and p-cymene
in thyme, savory and oregano essential oils by gas chromatography-pyrolysis-
isotope ratio mass spectrometry. J Chromatog A 1132: 219-27.
18. Pellati F, Orlandini G, van Leeuwen KA, Anesin G, Bertelli D, et al. (2013) Gas
chromatography combined with mass spectrometry, ame ionization detection
and elemental analyzer/isotope ratio mass spectrometry for characterization
and detecting the authenticity of commercial essential oils of Rosa damascena
Mill 27: 591-602.
19. Vankar PS (2003) Adulteration in Rose Oil. Natural Product Radiance 2: 180-
20. Chanotiya CS, op. cit.
21. Moein M, op. cit.
22. Howes MJ, Simmonds MS, Kite GC (2004) Evaluation of the quality of
sandalwood essential oils by gas chromatography-mass spectrometry. J
Chromatogr A 1028: 307-312.
23. Kuriakose S, Thankappan X, Joe H, Venkataraman V (2010) Detection
and quantication of adulteration in sandalwood oil through near infrared
spectroscopy. Analyst 135: 2676-2681.
24. Kuriakose S, Joe IH (2013) Feasibility of using near infrared spectroscopy to
detect and quantify an adulterant in high quality sandalwood oil. Spectrochim
Acta A Mol Biomol Spectrosc 115: 568-573.
Citation: Boren KE, Young DG, Woolley CL, Smith BL, Carlson RE
(2015) Detecting Essential Oil Adulteration. J Environ Anal Chem 2: 132.
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... For instance, peppermint oil obtained from Mentha piperita is a rich source of menthofuran (0.4-14.6%) and viridifloral generally adulterated with menthol oil obtained from Mentha arvensis in which both of these valuable compounds are either very low or absent. Therefore, to fulfil market demands, peppermint is adulterated with menthol oil [4]. ...
... For instance, peppermint oil obtained from Mentha piperita is a rich source of menthofuran (0.4 to 14.6%) and viridifloral generally adulterated with menthol oil obtained from Mentha arvensis in which both of these valuable compounds are either very low or absent. Therefore, to fulfil market demands, peppermint is adulterated with menthol oil [4]. ...
Full-text available
Several species of the Lamiaceae family are the primary source of bioactive aromatic oils and secondary metabolites, having broader applications in the cosmetics, pharmaceuticals, food, confectionery and liquor industries. Due to the scarcity of raw materials and high costs of this family's economically vital species, its products often adulterated to cater to the market's high demand. The present study provides a DNA based approach for identifying different species of this family. Henceforth, the performance of three already proposed barcode loci (matK, trnH-psbA and trnL) was examined for their PCR amplification and species recognition efficacy on various Lamiaceae species and cultivars using three different approaches such as pairwise genetic distance method, BLASTn and phylogenetic tree based on maximum likelihood (ML) analysis. Results illustrate that among all the DNA barcoding loci, matK locus can accurately and efficiently distinguish all the studied species followed by trnH-psbA and trnL. Present investigation may help diminish the illegal trade and events of adulteration of medicinally important plants species in genus Mentha, Ocimum and Plectranthus. This investigation will also help fulfil the scarcity of sequences of barcode loci of these species in the NCBI database. Apart from providing a molecular level reference for identifying processed herbal products, this technique also offers a convenient method for species identification and germplasm conservation of the Lamiaceae family.
... The global market for essential oils has increased steadily over the past several decades due to an increasing demand for pure and natural ingredients in various industries, including flavors and fragrances, cosmetics, and aromatherapy [1,2]. Unfortunately, the increased demand for essential oils has also intensified their economically motivated adulteration by unscrupulous providers [3]. In addition to the dishonest economics, adulterated essential oils could pose serious public health consequences, given the proclivity of consumers to use essential oils for their medicinal properties [2,4,5]. ...
... The level of adulteration of essential oils varies depending on the expertise of the adulterers [6]. The challenges associated with the authentication of essential oils are compounded by the natural variations in chemical composition due to geography, climate, and altitude, and the lack of an international organization that regulates standards for essential oil trade and commerce [3,7,8]. Correspondingly, a broad range of analytical methods are required to determine the authenticity of essential oils, including physical, chemical, chromatographic, spectroscopic, and thermal techniques [9]. ...
