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Detecting Essential Oil Adulteration

January 2015
International Journal of Environmental Analytical Chemistry 02(02)

DOI:10.4172/2380-2391.1000132

Authors:

Karen E Boren

Young Living Essential Oils

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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

http://dx.doi.org/10.4172/jreac.1000132

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:

richcarlson@youngliving.com

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

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.

Introduction

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.

Abstract

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.

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.

doi:10.4172jreac.1000132

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

disrupter.

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].

Summary

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.

Reference

1. Browne CA (1909) Adulteration and the Condition of Analytical Chemistry

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-

735.

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,

87-89.

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.

doi:10.4172jreac.1000132

Page 3 of 3

8. Mosandl A (2004) Authenticity assessment: a permanent challenge in food

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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

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15. Moein M, Zarshenas MM, Delnavaz S (2014) Chemical composition analysis of

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2014.

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18. Pellati F, Orlandini G, van Leeuwen KA, Anesin G, Bertelli D, et al. (2013) Gas

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181.

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

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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

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İndiki zamanlarda insan həyatının bəzi maraqlı rolları məlumat, informasiya və bilikdir. Böyük məlumatların təhlili və modelləşdirilməsi məlumatların gələcək meyllərini proqnozlaşdırmaq və təhlil etmək üçün sürətli texnologiyaların inkişafı ilə birlikdə kütləvi məlumat anbarları tərəfin¬dən tələb olunur. Verilənlər bazalarında biliyin aşkarlanması üçün müxtəlif informasiya sistemlə¬rinin əhatə dairəsində istifadə olunan metodologiya və texnikalar lazımdır. Biliyi kəşf etmək üçün sərfəli məlumatları çıxaran texnologiyaya data mining deyilir. İnformasiya texnologiyalarının in¬san həyatının müxtəlif sahələrində yaranması qeydlər, sənədlər, şəkillər, səs yazıları, videolar, elmi məlumatlar və bir çox yeni məlumat formatları kimi müxtəlif formatlarda böyük həcmdə mə-lumatların saxlanmasına səbəb olmuşdur. Müxtəlif tətbiqlərdən toplanan məlumatlar daha yaxşı qərar qəbul etmək üçün böyük depolardan bilik/məlumat çıxarmaq üçün düzgün mexanizm tələb edir. Verilənlər bazasında bilik kəşfi (Discovery of Knowledge in Data KDD), çox vaxt da¬ta mi-ning adlanır, məqsəd böyük məlumat kolleksiyalarından faydalı məlumatların aşkar edilməsidir. Da¬ta mining-in əsas funksiyaları saxlanılan verilənlərin nümunələrini aşkar etmək və çıxarmaq üçün müxtəlif üsul və alqoritmlərin tətbiqidir. Son illərdə məlumatların öyrənilməsi və bilik kəşfi tətbiqləri qərar qəbul etmədəki əhəmiyyətinə görə diqqətə layiq görülmüş və müxtəlif təşkilatlarda vacib komponentə çevrilmişdir. Həmçinin böyük məlumat anbarlarından biliklərin/informasiya¬la¬rın çıxarılmasının vacibliyinə görə verilənlərin istehsalı müxtəlif sahələrdə insan həyatına birbaşa və ya dolayı təsir göstərən çox vacib və zəmanətli mühəndislik sahəsinə çevrilmişdir. Statistika, verilənlər bazaları, maşın öyrənməsi, nümunələrin yenidən təşkili, süni intellekt və hesablama imkanları və s. sahələrdə müxtəlif inteqrasiyalar və irəliləyişlərlə məlumatların əldə edilməsi sahəsi inkişaf etmiş və insan həyatının yeni sahələrinə daxil edilmişdir. Data mining müxtəlif tətbiqlərə malikdir və bu proqramlar insan həyatının müxtəlif sahələrini zənginləşdirib, o cümlə¬dən biznes, təhsil, tibb, elmi və s. gələcək tendensiyaları araşdırmaq. Məlumatların öyrənilməsinin müxtəlif tətbiq sahələri İnsan Resursları (HR), Müştərilərlə Əlaqələrin İdarə Edilməsi (CRM), Veb Tətbiqləri, İstehsalat, Rəqabət Kəşfiyyatı, Pərakəndə satış/Maliyyə/Bankçılıq, Kompü¬ter/Şə¬bə¬kə/Təhlükəsizlik, Monitorinq/Nəzarət, Tədris Dəstəyi, İqlim modelləşdirməsidir. İnsan həyatı¬nın hər bir sahəsi verilənlərin intensivliyinə çevrildi, bu da verilənlərin çıxarılmasını vacib kom¬po¬nentə çevirdi. Beləliklə, bu məqalə keçmişdən bu günə qədər verilənlərin əldə edilməsinin müxtəlif tendensiyalarını və onun nisbi sahələrini nəzərdən keçirir və onun gələcək sahələrini araşdırır. Açar sözlər: Verilənlər bazalarında bilik kəşfi, verilənlərin intellektual analizi, qeyri-səlis çox¬luq, Mininq(verilənlərin çıxarılması) texnikaları.

