A Study on the use of Spectroscopic Techniques to

Identify Food Adulteration

Ajith Ravindran Flavia Princess Nesamani Nirmal D
1Research Scholar, Karunya Institute of School of Electrical Engineering and Karunya Institute of Technology and
Technology and Sciences Computer Science Sciences
India Ohio University India
ajithravindran@ieee.org Athens, United States dnirmalphd@gmail.com
fn042018@ohio.edu

Abstract—Due to the ever increasing demand of food materials,
adulteration is very common for gaining extra profits. Most of the
adulterants used are harmful chemicals that causes damage to
humans and the green ecosystem of the earth. Quality of food is
generally assessed by laboratory methods like chemical tests. By
utilizing wide variety of laboratory methods, experts can identify the
adulterants and can even calculate the quantity of the composition
of adulterants and compounds. But all these detection methods are
not user friendly, time consuming and employs destructive testing
mechanisms. The development of spectrometry leads to the
development of non-destructive, fast and accurate method to detect
the food adulteration. Various types of spectroscopy and different
techniques can be utilized for the detection of adulteration in food
particles like Spices, Natural Oil, Juice, Honey, Milk Products and
Wines.
Keywords— Spectroscopy; Adulteration in food; Reflection
Spectra; Fourier Transform Infrared Spectroscopy; NIR
Spectroscopy.
I. INTRODUCTION
Today, people tend to buy every article from shops unlike the
olden days. Years before, it was usual that people grew
vegetables, cultivated and harvested food grains. As time went
on, people started buying food items from market thus
avoiding the hardships of cultivation and harvesting. This was
also based on the trust people showed on the agriculture
industry and market. But now, it is very common, by the
farmers, vendors and shop keepers to indulge in activities of
adulteration for gaining immediate profit. Issues like ripening
of mango by artificial methods, additions of harmful pesticides
in vegetables and use of banned chemicals in curry powders
have been reported quite often. These activities provide better
results immediately, but are extremely harmful on a long term
basis. This is a matter of concern at the present scenario. It’s
high time that remedial measures to be devised
Spectroscopy can be defined as the study of
absorbance, transmittance and emission of light and
other radiation by matter, and its dependence to
the wavelength of the radiation[1]. The spectrum of the
components in a material is obtained by the unique interaction
of components present in the material with particular
frequencies of electromagnetic waves (absorption,
transmittance or emission). The spectrum of the particular
material is the graphical representation of the interaction
results with respect to frequency. Now a days, spectroscopic
techniques are used almost in all technical fields
of science and technology. Comparing the spectrum of
different materials having similar properties on the same scale,
it is possible to point out the differences between them. The
terms spectrography and Spectrophotometry are also
commonly used instead of spectrometry.
The basic block diagram showing the principle of
spectroscopy is shown in Fig. 1. The interaction of the
components present in a material and the electromagnetic
energy will characterize the components present in the
material to different levels such as atomic, nuclear,
supramolecular and molecular scales. In other words, it is
easy to obtain information about a material like its atoms,
molecules, crystal structure etc. and that depends on the
method and the source used for generating electromagnetic
waves.
Fig 1: Block Principle of Spectroscopy
The spectroscopic equipment type used for spectroscopic
analysis depends on the method used for detection. If the
material selected for analysis is soluble, a thin film, or a
coating, the analysis need to be start with UV-visible
spectroscopy (UV-VIS). The design of the spectroscopic
instrument is based on the nature of the electromagnetic
interactions involved, the particulars of the radiative process
and as well as the material like absorbing, transmitting or
reflecting[1]. The above mentioned factors determine the
wavelength of light source used and the method of detection

978-1-5386-0576-9/18/$31.00 ©2018 IEEE

of electromagnetic radiation. Methods commonly used are
emission, transmission and reflection.
II. TYPES OF SPECTROSCOPY
Spectroscopic Analysis are mainly classified in to two types
namely Quantitative Analysis[2] and Qualitative Analysis[3].