Full-text available
Current methods for the authentication of essential oils focus on analyzing their chemical composition. This study describes the use of nanofluidic protein post-translational modification (PTM) profiling to differentiate essential oils by analyzing their biochemical effects. Protein PTM profiling was used to measure the effects of four essential oils, copaiba, mandarin, Melissa, and turmeric, on the phosphorylation of MEK1, MEK2, and ERK1/2 in the MAPK signaling pathway; Akt and 4EBP1 in the pI3K/Akt/mTOR signaling pathway; and STAT3 in the JAK/STAT signaling pathway in cultured HepG2 cells. The gain or loss of the phosphorylation of these proteins served as direct read-outs for the positive or negative regulatory effects of essential oils on their respective signaling pathways. Furthermore, protein PTM profiling and GC-MS were employed side-by-side to assess the quality of the essential oils. In general, protein PTM profiling data concurred with GC-MS data on the identification of adulterated mandarin, Melissa, and turmeric essential oils. Most interestingly, protein PTM profiling data identified the differences in biochemical effects between copaiba essential oils, which were indistinguishable with GC-MS data on their chemical composition. Taken together, nanofluidic protein PTM profiling represents a robust method for the assessment of the quality and therapeutic potential of essential oils.
... With these increased health claims around botanical sources of linalool comes a greater need to ensure their identity. The specific symmetry of the enantiomer ratio that is produced is specific to a given botanical and, therefore, is used to ensure its identity [7]. Chirality specifications are an important tool in confirming the authenticity of extracted essential oils. ...
Full-text available
The chiral analysis of terpenes in complex mixtures of essential oils, necessary for authentication, has been further developed using chiral tagging molecular rotational resonance (MRR) spectroscopy. One analyte that is of particular interest is linalool (3,7-dimethyl-1,6-octadien-3-ol), a common natural chiral terpene found in botanicals with its enantiomers having unique flavor, fragrance, and aromatherapy characteristics. In this MRR demonstration, resolution of the enantiomers is achieved through the addition of a chiral tag, which creates non-covalent diastereomeric complexes with distinct spectral signatures. The relative stereochemistry of the complexes is identified by the comparison of calculated spectroscopic parameters with experimentally determined parameters of the chiral complexes with high accuracy. The diastereomeric complex intensities are analyzed to determine the absolute configuration (AC) and enantiomeric excess (EE) in each sample. Here, we demonstrate the use of chiral tagging MRR spectroscopy to perform a quantitative routine enantiomer analysis of linalool in complex essential oil mixtures, without the need for reference samples or chromatographic separation.
... One of them is the addition of single raw materials. This form of adulteration can be easily detected by analytical methods or not, depending on the substance in question [27]. ...
Diffraction gratings are recorded in a holographic photopolymer containing nematic liquid crystal and peppermint oil. The presence of the oil modifies the polymerization and the holographic response. The composite containing oil adulterated with triethyl citrate obtains a diffraction efficiency related to the oil's purity. The results obtained suggest the possibility of developing a holographic chemical analysis method for quality control of raw materials.
... To the best of the authors' knowledge, several papers describing strategies for revealing EO adulterations that occur via the addition of cheaper EO or synthetic compounds have been reported in the literature and have recently been reviewed [4,7,8]. Conversely, there are few papers that describe approaches to reveal the addition of vegetable oils to dilute EO [9][10][11]. ...
Full-text available
The quality control of essential oils (EO) principally aims at revealing the presence of adulterations and at quantifying compounds that are limited by law by evaluating EO chemical compositions, usually in terms of the normalised relative abundance of selected markers, for comparison to reference values reported in pharmacopoeias and/or international norms. Common adulterations of EO consist of the addition of cheaper EO or synthetic materials. This adulteration can be detected by calculating the percent normalised areas of selected markers or the enantiomeric composition of chiral components. The dilution of the EO with vegetable oils is another type of adulteration. This adulteration is quite devious, as it modifies neither the qualitative composition of the resulting EO nor the marker’s normalised percentage abundance, which is no longer diagnostic, and an absolute quantitative analysis is required. This study aims at verifying the application of the two above approaches (i.e., normalised relative abundance and absolute quantitation) to detect EO adulterations, with examples involving selected commercial EO (lavender, bergamot and tea tree) adulterated with synthetic components, EO of different origin and lower economical values and heavy vegetable oils. The results show that absolute quantitation is necessary to highlight adulteration with heavy vegetable oils, providing that a reference quantitative profile is available.
