Nutrition 34 (2017) 29–46

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Nutrition
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Review

Converting citrus wastes into value-added products: Economic

and environmently friendly approaches
Kavita Sharma Ph.D., Neelima Mahato Ph.D., Moo Hwan Cho Ph.D.,
Yong Rok Lee Ph.D. *
School of Chemical Engineering, Yeungnam University, Gyeongsan, Republic of Korea

a r t i c l e i n f o a b s t r a c t

Article history: Citrus fruits, including oranges, grapefruits, lemons, limes, tangerines, and mandarins, are among
Received 27 June 2016 the most widely cultivated fruits around the globe. Its production is increasing every year due to
Accepted 20 September 2016 rising consumer demand. Citrus-processing industries generate huge amounts of wastes every
year, and citrus peel waste alone accounts for almost 50% of the wet fruit mass. Citrus waste is of
Keywords: immense economic value as it contains an abundance of various flavonoids, carotenoids, dietary
Citrus waste
fiber, sugars, polyphenols, essential oils, and ascorbic acid, as well as considerable amounts of some
Dietary fibers
trace elements. Citrus waste also contains high levels of sugars suitable for fermentation for bio-
Extraction methods
Enzymes ethanol production. However, compounds such as D-limonene must be removed for efficient
Phytochemicals bioethanol production. The aim of the present article was to review the latest advances in various
popular methods of extraction for obtaining value-added products from citrus waste/byproducts
and their potential utility as a source of various functional compounds.
Ó 2016 Elsevier Inc. All rights reserved.

Introduction
Citrus crops are among the most abundant popularly grown
in tropical and subtropical regions worldwide. The actual origin
of citrus is believed to be the warm southern slopes of the
Himalayas in northeastern India and Northern Myanmar.
Researchers have proposed that some species of citrus originated
in the Yunnan province of China [1–3]. Citrus fruits belong to the
rutaceae family, and various parts of the plant or tree are
appreciated for their health benefits. Sweet orange (Citrus
sinensis) is the major fruit in this group constituting w70% of the
total citrus production and consumption. Other citrus fruits, such
as tangerine or mandarin (Citrus reticulata), grapefruit (Citrus
vitis), lime (Citrus aurantifulia), and lemon (Citrus limonum), are
also grown and consumed extensively [4]. Main types of citrus
fruits, their byproducts and general anatomy are present in
Figure 1.
This study was supported by the National Research Foundation of Korea (NRF)
grant funded by the Korea government (MSIP) (NRF-2014 R1 A2 A1 A11052391),
the Nano Material Technology Development Program (2012 M3 A7 B4049675),
and Priority Research Centers Program of the Ministry of Education (2014 R1 A6
A1031189).
* Corresponding author. Tel.: 82-53-810-2529; fax: 82-53-810-4631.
E-mail address: yrlee@yu.ac.kr (Y. R. Lee).
It is well established that citrus fruits and its products are rich
sources of vitamins, minerals, and dietary fibers (nonstarch
polysaccharides) essential for nutrition, growth, and overall
development of the human body [5]. Recently, citrus fruits have
been examined for other nonnutrient yet biologically active
compounds, such as flavonoids, carotenoids, vitamins, and
minerals, which can help reduce the risk for many chronic dis-
eases (e.g., cardiovascular diseases and age-related macular
degeneration) [6]. The bioactive compounds extracted from cit-
rus fruits are rich in therapeutic properties and act as antioxi-
dant, anticancer, antitumor, and antiinflammatory agents. These
also are known for their antiviral, antiplatelet aggregation, and
antiinflammatory activities. Some of the bioactive compounds
have been reported to form protective enzymes in the liver and
to block the damage of the genetic materials in the cells
(Table 1 [6–20]).
The geographic distribution of production of the four main
types of citrus fruits varies in different countries, as shown in
Figure 2. For instance, Brazil is the dominant producer of sweet
orange. Brazil processes 47% of the world’s citrus fruits (the main
citrus-processing country in the world), followed by the United
States (29%) [21]. According to US Department of Agriculture-
Foreign Agricultural Service, 2010 [22], w30% of the citrus fruit
production is processed principally to make juice. China is

http://dx.doi.org/10.1016/j.nut.2016.09.006
0899-9007/Ó 2016 Elsevier Inc. All rights reserved.
30 K. Sharma et al. / Nutrition 34 (2017) 29–46

