Vibrational Spectroscopy 102 (2019) 79–84

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Vibrational Spectroscopy
journal homepage: www.elsevier.com/locate/vibspec

Argan oil authentication using visible/near infrared spectroscopy combined T

to chemometrics tools
⁎
Sofia Farres, Loubna Srata, Fouad Fethi , Asmae Kadaoui
Laboratory of Physics of Matter and Radiations (LPMR), Physics Department, Mohammed First University Oujda, Morocco

A R T I C LE I N FO A B S T R A C T

Keywords: Visible and Near Infra-Red Spectroscopy (Vis/NIRS) technique was investigated as a non-destructive optical
Authentication method in order to authenticate argan oil. This study focuses on the detection and quantification of argan oil
Argan oil adulteration with cheap vegetable oils, using Vis/NIRS associated with chemometric tools in the spectral ranges
Adulteration from 500 to 1000 nm and 1000 to 1700 nm. The results achieved using baseline and first derivative pretreat-
Absorbance and chemometrics
ments before analyzing data set with multivariate calibration methods are the best. Partial Least Squares (PLS)
model has been established to predict the concentration of adulterants in pure argan oil with a correlation of
0.90, Root Mean Square Error of Prediction (RMSEP) of 4.67, Standard Error of Prediction (SEP) of 4.57 and a
bias of 1.26. Principal Component Analysis (PCA) model was established to discriminate samples according to
the type of adulterants. The results show Vis/NIRS efficiency as a rapid and non-destructive method and the
importance of chemometric tools in order to develop accurate models to authenticate argan oil. Less than 1 s run
by NIRS allows the identification of adulterants in pure argan oil from a percentage of adulteration of 0.35%
without needing to prepare or destruct samples.

1. Introduction producer to provide high-quality products. Different companies in

Food authentication has many sides including adulteration, mis-
labeling and misleading origin [1]. Adulteration of food products is a
current process motivated by economic reasons. It is defined as the
process by which quality of a given substance is reduced by the re-
placement of high cost ingredients with lower grade and cheaper sub-
stitutes. Argan oil is one of food that has been subjected to adulteration.
Given its several benefits as an important traditional alimentary med-
icine [2], it has many uses in cosmetics [3]. Because of its high price,
this oil is considered as a luxury food. One reason why there is always a
possibility of adulteration by cheap oils.
Argan oil comes from the argan tree (Argania spinosa), a species of
tree native to southwestern Morocco. Virgin argan oil is extracted from
the fruits of the argan tree, specifically the kernel contained in its core.
It is traditionally prepared by Berber women following an ancestral,
multistep process [4]. However, this traditional extraction is carried out
in inappropriate sanitary conditions and is time consuming. As a result,
attempts were made in order to improve argan oil quality by improving
its extraction process [5].
Worldwide, health and social improvement in food industry has a
direct relation with food safety and quality. Consumers are increasingly
asking for trusted trademarks in food, and therefore expect the
Europe and North America distribute the oil around the globe but the
product is exported only by Morocco [4]. Thus, due to the economic,
social and cultural importance of argan oil in Morocco, it is important
to prevent this unfair trade and ensure its origin and quality by estab-
lishing accurate models allowing the detection of possible adulterations
in short time [6].
Several methods were used to detect argan oil adulteration by dif-
ferent adulterants. These methods are based on liquid chromatography
[7], inductively coupled with plasma optical emission spectrometry [8],
Fourier Transform Infra-Red spectroscopy (FTIR) [9], Laser Induced
Fluorescence (LIF) [10], Electronic Nose and a Voltammetric Electronic
Tongue [11].
Most of these techniques are usually time-consuming, costly for
routine use in food industry, they require skilled operators and they can
have a high environmental impact. Hence there is a large demand for
rapid, cheap, and effective techniques for food quality control and
especially for food detection adulteration. The most flexible technique,
however, is NIRS. It is one of analytical tools used in food product
analysis [12,13] as an extremely powerful technique for industrial
quality control and process monitoring. Comparing to other analytical
technique, NIRS has advantages as a simple technique, quick, non-
destructive and it require no sample preparation or manipulation with

⁎
Corresponding author.
E-mail address: fouad@yahoo.fr (F. Fethi).