... [8,9] For essential oils containing chiral compounds, enantioselective gas chromatography is a very useful technique to detect the adulteration by the addition of synthetic compounds. [7,9,10] Spectroscopic techniques, such as nuclear magnetic resonance (NMR), fluorescence spectroscopy, and nearinfrared spectroscopy, have also been proposed for authentication of essential oils. [7,[11][12][13][14] Usually, spectroscopic techniques are combined with chemometric methods, thus resulting in very effective tools for the rapid identification/characterization of samples. ...
Essential oils are liquid mixtures of volatile compounds extracted from plants. Their quality is usually controlled via gas chromatography (GC), although with limitations when adulterants are nonvolatile substances. The essential oils of lavender (Lavandula angustifolia Mill.), peppermint (Mentha piperita L.), patchouli (Pogostemon cablin Benth), and their adulterated versions were measured by GC coupled to flame ionization detector (GC‐FID) and Raman spectroscopy. Canola oil, a nonvolatile substance, was used as the adulterant. The adulterated essential oils contained 1%, 3%, 5%, 10%, 15%, and 20% (v/v) of canola oil. Chromatograms of the adulterated essential oils containing 20% (v/v) of canola oil showed decrements in peak areas of the essential oil components, compared with peaks of the pure essential oils. The highest decrements were observed for the adulterated essential oil of patchouli. In general, detection of adulterated essential oils by simple visual inspection of the Raman features was difficult, due to slight differences observed in the spectra. Principal Components Analysis (PCA) allowed achieving a good spectral discrimination between pure and adulterated essential oils. These results suggest that Raman spectroscopy can overcome limitations of GC‐based methods, thus becoming an interesting alternative and complementary technique for quality control of essential oils. The detection of adulterated essential oils by mean of Raman spectroscopic measurements and the application of Principal Components Analysis (PCA) is possible. A good spectral discrimination between pure and adulterated essential oils can be achieved. Raman spectroscopy can overcome limitations of gas chromatography‐based methods.
... Essential oils are natural lipidic substances extracted from fruits, vegetables, and spices, and they are used in many sectors throughout the whole world due to their unique pure and characteristic functional properties [1]. Flavor, fragrances, cosmetics, aromatherapy, and phytomedicine industries demand essential oils because of their unique characteristic properties [2]. Previous studies have shown that citrus essential oils have been used as natural preservatives, flavorings, antioxidants, antibacterial, and antifungal agents in various foods [3]. ...
Full-text available
Essential oils are high-valued natural extracts that are involved in industries such as food, cosmetics, and pharmaceutics. The lemon essential oil (LEO) has high economic importance in the food and beverage industry because of its health-beneficial characteristics and desired flavor properties. LEO, similar to other natural extracts, is prone to being adulterated through economic motivations. Adulteration causes unfair competition between vendors, disruptions in national economies, and crucial risks for consumers worldwide. There is a need for cost-effective, rapid, reliable, robust, and eco-friendly analytical techniques to detect adulterants in essential oils. The current research developed chemometric models for the quantification of three adulterants (orange essential oil, benzyl alcohol, and isopropyl myristate) in cold-pressed LEOs by using hierarchical cluster analysis (HCA), principal component regression (PCR), and partial least squares regression (PLSR) based on FTIR spectra. The cold-pressed LEO was successfully distinguished from adulterants by robust HCA. PLSR and PCR showed high accuracy with high R2 values (0.99–1) and low standard error of cross-validation (SECV) values (0.58 and 5.21) for cross-validation results of the raw, first derivative, and second derivative FTIR spectra. The findings showed that FTIR spectroscopy combined with multivariate analyses has a considerable capability to detect and quantify adulterants in lemon essential oil.