Fig. 1. (A) Main types of citrus fruits and their byproducts. (B) General anatomy of a typical citrus fruit.
 K. Sharma et al. / Nutrition 34 (2017) 29–46 31

Table 1
Important biological properties of bioactive compounds in citrus waste

Principle compound Function Action mechanism

Essential oil Antibacterial effect Active components influence certain metabolic functions of microbial cells [7]
Flavonoids, citrus essential Antifungal, antiviral Stimulates cyclic AMP synthesis in the cells [8,9]
oils activity
Hesperidin and naringin Antiplatelet activity Inhibits thromboxane A2 formation [10]
Hesperidin Antiinflammatory Inhibits eicosanoid synthesis and promotes antioxidant free radical scavenger activity, also
inhibits the kinases and phosphodiesterases essential for cellular signal transduction and activation [11]
Polymethoxyflavones, Anticancer effect Cell cycle arrest, suppresses proliferation and proapoptosis, antiangiogenesis [12,13]
flavonoids, limonoids,
b-carotene
Flavonoids (naringenin Antimutagenic effect Absorbs ultraviolet light and protects DNA by interacting directly with the tumoral agents, as in the
and rutin) induced chromosomal aberrations by bleomycin [11]
Flavones, polyphenols Antiproliferative effect Inhibits proliferation of MDA-MB-435, MCF-7, and human breast cancer cells [6]
Essential oil (flavonoids), Antioxidant activity Flavonoids, limonoids, coumarins act as a donor for hydrogen atoms or electrons in the transformation
phenolics, limonoids, of DPPH radical into its reduced form DPPH-H [7,14]
coumarins
Peel extracts Antilipoperoxidation Inhibits tissue lactoperoxidase and reduces the level of serum thyroid hormones and glucose,
activities with a parallel increase in insulin concentration [15]
Flavonoids Cardiovascular diseases Improves coronary vasodilation, decreases platelet activity to clot the blood, and prevents
low-density lipoproteins from oxidizing [6,16]
Flavonoids Antihyperglycemic Citrus flavonoids partly bind to starch, increase hepatic glycolysis and glycogen concentration,
and lower hepaticgluconeogenesis [17]
Peel oils Lipolytic effects The presence of ç-terpinene and p-cymene showed lipolytic effect; monoterpene hydrocarbons
consisting of one or two double bonds show stronger lipolytic effect than those having
three double bonds [18]
Flavonoids Neuroprotective effects Protects cortical neurons against oxidative stress, Ab-associated neurotoxicity, and glutamate-induced
excitotoxicity [19]
Polymethoxyflavones Biofilm inhibitory Inhibit cell–cell signaling and biofilm formation [20]

DPPH, 1,1-diphenyl-2-picryl-hydrazyl

leading in the production of mandarins and the United States
leads in grapefruit production. The European Union countries are
a major producer of sweet oranges, lemons, and mandarins.
Mexico is the fifth largest orange-producing country [21]. The
global production of all four types of citrus in the world (lemons,
oranges, tangerines/mandarins, and grapefruits) is expected to
increase in the future due to scientifically improved cultivation,
management techniques, better phytosanitary conditions,
favorable weather, and awareness [23]. Oranges, lemons, and
grapefruits are important cash crops in the tropical and

Fig. 2. Geographic distribution of production of major citrus fruits, namely, oranges, tangerines/mandarins, lemons/limes, grapefruits, and others across the globe (average
production during the years 2007–2016).
32 K. Sharma et al. / Nutrition 34 (2017) 29–46

Fig. 3. Classification of phytochemicals present in citrus fruits.

subtropical zones. Also, the consumption of fresh oranges is The composition of citrus fruits is affected by several factors,
exponentially increasing in many developing countries, such as such as variety, growth, maturity stage, and climatic conditions
Mexico, India, Argentina, Brazil, and China [24]. of that particular region [25]. During the fruit’s growth period,
 K. Sharma et al. / Nutrition 34 (2017) 29–46 33