https://doi.org/10.1016/j.vibspec.2019.04.003
Received 16 September 2018; Received in revised form 12 March 2019; Accepted 23 April 2019
Available online 25 April 2019
0924-2031/ © 2019 Elsevier B.V. All rights reserved.
S. Farres, et al.
hazardous chemicals, solvents, or reagents [14]. It makes the detection
of possible adulteration easy via multivariate analysis methods
[15–17]. In recent years, NIRS has become an important industry for
studying food product quality, as well as their authentication [18–22],
thanks to the availability of light-fiber optics and the development of
chemometric data processing tools and software.
NIRS is distinguished by the possibility of on-site measurements and
remote sampling, in particular because the spectrometer can be placed
far from the sample. As another great benefit, it is considered as an
economic technique, its device is less expensive than other analytical
techniques device (total price around 3500 euro).
NIR spectra of foods comprise broad band arising from overlapping
absorptions corresponding mainly to overtones and combinations of
vibrational modes involving CH, OH and NH chemical bonds [23].
Many studies have been conducted on food products using NIRS such as
: The application of Near-Infrared Reflectance Spectroscopy (NIRS) to
detect melamine adulteration of soya bean meal [24], NIR spectroscopy
and chemometric for the discrimination of pure, powdered, purple
sweet potatoes and their samples adulterated with the white sweet
potato flour [25], Application of Vis/NIR spectroscopy for predicting
sweetness and flavor parameters of Valencia orange and grapefruit
[26], Simultaneous determination by NIR spectroscopy of the roasting
degree and Arabica / Robusta ratio in roasted and ground coffee [27].
In this work, NIRS combined to chemometric tools has been
exploited [17,28–30], particularly PCA [31] and PLS [32] in order to
establish an accurate and robust model allowing the detection of argan
adulteration by cheap vegetable oils.
2. Material and methods
2.1. Samples
Virgin argan oil samples (noted AO) were obtained from Agadir
(southwest of Morocco), made by traditional methods (hand-made), the
quality of the handmade argan oil used in this study is guaranteed,
whereas the cheap vegetable oils (noted respectively VO1 and VO2)
were purchased from a local market in Oujda (North east of Morocco).
Before mixing samples, VO1 and VO2 were heated repeatedly in order
to get a color similar to that of AO. To study the adulteration, a sum of
112 oil samples mixture were prepared by mixing pure AO with pure
VO1 and VO2 separately at levels between 0% and 30% (w/w) with a
percentage rate of adulteration about 0.4% for each sample.
Samples are gotten by measuring AO mass contained in a spectro-
photometer cell (1 cm) using a high-precision scale (SHIMADZU AUX
220, Max = 220 g, Min = 10 mg, e = 1 mg and d = 0.1 mg) and adding
VO1 and VO2 by drops using a micropipette (100–1000 μl, digital dial,
tip ejector), so as keeping the same mass of AO. Samples were num-
bered and classified in an increasing order according to their percen-
tage of adulteration, were stirred in order to homogenize the mixture
and stored in the dark until the day of analysis. To set the model al-
lowing the detection of the amount of adulterants in pure argan, 80
samples were used in the calibration/validation and 30 samples were
exploited to make the prediction.
2.2. Experimental set up
The absorbance of samples is measured using a halogen lamp (5 W,
6 V AC). All NIR spectra of different samples were acquired by a (CCD)
spectrophotometer (AVS-USB2000, Netherland) equipped with a mul-
timode fiber (SMA905) with core diameter 400 μm, a length of 2 m
(NA = 0.22) used to guide the light to the detector spectrometer. The
acquisition and storage of spectral data is done via Spectra Win soft-
ware for Windows using an integration time of 100 ms and spectra
average equal to 1 as adequate experimental conditions. Measurements
were taken at room temperature (25 °C), in the dark within the range
500–1000 nm and 1000–1700 nm. The absorbance spectra are obtained
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Vibrational Spectroscopy 102 (2019) 79–84
first of all by recording dark (light existing in room of manipulations); it
is considered as noise that should be eliminated to detect only the signal
coming from the sample. Then the reference signal I0 is recorded as the
light irradiating the sample. The absorbance spectrum was detected in
transmission mode using the equation:
A = log10 (I0 − ID/ I − ID )
With:
ID: Dark light
I0: Reference light
I: Transmitted Light
All obtained spectra were treated using chemometrics tools.
3. Theory
3.1. Near Infra-Red Spectroscopy (NIRS)
NIRS is based on the absorption of electromagnetic radiation at
wavelengths in the range 780–2500 nm. This technique has emerged
over the last decade in combination with the development of the fiber
optics, on-line probe accessories and chemometric evaluation proce-
dures, as an extremely powerful tool for industrial quality control and
process monitoring. NIRS is a physical-chemical analysis method based
on the interaction of light radiation in the near infrared area and mo-
lecules of samples [23,33]. The technique involves subjecting a sample
to radiation in the near infrared range. For each wavelength, the part of
the radiation reflected or transmitted by the sample is measured using
detectors and converted to absorbance. All these form the absorbance
spectrum which reflect the chemical composition of the analyzed object
[34].
3.2. Chemometrics
The complexity of NIR spectrum makes spectral interpretation and
quantitative parameter prediction difficult. Statistical approaches or
chemometric multivariate analyzes are developed to improve the use
and the interpretation of NIR spectra.
Chemometrics is defined as a mathematical technique used to ex-
tract useful information from measured physicochemical data. It is
based on the construction and exploitation of a behavioral model using
statistical tools and can handle complex and multivariable systems.
Thanks to chemometrics, both qualitative and quantitative data can be
included in qualitative analyses and modeled for a qualitative analysis
goal [35]. In order to take into account theoretical gaps and un-
controlled variations, it is necessary to accumulate spectra of many
samples and to treat the spectral collection thus obtained by chemo-
metric methods [35,36].
3.2.1. Principal Component Analysis (PCA)
PCA is one of the multidimensional descriptive techniques particu-
larly well adapted to the exploratory study of spectral data. This tech-
nique gives a synthetic representation by providing factorial cards in
which each spectrum is represented by a point. PCA substitutes the
original variables by synthetic ones called Principal Components (PC),
which contain the whole information. These new variables are ortho-
gonal to each other and they are classified according to their decreasing
importance. The interpretation of these graphs makes the under-
standing of analyzed data structure possible and easy. This interpreta-
tion will be based on some numerical and graphical indicators, which
help the user to interpret these data objectively [37].
3.2.2. Partial Least Squares Regression (PLSR)
PLSR is the most widely used chemometrics method in infrared
spectroscopy field. It consists of relating two data matrices, X and Y, by
a linear multivariate model and modeling their structure. It is based on
the projection of data on new axes that maximize the information. PLS
S. Farres, et al. Vibrational Spectroscopy 102 (2019) 79–84