One of the important applications of the spectroscopy is the
determination of the concentration of different components in
foods materials. This application is based on the relationship
between the amount of electromagnetic radiation interacted
with the sample and he concentration of the chemical
components present in the sample. In Fig. 2 the beam of light
(single wavelength) passes through a sample, it may be
transmitted as such or a fraction of it may absorb. Io and I
represent intensities of the incident light and the transmitted
light respectively. Transmittance, denoted by T, is the ratio of
the intensity of incident and transmitted radiation.
The quantitative determination of compounds by
spectrometric technique is based on two simple laws namely
Beer’ law and Lambert’s law[4]. The laws relates the light
absorbed by a solution and the length of light path through the
solution.Spectroscopy techniques can be used to provide
qualitative analysis of food materials. Each atom or molecule
in a material has a particular set of energy which helps to
show a unique spectrum.
Fig. 2: Light passing through a Spectrometer
By analyzing the spectrum of a material, its magnitude and
position of the peaks (absorption or emission), it is possible to
determine the type of atoms or molecules present. For
example, specific chemical components shows absorption
peaks at specific wavelengths in NIR(near Infrared Region)
spectrum, whereas the type, number and bonding of the atom
within that molecule leads to unique absorption peaks in
spectroscopy. The sample reflectance spectrum is shown in the
Fig. 3. Spectroscopy is an efficient mechanism to detect the
physicochemical changes due to the alteration of the
molecules in a material. e.g., Detection of urea in milk, Starch
in curry powders etc.
Common spectrochemical analysis methods include Ultra
Violet & Visible Infrared Spectroscopy, IR absorption
Spectroscopy, molecular fluorescence, Spectroscopy, Raman
Spectroscopy, NMR(Nuclear magnetic resonance )
spectroscopy and Fourier transform infrared Spectroscopy.
Fig. 3: Sample Reflectance Spectrum
All of these methods, make use of the facts that the energy
of electromagnetic radiation may be absorbed or emitted by
the matter, when the energy associated with the
electromagnetic radiation equals the energy difference for
allowed transition of that sample. Here are some examples:
A) Ultraviolet and Visible Spectroscopy
The UV-VIS spectrometry is the oldest techniques of analysis
and also it is the basis for different methods used for the
determination of micro and semi micro quantities of sample.
In order to obtain a UV-VIS spectrum, the sample to be
analyzed, is irradiated with the electromagnetic radiation over
a particular range of wavelength[6]. At a time monochromatic
radiation in a single wavelength is employed. Thus, a UV
spectrum is a plot of wavelength vs the intensity of absorption.
These type of spectrometers are designed for a range of
200nm to 400nm (UV Range) and 400nm – 700nm (Visible
Range).
B) Fluorescence Spectroscopy
Fluorescence is the emission of light with respect to the
absorption of UV or VIS light of a fluorescent molecule
fluorophore[7]. Normally in fluorescence spectroscopy, two
basic types of spectra measured, (i) when a material sample is
excited at a fixed wavelength λx, emission spectrum is
generated by plotting emission intensity and emission
wavelength λm and (ii) an excitation spectrum obtained
when λx is scanned while the observation is plotted at fixed λm.
In food analysis, the emission spectra at a particular λx is used.
C) NIR Spectroscopy
Near‐infrared (NIR) spectroscopy is related to the emission
and absorption of electromagnetic radiations with
wavelengths in the range 780–2500 nm[7],[8].The
concentrations of constituents like water, fat, protein and
carbohydrate can be determined using normal absorption
spectroscopy. NIR spectroscopy is commonly used for the
analysis of food samples at the stage of process intermediates
and final products. The important advantage of NIR is that it
doesn’t require no sample preparation and hence, the analysis
is fast and user friendly. Another advantage is that, NIR
technology allows concurrent detection of several constituents
in a sample.
 D) Raman Spectroscopy
Information about the chemical composition of a sample can
be obtained with the help of Raman scattering of light by
molecules present in the sample. It employs a laser light
source which irradiate sample, and produce sufficient amount
of Raman scattered light, from there it is detected as a Raman
spectrum using CCD (Charge Coupled Device) camera. The
unique characteristic of finger printing pattern obtained
Raman spectrum helps to identify properties of sample
including crystallinity, orientation and stress. This
spectroscopy technique can be used to detect organic as well
as inorganic materials [9].