... Adulteration also is intended to gain volume or weight to get a higher profit. Adulteration essential oils in various ways are by mixing it using cheaper essential (Do et al., 2015), add compound isolate or synthesis-dilution with inert material (Ng et al., 2015;Ke et al., 2015;Schipilliti et al., 2010) or add with other oil include nutmeg oil contaminant with castor oil (Yunilawati et al., 2013), lemongrass oil identified kerosene or coconut oil as adulterants (Do et al., 2015) and sandalwood oil diluted with cedarwood oil (Howes et al., 2004). The adulteration can degrade the quality and can lead to safety issues, health hazards, or noncompliance with the natural grade. ...
2-acetonaphthone (2-ACN) is a synthetic fragrance material used in various cosmetics, as an adulterant. Due to its frequent use, we have conducted an in-depth study to understand the photosensitizing potential of 2-ACN. Results of this study illustrate that 2-ACN showed photodegradation in 4 hrs under ambient UVR (UV radiations) and sunlight exposure. It generated (1-25µg/ml) superoxide anion radical (O2·‒) and singlet oxygen (¹O2) in the presence of UVR/sunlight through in-chemico and in-vitro test systems. 2-ACN (10 µg/ml) showed 43.9 % and 57.4 % reduction in cell viability under UVA and sunlight, respectively. Photosensitized 2-ACN generated intracellular ROS (6 folds in UVA; 8 folds in sunlight), which compromises the endoplasmic reticulum and mitochondrial membrane potential leading to cell death. Acridine orange/ethidium bromide dual staining and annexin-V/PI uptake showed cell death caused via 2-ACN under UVR exposure. The above findings signify the role of ROS via Type-I & Type-II photodynamic pathways in photosensitization of 2-ACN that ultimately promotes photodamage of important cellular organelles leading to cell death. The study advocates that solar radiation should be avoided by the users after the application of cosmetic products contain 2-ACN.
α-Pinene represents a member of the monoterpene class and is highly distributed in higher plants like conifers, Juniper ssp. and Cannabis ssp. α-Pinene has been used to treat respiratory tract infections for centuries. Furthermore, it plays a crucial role in the fragrance and flavor industry. In vitro assays have shown an enantioselective profile of (+)- and (−)-α-pinene for antibacterial and insecticidal activity, respectively. Recent research has used pre-validated biological structures to synthesize new chemical entities with pharmacological and herbicidal activities. In summary, this review focuses on recent literature covering synthetic pathways of flavor compounds and scaffold hopping based on the α-pinene core domaine, as well as the (enantioselective) activities of α-pinene. Recent approaches for authenticity control of essential oils based on their enantiomeric profile are also presented.
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Economically motivated adulteration (EMA) of food, also known as food fraud, is the intentional adulteration of food for financial advantage. A common form of EMA, undeclared substitution with alternative ingredients, is usually a health concern because of allergen labeling requirements. As demonstrated by the nearly 300,000 illnesses in China from melamine adulteration of infant formula, EMA also has the potential to result in serious public health consequences. Furthermore, EMA incidents reveal gaps in quality assurance testing methodologies that could be exploited for intentional harm. In contrast to foodborne disease outbreaks, EMA incidents present a particular challenge to the food industry and regulators because they are deliberate acts that are intended to evade detection. Large-scale EMA incidents have been described in the scientific literature, but smaller incidents have been documented only in media sources. We reviewed journal articles and media reports of EMA since 1980. We identified 137 unique incidents in 11 food categories: fish and seafood (24 incidents), dairy products (15), fruit juices (12), oils and fats (12), grain products (11), honey and other natural sweeteners (10), spices and extracts (8), wine and other alcoholic beverages (7), infant formula (5), plant-based proteins (5), and other food products (28). We identified common characteristics among the incidents that may help us better evaluate and reduce the risk of EMA. These characteristics reflect the ways in which existing regulatory systems or testing methodologies were inadequate for detecting EMA and how novel detection methods and other deterrence strategies can be deployed. Prevention and detection of EMA cannot depend on traditional food safety strategies. Comprehensive food protection, as outlined by the Food Safety Modernization Act, will require innovative methods for detecting EMA and for targeting crucial resources toward the riskiest food products.