regression determines spectrum regions where variations of spectrums

are correlated to concentration variations. Its advantages are evident in
its ability to analyze data with many, noisy, collinear, and even in-
complete variables in both X and Y and the precision of the models
parameter improves with the increasing number of relevant variables
and observations [38]. PLS regression has the advantage of treating the
entire spectrum even when the total composition of the calibration
samples is ignored. Only the concentration of the element should be
known, others are implicitly taken into account. Working over the
whole spectra makes the accuracy of the prediction better considering
the baseline. Besides, other spectra estimated by the model can be vi-
sualized, especially the residues, in order to check the spectral zones
poorly covered by the model or to identify aberrant spectra.
When PLS is properly used, the adjusted model is avoided, meaning
that when there is several variables, noise risk to be modeled, because
being a stepwise regression, the process of regression can be stopped
before modeling the error. This chemometric method is particularly
useful for the prediction of a set of dependent variables from a large set
of independent ones. There are two phases to set PLS Model calibra-
tion/ validation:
1- It is necessary to know the concentration associated with every
spectrum.
2- A part of the data is used for the calibration and the rest used in
the validation.

4. Results and discussion

4.1. Data processing

Was performed using the Unscrambler software (version 9.7, CAMO

ASA, Oslo, Norway) before multivariate analysis. The spectral range
500–1000 nm was reduced to 544–900 nm in order to remove noise.
Then, in order to minimize the effect of baseline shifts and noise, the
spectra were pre-processed using pretreatments which objectives are
attenuation and elimination of non-linearity between the dependent
and independent variables, elimination of interference and mitigation
of the random noise related to the experimental conditions [39].
Keeping in mind that it is impossible to know in advance which treat-
ment is the best for a given problem. Consequently all pretreatments are
Fig. 1. (a) Spectra of adulterated argan oil samples without any pretreatments
tested and the one that gives best results is applied.
in the spectral range 500–1000 nm. (b) NIR spectra of adulterated argan oil
samples after baseline preprocessing in the spectral range. 500–1000 nm.
4.2. Spectral features