E) Fourier Transform Infrared Spectroscopy
The FTIR spectroscopy means Fourier Transform Infrared
spectroscopy, and this is the most preferred method among
infrared spectroscopy[10],[11]. When Infrared radiation hits a
sample, some fraction of radiation got absorbed by the sample
and some portion got transmitted. The signal obtained at the
detector is a spectrum corresponding to a molecular
‘signature’ of the sample.
The usefulness of spectroscopy for food samples arises
because different chemical composition in samples exhibit its
own unique spectral signature. The different spectroscopic
techniques and its operation range is tabulated in Table 1. The
coming section gives a detailed study on the adulteration in
different food substances and the spectroscopic techniques for
its detection.
Table 1: Spectroscopic techniques and its range
Spectroscopic Technique Range
Ultraviolet and Visible Spectroscopy 190nm – 800nm
Fluorescence Spectroscopy 190nm – 750nm
NIR Spectroscopy 780nm – 2500nm
Raman Spectroscopy 2500nm – 20000nm
FTIR Spectroscopy 2000nm – 25000nm
III. CHEMICAL DETECTION OF ADULTERATION
Conventional residue analysis consists of lot of procedural
steps, most of them are not easily understood by a common
man, but only by a trained person, because the analysis is
challenging. The analyst should be a trained person in
chemical analysis.They need to have a thorough understanding
of the behavior of the reactions of the chemical with different
residue samples.
The laboratory and its facilities must be designed in such a
way that it should ensure less contamination of samples as
well as maximum safety in handling different chemicals. The
laboratory should be equipped with all adequate facilities like
electricity, water, reagents, glassware, solvents and testing
apparatus.
IV. SPECTROSCOPY FOR FOOD ADULTERATION
Food adulteration can be generally classified into two separate
types, namely, incidental adulteration and intentional
adulteration. Incidental adulteration is the addition of foreign
substances to food particles as a result of negligence,
ignorance, or improper facilities which results in attaining
greater profits. These inferior substances include ground
material like sawdust, leaves etc. Intentional adulteration is the
addition of other low cost chemicals with a n intention of
getting extra profit. Eg., addition of starches in curry powders
species. Consumption of such substances may result in serious
damage to human health. Another example is the adulteration
of milk with adulterants that contains toxic substances like
caustic soda, urea, and vegetable oil. The cutoff limit of urea
concentration in milk is 700mg/L and the presence beyond
that limit may cause diseases such as kidney malfunction,
acidity, indigestion, cancer and ulcers. Spectroscopic
technique is an easy method for the detecting adulteration in
the following food substances.
A) Adulteration in Spices:
Spices are widely used in day to day life as food and also as
ingredient for medicine. In Ayurveda medicine, they are used
because of their antimicrobial as well as therapeutic effects.
Spices are commonly adulterated with low cost imitation
products and fillers[12]. Commonly used spices like paprika,
ginger and turmeric are often added with adulterants like corn
starch and sawdust. Sometimes, dyes which are toxic and
carcinogenic are also added along with this to hide the
presence of adulterants as well us the aging of a product
commonly used carcinogenic dye in chili powder is Sudan 1
dye. This dye comes under category 3 carcinogen which is
very harmful for human.
Fig. 4: Spectrum of Ginger Adulterated with Turmeric
Spectroscopy is an accurate testing technique for the detection
of this kind of adulteration in spices. This type of adulteration
can be detected with the help of VIS-NIR (Visible-Near
Infrared Region) spectrometers. The reflectance spectrum of
ginger adulterated with turmeric and with other spices are
shown in Fig. 4 and Fig. 5. Considering ginger, the spectrum
of pure ginger, we can see that it is smooth with a deep
absorption band around 400nm as shown in Fig. 4 and Fig.5.
The addition of external species will reflect in the spectrum.
When ginger is mixed with other spices, it shows a sudden dip
in its reflection spectrum around 670 nm, even visible with a
low concentration of 10%. At the same time, turmeric shows
an absorption band in the region between 400nm and 500 nm,
making its visibility at even 20% of concentration.