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Enantiomeric ratios of linalool have been determined in various authentic essential oils of Indian origin using 10% heptakis(2,3-di-O-methyl-6-O-tert-butyldimethylsilyl)-beta-cyclodextrin as a chiral stationary phase. A complete enantiomeric excess (ee) for (3S)-(+)-linalool was characteristic of Lippia alba and Cinnamomum tamala leaf oils while less than 90% excess was noticed in Zanthoxylum armatum leaf, Zingiber roseum root/rhizome and Citrus sinensis leaf oils. On the contrary, an enantiomeric excess of (3R)-(-)-linalool characterizes essential oils of basil (100% for Ocimum basilicum) and bergamot mint (72 to 75% for Mentha citrata). Notably, some essential oils containing both enantiomers in equal ratios or in racemic forms are rose, geranium, lemongrass and Origanum. The enantiomeric composition studies are discussed as indicators of origin authenticity and quality of essential oil of Indian origin.
Content: Rosa damascena Mill. (Rosaceae) is an important ornamental and medicinal plant and a source of fragrance. Its hydrosol is known in Iran as golab (rose water) and has applications in religious ceremonies, food, and pharmaceuticals. Hydrosol is traditionally and industrially produced by distillation. The increase in market demand has led to production of inferior products for hydrosol that contain synthetic essences or essential oils of other plants, or that have been diluted with water. Inferior product often may be distinguished via its color changes and weak odor. However, details need to be determined by chemical analysis. Objective: The current study evaluated the composition and quality of 10 rose water samples purchased from local markets in Shiraz, capital of Fars province in Iran. Materials and methods: The essential oils of the samples were extracted and analyzed using gas chromatography-mass spectrometry. Results: RESULTS revealed that phenethyl alcohol, geraniol, and β-citronellol were the main constituents of most samples. In total, 22 constituents were detected and identified in the samples. Identification was determined for 60.97-96.07% of the essential oil components. Discussion and conclusion: It was concluded that Pelargonium and Dianthus essential oils and synthetic essences had been added to some samples. Dibutyl phthalate was also detected in most samples. This substance, which commonly exists as polyethylene terephthalate, may have been released into the samples from their containers.
Chirality evaluation is proved to be an efficient tool for the authenticity control of neroli, petitgrain and bergamot oils by enantioselective multidimensional gas chromatography (enantio-MDGC). The simultaneous stereochemical analysis of the main compounds linalool, linalyl acetate, α-terpineol using heptakis-(2,3-di-o-acetyl-6-o-tert.-butyldimethyl-silyl)-β-cyclodextrin as the chiral main column is described. α-Pinene, β-pinene, limonene, terpinen-4-ol and nerolidol are simultaneously stereoanalyzed with heptakis-(2,3-di-o-methyl-6-o-tert.-butyldimethylsi-lyl)-β-cyclodextrin. Characteristic authenticity profiles of neroli, petitgrain, bergamot and other citrus oils are deduced by enantioselective cGC as well as isotope ratio mass spectrometry (IRMS), online coupled with capillary gas chromatography. Enantiomeric ratios, isotopic data as well as quantification of bergamot oil compounds are evaluated integrally. Scope and limitations of the techniques are discussed.
The present contribution is focused on the off-line combination of high performance liquid chromatography (HPLC) and comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry (GC×GC-quadMS), and its application to the detailed qualitative analysis of essential oils. Specifically, a silica column was exploited for the separation of the essential oil constituents in two groups, namely hydrocarbon and oxygenated compounds. After, each HPLC-fraction was reduced in volume, and then subjected to cryogenically modulated GC×GC-quadMS analysis. The volatiles were separated on a normal-phase GC×GC column set, and identified through database matching and linear retention index information. The concentrated HPLC fractions gave origin to unexpectably crowded chromatograms, due to two fundamental GC×GC characteristics, namely the enhanced separation power and sensitivity. The results attained were particularly stimulating with regards to the oxygenated compounds, namely those constituents which contribute most to the essential oil aroma, and are of more use for the evaluation of quality and genuineness. Two genuine Citrus essential oils, bergamot and sweet orange, were subjected to analysis, and compared to applications carried out with a GC-quadMS instrument.