Fig. 4. Outline of citrus processing and product formation from citrus farm to the market.

formation of a variety of phytochemicals takes place. These stilbenes, and condensed tannins. Later on, these phytochemicals
include low-molecular-weight phenolic (hydroxybenzoic and accumulate in the cells of the citrus fruits [4,26]. Generally, all
hydroxycinnamic acids), acetophenones, terpenoids, flavonoids, citrus fruits contain considerable amounts of lipids (oleic,

Fig. 5. Production of various byproducts from citrus industries.

34 K. Sharma et al. / Nutrition 34 (2017) 29–46
Table 2
Proximate composition of citrus byproduct, peel, pulp, and juice
Composition (g/100 g) Citrus byproduct Peel Pulp
Moisture content 8.51  0.2* 75.3  10.2y 85.7  0.0z
Crude protein 12.51  0.87x 10.2  3.70y 8.6  0.0z
Crude fiber 75.69  2.1* 57.0  10.0y 7.34  0.8k
Crude fat 0.52  0.02x 2.22  6.10y 4.9  0.0{
Total ash 8.09  0.41x 3.33  0.50y 6.5  0.0z
* From reference [38].
y
From reference [39].
z
From reference [40].
x
From reference [31].
k
From reference [41].
{
From reference [42].
linoleic, linolenic, palmitic, stearic acids, glycerol, and
aphytosterol), sugars (glucose, fructose, and sucrose), and
acids (primarily citric and malic). They also contain tartaric,
benzoic, oxalic, and succinic, insoluble carbohydrates (cellulose,
pectin), enzymes (pectinesterase, phosphatase, peroxidase),
flavonoids (hesperidin, naringin), limonin, isolimonin, peel oil
(D-limonene), volatile constituents (alcohols, aldehydes, ke-
tones, esters, hydrocarbons, acids), pigments (carotenes, xan-
thophylls), vitamins (ascorbic acid, vitamin B complex, and
carotenoids), and minerals (primarily calcium and potassium).
The different phytochemicals present in citrus fruits are pre-
sented in Figure 3.
Currently, individuals are becoming increasingly aware of
health and healthy diet, and therefore, the demands of natural
food additives have increased drastically. Consumers expect the
diet to be safe and health promoting. Citrus fruits are consumed
either fresh or in the form of different kinds of processed prod-
ucts. Figure 4 represents an outline of citrus processing and
product formation from citrus farm to the market.
Approximately >40% of the oranges produced globally are
used in processing to make different commercial products, such
as dehydrated citrus products or marmalades, jams, fresh juice,
and flavoring agents for beverages [24]. As a result of processing,
large amounts of after-wash waste water; solid residues (mainly
peels, membranes, and seeds); and semisolid residue after the
extraction of juice, in the form of centrifugation pulp, remain as
waste products. Figure 5 represents the production of various
byproducts from citrus industries.
The semisolid residue is mainly composed of endocarp re-
sidual membranes, vesicles, some extent of albedo, and exocarp.
This waste is rich in sugars, fibers, organic acids, amino acids and
proteins, minerals, oils, lipids, and large amounts of flavonoids
and vitamins [27]. The above components are found in various
amounts depending on different fractions of the fruit, such as
juice, albedo, flavedo, rag and pulp, or seeds [28]. Also, the pro-
portion of these components in citrus depends on different
methods or techniques employed for juice extraction [29]. The
citrus pulp constitutes w50 to 70% of the fruit, w60 to 65% peels,
w30 to 35% of internal tissues, and
10% seeds, by weight [30].
Industrial citrus waste is estimated to be >40 million tons
worldwide, and the amount of residue obtained from the fruits
accounts for w50% of the original whole fruit mass [31]. Citrus
pulp contains high contents of water and soluble sugars, which
make it highly perishable. These render a high rate of ferment-
ability, which causes many economic and environmental prob-
lems [32,33]. Additionally, a high content of organic matter
restricts its direct disposal as this might affect the natural and
beneficial microbial flora of the soil [34]. The processing of citrus
pulp includes addition of lime to neutralize the free acids. It
binds with pectins and releases water [35]. The composition of
dried citrus pulp is variable according to the relative proportions
Juice of skins and seeds. The latter mainly depends on the citrus
– species, variety, and the harvesting season. In addition to dried