CAUSES, PREVENTIONS AND RECOVERY OF STUCK PIPE

Article

Full-text available

Feb 2023

Drilling an oil or gas well is a complex process which involves number of challenges associated with hydraulics, mechanics and geology. Although comprehensive planning activities take place prior to drilling, it is not always possible to avoid downhole problems. One of those problems is pipe sticking in which movement of the pipe is impossible. Many factors can lead to this undesirable incident. Keywords: pipe sticking, differentially stuck pipe, free pipe, invasive and non-invasive drilling fluid, overbalance, stuck point determination

The Use of Instrumental Technique and Chemometrics for Essential Oil Authentication: A Review

Article

Oct 2022

The use of essential oils for diverse purposes shows the increasing demand worldwide. These conditions encouraged fraudulent practices to maximize profit and set competitive prices. This review describes the characterization of essential oils (EOs) and their extraction technique before analysis. The type of adulteration and the technique for authentication, including chromatographic, spectroscopic, and others, either alone or in combination with the chemometrics technique, are also profoundly explained. Many studies use a combination of targeted and non-targeted approaches. Combining these two approaches were considered to produce accurate and reliable results for the authentication of EOs. The most advanced method was for authentication of lavender oil, citrus oils (lemon, bergamot, neroli), rose oil, peppermint oil, wintergreen oil, patchouli oil, and citronella oils. However, many EOs traded, and no international standards to regulate them.

Huile essentielle d’écorce de Cannelle de Ceylan

Article

Jun 2022
Actualit Pharm

La cannelle de Ceylan est une épice très appréciée pour ses qualités alimentaires dont est extraite de l’huile essentielle issue des feuilles ou du bois. Elle contient un aldéhyde aromatique, le cinnamaldéhyde, puissant et caustique, ainsi qu’un phénol considéré comme moins caustique que les autres. Ces deux molécules ont des propriétés anti-infectieuses importantes et à large spectre.

Economically Motivated Adulteration (EMA) of Food: Common Characteristics of EMA Incidents

Article

Full-text available

Apr 2013
J FOOD PROTECT

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.

Enantiomeric Composition of (3R)-(-)- and (3S)-(+)-Linalool in Various Essential Oils of Indian Origin by Enantioselective Capillary Gas Chromatography-Flame Ionization and Mass Spectrometry Detection Methods

Article

Full-text available

Apr 2009
NAT PROD COMMUN

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.

Chemical composition analysis of rose water samples from Iran

Article

May 2014
PHARM BIOL

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.

Comprehensive profiling and marker identification in non-volatile citrus oil residues by mass spectrometry and nuclear magnetic resonance

Article

Sep 2013
FOOD CHEM

Advances in the Authenticity Assessment of Citrus Oils

Article

Jan 1997

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 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

Article

Jul 2013

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.

Feasibility of using near infrared spectroscopy to detect and quantify an adulterant in high quality sandalwood oil

Article

Jul 2013

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.

Gas chromatography combined with mass spectrometry, flame ionization detection and elemental analyzer/isotope ratio mass spectrometry for characterizing and detecting the authenticity of commercial essential oils of Rosa damascena Mill

Article

Mar 2013
RAPID COMMUN MASS SP

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.

Detection and quantification of adulteration in sandalwood oil through near infrared spectroscopy

Article

Oct 2010
ANALYST

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.

Authenticity Assessment: A Permanent Challenge in Food Flavor and Essential Oil Analysis

Article

Oct 2004

Armin Mosandl

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.