Chemometric analysis are used for the improvement in the
limit of detection, and for the easy identification of the
adulterant.
Fig. 5: Spectrum of Ginger Adulterated with other Spices
B) Adulteration in Natural Oils:
The “Extra virgin olive” oil abbreviated as EVOO shows high
level nutritional properties as well as a very special good taste
and it is manufactured by a process called “cold press”[13].
Consequently, the EVOO is the most expensive one in the
world market and its high commercial value stimulated some
vendors to adulterate the olive oil with lower price oils
obtained from different plants. Many efficient analytical
methods are developed for identifying adulterated olive oil
like nuclear magnetic resonance, mass spectrometry, gas
chromatography and chemical analysis. But all these
techniques are not practical options for the food industry since
they require time consuming processes which must be done in
dedicated laboratories by expert personnel and are not
convenient for online process.
Fig. 6: FTIR Spectra of Olive Oil[13]
FTIR spectroscopy can be used to detect adulterated olive oil.
The FTIR spectra obtained for the extra virgin olive oil EVOO
and for the sunflower oil (SFO) are shown in Fig. 5. The
spectral structure of the edible oils is mainly due to lipid
molecules containing fatty acids. This determines the presence
of characteristic absorption bands in the mid infrared region of
electromagnetic spectrum. Because the fatty acids composition
of a given edible oil is closely related to the vegetable variety
from which the oil is obtained, adulteration is easy. But
spectroscopic output reflects the similarity in the chemical
composition of the oils. At a closer inspection of the infrared
spectrum, some differences between oils located around 900,
1100 and 1400 cm-1 can be noted and that can be used as a tool
for determining the adulteration in EVOO.
C) Adulteration in Juices:
While considering adulteration in juices, Acai berry juice
contains the highest levels of antioxidant, anthocyanins,
which is directly related to the measurement of oxygen radical
absorption capacity, ORAC of any fruit. Anthocyanins are
natural pigments in acai berry which gives the color and its
antioxidant properties[14][15]. When we consider the
absorbance of a nutrient-dense juice blend comprising acai
berries and other fruits, UV-VIS spectra is very effective in
detecting Anti-Oxidants in Fruit Juice Blend.
Fig. 7: Absorbance Specrrum of Acai berry Juice at different pH[14]
The coloring pigments of our fruits and vegetables reduce
damage from free radicals and inflammatory processes. They
also reduce the risk of cancers and make our immune systems
more efficient. Anthocyanins in the juice blend are responsible
for its dark color whose absorbtion peak at 530 nm. The
spectra of the juice samples shows a peak at 260 nm.The
absorbance of the spectra of the juice under different acidic
conditions are shown in Fig. 7.
D) Adulteration in Honey:
As a natural product of a relatively high price, honey has been
a prime target for adulteration reasons of economic gain for a
long time[16][17]. Adulteration of honey is a highly
disgraceful practice which consists of incorporating sugar
syrups into the genuine product. For the adulteration of honey,
the concentration of the adulterant should be no less than 7%.
Molasses, starch solution, commercial glucose, sucrose, water
and inverted sugar are some examples of adulterants in honey.
There is a large natural variability of honey, such as
differences in species, maturity, environment, processing and
storage. Hence, detection of adulteration in honey is rather
difficult.
Fluorescence Spectroscopic technique is ideal for a rapid
screening of honey samples because they are simple to
perform. Very little sample preparation is necessary and
testing does not require expensive instrumentation or highly
trained personnel. The broad fluorescence peak observed
between 420-620 nm in spectrum is used to detect the samples with an accuracy of greater than 90%. The Raman
adulteration in honey. spectra of original milk versus milk contaminated with urea is
shown in Fig. 10

Fig.8: Spectrum of adulterated Honey with Starch[16]

Fig. 10: Raman spectrum of Milk containing Urea[18]

F) Adulteration in Wines
The adulteration of alcoholic beverages is also common now a
days. It is done to increase the apparent quality of the product
as well as to increase the alcoholic strength by using cheaper
sources of sugar and starch besides the fruit juice. One
example is the addition of diethylene glycol to wine to
increase sweetness[19]. Spectroscopic techniques are used for
the detection of red wine adulterated with glycerol. FTIR
spectra is used for the detection purpose.