Spectra were exported from Microsoft office excel format to
Unscrambler software for chemometric analysis. Figs. 1a and 2 a re-
present respectively raw spectra of 112 samples of the mixture of pure
argan oil with two cheap vegetable oils without any pretreatment in
two spectral ranges, 544–900 nm and 1000–1700 nm.
Spectra are similar to each other, there is a vertical offset between
them and a little bit noisy, this is due to the different optical paths run
through by light from sample to another. Thus before applying che-
mometric calculations, these deformations have to be processed by
applying chemometric pretreatments. To eliminate spectral variability
and improve signal-to-noise ratio, baseline pretreatment was applied on
spectra in the spectral range 544–900 nm (Fig. 1b) and baseline com-
bined to first derivative pretreatment, using Savitzky-Golay method
[40] with a second order polynomial on NIR spectra in the spectral
range 1000–1700 nm (Fig. 2b). Baseline makes the assumption that the
observed spectrum is the sum of a signal corresponding to uncontrolled
variations (background) and a "useful" signal containing the spectral
information. The correction consists of modeling the background and
subtracting it from observed signal. First derivative reduces baseline
variations and separates absorption bands more clearly. Hidden bands
of NIR spectra are thus exalted.
Before taking baseline and baseline combined to first derivative as
adequate preprocessing, several corrections were tested such as
smoothing, Multiplicative Scatter Correction (MSC), Standard Normal
Variate (SNV), first and second derivative and so on.
In Fig. 1b, a strong absorbance exists around the wavelength 545 nm
in the spectral range 544–735 nm (visible region) and in Fig. 2a, NIR
spectra show major peak around 1200 nm related to C–H second
overtone and OeH combination, and two other ones between 1370 nm
and 1450 nm related to C–H combinations [23]. Note that these bands
are very wide owing to the recombination of different frequencies of
absorbance.
After preprocessing spectra, chemometric methods were exploited
in order to extract hidden information. To do this, spectra were con-
verted to ASCII data and inserted in UNSCRAMBLER software.
4.3. PCA results
After pre-treating spectra, PCA was applied to extract the main in-
formation and reduce number of variables. All of spectra were ex-
amined using PCA on both raw and pretreated ones. In Fig. 3a samples
are dispersed in a bi-dimensional space PC1 and PC2 and are divided in
two distinct groups. The group of the top of scores plot is formed by
samples of AO adulterated by VO1, noted (group A) and the group in
the bottom refers to AO adulterated by VO2, noted (group B). The
majority of the information is explained by PC1 with a percentage of