Determination of the authenticity of essential oils has become more significant, in recent years, following some illegal adulteration and contamination scandals. The present investigative study focuses on the application of near infrared spectroscopy to detect sample authenticity and quantify economic adulteration of sandalwood oils. Several data pre-treatments are investigated for calibration and prediction using partial least square regression (PLSR). The quantitative data analysis is done using a new spectral approach - full spectrum or sequential spectrum. The optimum number of PLS components is obtained according to the lowest root mean square error of calibration (RMSEC=0.00009% v/v). The lowest root mean square error of prediction (RMSEP=0.00016% v/v) in the test set and the highest coefficient of determination (R(2)=0.99989) are used as the evaluation tools for the best model. A nonlinear method, locally weighted regression (LWR), is added to extract nonlinear information and to compare with the linear PLSR model.
The essential oil of Rosa damascena Mill. is known for its fine perfumery application, use in cosmetic preparations and for several pharmacological activities. Due to its high value, it can be easily adulterated with flavors or cheaper oils. This study is aimed at a detailed phytochemical characterization of commercial samples of R. damascena essential oil and at their authenticity assessment. Nineteen commercial samples of R. damascena essential oil of different geographic origin and an additional authentic one, directly extracted by hydro-distillation from fresh flowers, were considered. GC/MS and GC/FID techniques were applied for the phytochemical analysis of the samples. EA/IRMS (Elemental Analyzer/Isotope Ratio Mass Spectrometry) and GC/C (Combustion)/IRMS were used to determine the δ(13) C composition of bulk samples and of some specific components. Citronellol (28.7-55.3%), geraniol (13.5-27.3%) and nonadecane (2.6-18.9%) were the main constituents of Bulgarian and Turkish essential oils, while those from Iran were characterized by a high level of aliphatic hydrocarbons (nonadecane: 3.7-23.2%). The δ(13) C values of bulk samples were between -28.1 and -26.9‰, typical for C3 plants. The δ(13) C values of specific components were in the usual range for natural aromatic substances from C3 plants, except for geranyl acetate, which displayed higher values (up to -18‰). These unusual δ(13) C values were explained by the addition of a natural cheaper oil from a C4 plant (Cymbopogon martinii, palmarosa), which was found to occur in most of the essential oils. GC/C/IRMS, in combination with GC/MS and GC/FID, can be considered as an effective and reliable tool for the authenticity control of R. damascena essential oil. Copyright © 2013 John Wiley & Sons, Ltd.
The confirmation of authenticity of essential oils and the detection of adulteration are problems of increasing importance in the perfumes, pharmaceutical, flavor and fragrance industries. This is especially true for 'value added' products like sandalwood oil. A methodical study is conducted here to demonstrate the potential use of Near Infrared (NIR) spectroscopy along with multivariate calibration models like principal component regression (PCR) and partial least square regression (PLSR) as rapid analytical techniques for the qualitative and quantitative determination of adulterants in sandalwood oil. After suitable pre-processing of the NIR raw spectral data, the models are built-up by cross-validation. The lowest Root Mean Square Error of Cross-Validation and Calibration (RMSECV and RMSEC % v/v) are used as a decision supporting system to fix the optimal number of factors. The coefficient of determination (R(2)) and the Root Mean Square Error of Prediction (RMSEP % v/v) in the prediction sets are used as the evaluation parameters (R(2) = 0.9999 and RMSEP = 0.01355). The overall result leads to the conclusion that NIR spectroscopy with chemometric techniques could be successfully used as a rapid, simple, instant and non-destructive method for the detection of adulterants, even 1% of the low-grade oils, in the high quality form of sandalwood oil.
Both phenomena, enantioselectivity as well as isotope discrimination during biosynthesis, may serve as "endogenous" parameters, provided that suitable methods and comprehensive data from authentic sources are available. This review reports on enantioselective capillary gas chromatography and online methods of isotope-ratio mass spectrometry in the authentication of food flavor and essential oil compounds, referring to literature references published in the last decade.