(b)
Fig.9: Spectrum of Adulterated Honey with Glucose[17]

Generally, it is seen that the peak of honey decreases by

increasing the concentration of adulteration and impure honey
is easily detected. Adding any of glucose or starch into pure
honey considered to be dilution process and the overall shape
of the curve has no change with a clear decline of peak curve
compared with pure honey curve as shown in the Fig. 8 and
Fig.9.
E) Adulteration in milk and milk products:
Milk is assumed to be a best nutritional food in the form of liquid,
which can be consumed by all people ranging from small children to
older people. One common method practiced for adulterating
milk is the addition of water and then add urea for increasing
its solid not fat (SNF) value. A ratio between the amounts of
water and urea is maintained so that the specific gravity of the
adulterated milk equals to the natural milk and the lactometer
cannot detect the difference [18]. Milk with a urea
concentration above 700mg/L is harmful to human beings. Fig.12:FTIR spectra of Red Wine adulterated with different percentages of
Hence, detection and quantification of urea in milk is very Glycerol[19]
important for human health care.
FTIR spectra of glycerol adulterated wine samples were
Raman spectroscopy can be used for the detection of recorded in the region, 900–1500 cm-1.Fig. 13 presents the
impure milk. This method could detect urea mixed in milk FTIR spectra of red wine adulterated with different
percentages of glycerol with 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11,
12, 13, 14, and 15%. It is clear from Fig. 11 that when the
glycerol concentration increased a substantial increase in the
O-H bend occurred. The pronounced effect thus was effective
in detecting adulteration.
V. CONCLUSION
This review mainly list outs the recent advances in detecting
adulteration of powdered as well as liquid foods.
Spectroscopic techniques namely NIR and FTIR is very
efficient in predicting the features of liquid foods like
beverages, oils and dairy products. However, there are still
some limitations need to overcome in coming years. First one
is the, development of low cost, low powered handheld
instruments is needed for instant quality monitoring of food by
common people. Second one is that, in practical applications,
some calibration models available are not always stable and
reliable. Hence, development of chemometric techniques for
stable calibration model is necessary. In addition, the
effectiveness of NIR and FTIR spectrum is less in obtaining
information of certain minerals, therefore it cannot be used for
measuring all mineral contents sensitively. Development low
cost, low powered handheld instruments will revolutionize the
use of spectroscopic techniques for instant quality
measurement of foods.
ACKNOWLEDGMENT
This research work was supported by FACTS ElCi Research
Laboratory under Department of Electronics and
Communication Engineering of SAINTGITS College of
Engineering, Kottayam. I thank my fellow researchers who
provided insight into my research. I would also like to express
gratitude to my colleagues whose kind cooperation and
support provided the ambience for the progress of my
research.
REFERENCES
[1] C. P. Bacon, Y. Mattley, and R. DeFrece, “Miniature spectroscopic
instrumentation: Applications to biology and chemistry,” Review of
Scientific Instruments vol. 75, no. 1, pp. 1–16, 2004.
[2] Alessandrini, L., Romani, S., Pinnavaia, G. and Rosa, M. D. (2008).
"Near infrared spectroscopy: An analytical tool to predict coffee roasting
degree" ; Ann. Ahimica Acta. 625(1):95–102.
[3] Zalesskiy, S.S., E. Danieli, B. Blümich, et al., "Miniaturization of NMR
systems: desktop spectrometers, microcoil spectroscopy, and NMR on a
Chip for chemistry, biochemistry, and industry" ; Chem. Rev., 2014. 114
5641-5694.
[4] Cen, H., He, Y. and Huang, M. (2006) "Measurement of soluble solids
con- tents and pH in orange juice using chemometrics and VIS-NIRS" ;
J. Agric. Food Chem. 54(20):7437–7443.
[5] N. G. Osborne, T. Fearn, and P. H. Hindle, "Practical NIR Spectroscopy
with Applications in Food and Beverage Analysis", Long- man
Scientific and Technical, Harlow, 1993, p. 59
[6] Armenta, S., Garrigues, S. and Guardia, M. D. L. (2007). "Determination
of edible oil parameters by near infrared spectrometry"; Ann. Chim.