81
S. Farres, et al.
Fig. 2. (a) NIR spectra of adulterated argan oil samples without any pretreat-
ments in the spectral range 1000–1700 nm. (b) NIR spectra of adulterated argan
oil samples after baseline combined to first derivative preprocessing in the
spectral range. 1000–1700 nm.
99% of total variance. This separation is due to the strong absorbance of
samples in the spectral range 544–735 nm and this absorbance is
mainly caused by samples coloration. To sum up, it can be concluded
that coloration of samples is the factor responsible of this separation.
This means that by this model, it can be determined for an unknown
sample the type of adulterant by taking its spectrum and insert it in this
model. Fig. 4a represents dispersion of samples in a tri-dimensional
score plot of PC1, PC2 and PC3.
In Fig. 3b samples are dispersed in a bi-dimensional space PC1 and
PC2. The majority of the information is carried out by PC1 with a
percentage of 97% of total variance and the rest of the information
(2%) is carried out by PC2 (Fig 4b represents dispersion of samples in a
tri-dimensional score plot of PC1, PC2 and PC3). Samples are divided in
two main groups noted group A (AO adulterated by VO1) and group B
(AO adulterated by VO2). Samples dispersion according to PC1 is
mostly due to the existence of C–H 2nd overtone, OeH and C–H com-
binations. In loadings plot (Fig. 5a and b) PC1vectors plot has the shape
of samples spectra which prove that the whole information is contained
in PC1.
4.4. PLS results
The purpose of PLSR is to establish a mathematical model that links
82
Vibrational Spectroscopy 102 (2019) 79–84
Fig. 3. (a) Bi-dimensional Scores plot of PC1 and PC2 vectors of 112 adulter-
ated argan oil samples in the spectral range 500–1000 nm. (b) Bi-dimensional
Scores plot of PC1 and PC2 vectors of 112 adulterated argan oil samples in the
spectral range. 1000–1700 nm.
sample’s spectrum to the concentrations of the components dosed.
Before the PLS regression, the data were pretreated by taking one
smoothing point. The PLSR method was successfully applied in previous
studies to predict the percentage of adulteration of argan oil by dif-
ferent other oils [10]. In this work, PLS was applied to predict the
percentage of adulteration of pure argan oil by VO1 and VO2. After
outlier removal, sample set was divided at random into two sets,
namely, calibration/validation sets containing 80 samples (Fig. 6a) and
prediction sets containing 30 adulterated samples (Fig. 6b). The ro-
bustness of the calibration model is usually estimated from the corre-
lation (R), the Standard Error of Calibration (SEC) and Root Mean
Square Error of Calibration (RMSEC).
Calibration model results are illustrated by Fig. 6a with a correla-
tion of 0.92, a SEC of 3.22 and RMSEC of 3.24. The accuracy of models
can be tested by samples that are not included in the calibration model
and whose concentration of adulterant is known, once the model has
been established, it can be applied to unknown samples. Keeping in
mind that models are acceptable, if the correlation coefficient (R) is
close to the unity and the (SEC), (RMSEC), (SEP) and (RMSEP) errors
are close to each other with low values. In practice, R value greater than
0.9 indicates a good response from NIRS for the parameter, between 0.9
and 0.7 the answer is average and below 0.7 the response is considered
S. Farres, et al.
Fig. 4. (a) 3D Scores plot of 112 adulterated argan oil samples in the spectral
range 500–1000 nm. (b) 3D scores plot of 112 adulterated argan oil samples in
the spectral range. 1000–1700 nm.
poor. In Prediction, when a new spectrum is inserted, it is compared to
the spectral basis, then the spectra of which is the closest serve in the
realization of a PLS regression.
Prediction result of the content of vegetable oils in argan oil is il-
lustrated by Fig. 6b with a correlation of 0.90, SEP of 4.67, REMSEP of
4.57 and a bias of 1.26. Horizontal and vertical axes respectively re-
present measured and predicted values for the appropriate adulteration
parameter.
The low value of SEP and RMSEP as well as the value of the cor-
relation coefficient which is close to unity proves that this mathema-
tical model obtained by the PLS provides best estimates for adulteration
rate.
5. Conclusion
The main results of this work present a new measurement protocol
using NIRS combined to chemometric tools as a new spectroscopy
analysis in order to assess argan oil adulteration by two cheap vegetable
83
Vibrational Spectroscopy 102 (2019) 79–84
Fig. 5. (a) Bi-dimensional loadings plot in the spectral range 500–1000 nm. (b)
Bi-dimensional loadings plot in the spectral range. 1000–1700 nm.
oils. Less than 1 s run by NIRS allows the detection of the percentage of
adulteration of argan oil from 0.35%.
It was essential to use spectral preprocessing such as MSC,
Smoothing, first and second derivative to remove noise, deformations
and any irrelevant information that could not be processed properly. It
was demonstrated that PCA is an excellent method to discriminate
adulterated argan oil samples and allowed the distinction between
samples adulterated with cheap vegetable oils. Besides PLSR model is
an excellent alternative tool to detect percentage of adulteration in pure
argan oil. Analyzes are made on 112 samples, of which 80 were chosen
to make the model and 30 samples are used for the prediction.
Good results of PCA models were achieved in both spectral range
500–1000 nm and 1000–1700 nm but ones obtained in the second
spectral range are the best, and for PLS, best results were obtained in
the spectral range 500–1000 nm with a correlation R of 0.90, RESMEP
of 4.67 and SEP of 4.57.
Results prove that combining NIRS with chemometric methods lead
to very successful prediction models that show excellent predictive
performance.
S. Farres, et al.
Fig. 6. (a) Calibration model in the spectral range 500–1000 nm. (b) Prediction
of 30 unknown samples using PLSR model in the spectral range. 500–1000 nm.
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