Acta. 596:330–337.
[7] Azizian, H., Mossoba, M. M., Fardin-Kia, A. R. Delmonte, P. Karunathi-
laka, S. R. and Kramer, J. K. (2015). "Novel, rapid identification, and
quantification of adulterants in extra virgin olive oil using near-infrared
spectroscopy and chemometrics" ; Lipids. 50(7):705–718.
[8] Blanco, M., Peinado, A. C. and Mas, J. (2004). "Analytical monitoring
of alcoholic fermentation using NIR spectroscopy" ; Biotech. Bioeng.
88:536–542.
[9] T. Iliescu, M. Baia, and V. Miclaus, “A Raman spectroscopic study of
the diclofenac sodium-beta-cyclodextrin interaction,” Eur. J.
Pharmaceut. Sci. 22, 487–495 (2004).
[10] Levin IW, Bhargava R (1997) "Fourier transforms infrared vibrational
spectroscopic imaging: Integrating microscopy and molecular
recognition" ; Ann Rev Phys Chem 56: 429-474.
[11] Alvarez-Ordóñez A, Prieto M (2012) "Technical and methodological
aspects of fourier transform infrared spectroscopy in food
microbiology research"; Journal of Fourier Transform Infrared
Spectroscopy in Food Microbiology, 1-18. Springer US.
[12] G. Downey, P. McIntyre, and A.N. Davies, "Detecting and Quantifying
Sunflower Oil Adulteration in Extra Virgin Olive Oils from the Eastern
Mediterranean by Visible and Near-Infrared Spectroscopy", Journal of
Agricultural and Food Chemistry, vol. 50, no. 20, 5520–5525, 2002
T.Pugner.
[13] Bendini, A., Cerretani, L., Di Virgilio, F., Belloni, P., Bonoli-Carbognin,
M. and Lercker, G. (2007). "Preliminary evaluation of the application
of the FTIR spectroscopy to control the geographic origin and quality
of virgin olive oils." J. Food Qual. 30:424–437.
[14] Xie, L., Ye, X., Liu, D. and Ying, Y. (2009). "Quantification of
glucose, fruc- tose and sucrose in bayberry juice by NIR and PLS".
Food Chem. 114 (3):1135–1140.
[15] Stinco CM, Baroni MV, Romina D, Naranjo DP, Wunderlin DA,
Francisco JH, Antonio J,Isabel MV (2015) "Hydrophilic tioxidant
compounds in orange juice from different fruit cultivars: Composition
and antioxidant activity evaluated by chemical and cellular based
assays". J Food Compos Anal 37:1–10. doi:10.1016/j.jfca.2014.09.006
[16] Kelly JD, Petisco C, Downey G (2006) "Application of Fourier
transform midinfrared spectroscopy to the discrimination between Irish
artisanal honey and such honey adulterated with various sugar syrups";
J Agric 54: 6166-6171
[17] Gok S (2015) "Differentiation of Anatolian honey samples from
different botanical origins by ATR-FTIR spectroscopy using
multivariate analysis"; Food chemistry 170: 234-240.
[18] Cipolat-Gotet, C., Cecchinato, A., De Marchi, M., Penasa, M. and
Bittante, G. (2012). "Comparison between mechanical and near-
infrared methods for assessing coagulation properties of bovine milk"
;.J. Dairy Sci. 95 (11):6806–6819.
[19] Q. Wu, T. Hamilton, W. H. Nelson, S. Elliott, J. F. Sperry, and M. Wu,
“UV Raman spectral intensities of E. coli and other bacteria excited at
228.9, 244.0, and 248.2 nm,” Anal. Chem. 73, 3432–3440 (2001).
[20] Cozzolino D, Holdstock M, Dambergs RG, Cynkar WU, Smith PA
(2009) "Mid infrared spectroscopy and multivariate analysis: A tool to
discriminate between organic and nonorganic wines grown in
Australia" ; Food Chemistry. 116: 761-765.