– citrus pulp, citrus byproducts are used as functional ingredients
– for designing healthy foods (functional foods), which include
–
nondigestible carbohydrates and bioactive compounds, such as
–
dietary fibers, ascorbic acid, and flavonoids [29].
Citrus fruits have very high water content, making it difficult
to dry through common conventional methods or industrial
drying devices. Extraction of oils from the peel waste is very
important before disposal in landfills because the oils adversely
affect fermentation and bacterial decomposition. Murdock and
Allen reported that the oils present in the orange peels are toxic
to yeasts [36]. These have been found to exhibit inhibitory effects
on the growth of several useful bacteria, yeast and molds (e.g.,
Bacillus subtilis, Saccharomyces cerevisiae, Aspergillusawamorii)
[37]. Thus, it appears that the extraction of oil from peel waste
streams not only provide useful byproducts, but also contribute
to pollution abatement. Citrus waste, therefore, must be
processed quickly before compositional changes occur
(Table 2 [31,38–42]).
The environmental aspects of citrus waste reuse and its
management are described in Figure 6. The most common waste
management methods for citrus waste are composting, anaer-
obic digestion, incineration, thermolysis, and gasification [43].
The processing of citrus fruits generates different type of wastes,
which include solid, liquid, and distillery effluents. Solid waste
consists of peels, rags, seeds, sludge, and residue. Liquid waste
contains cannery effluents, can-cooler overflow, fruit-washing
waste waters, peeling and sectioning table waste waters, and
flushing water from floors. Distillery effluents include effluents
from citric acid and pectin, citrus molasses, and peel oil plants
[44]. Furthermore, citrus waste is disposed using different
methods (e.g., effluents are either directly released into lakes,
dumped in the ponding, discharged into groves or wells, or
managed by city sewage system). Discharge of wastes into lakes
may cause pollution and destruction of aquatic life, particularly
when the body of water is insufficient to dilute the waste
properly. On the other hand, ponding requires an isolated area.
Usually, several ponds are constructed, sometimes in a series, to
allow the waste to flow from one pond to another. Discharge into
groves or wells may result in defoliation of trees, possibly
because of the loss of oxygen in the soil around the roots of the
trees. Waste released into the city sewage system may contam-
inate the underground water sources, cause damage to pumps
and piping, clog sand beds, and leave foam in primary settling
tanks. Direct disposal of citrus waste (without proper processing)
causes environment problems. Therefore, it is important to treat
citrus waste systematically in food industries and other areas. In
recent years, researchers worldwide have been focusing on
developing different processing methods for complete
exploitation of various citrus fruit waste products [40,45,46].
Citrus waste is best used to obtain fiber and food ingredients
(e.g., pectins and mucilages) [47,48]. Additionally, many
value-added compounds or phytochemicals of commercial
importance can be efficiently extracted from citrus waste and
used in several ways. The purpose of this review was to describe
the potential benefits of citrus byproducts as a source of
functional compounds. In this regard, this review is unique in
presenting an extensive record of popular as well as
recently developed and advanced techniques of waste reuse,
extraction of various compounds, and their applications in
various fields.
 K. Sharma et al. / Nutrition 34 (2017) 29–46 35

Fig. 6. Environmental aspects of citrus waste reuse and its management.

Extraction methods used for citrus byproduct pharmaceutical industries have recently received a lot of
attention due to the increase in energy prices, carbon dioxide
In recent years, research and progress in developing emissions, and other environmentally related problems.
effective extraction techniques for chemical, food, and Techniques reported for the extraction of phenolic acids from
36 K. Sharma et al. / Nutrition 34 (2017) 29–46
Fig. 7. Different extraction methods and procedures involved in the extraction of value-added products. FTIR, Fourier transform infrared spectroscopy; HPLC, high-perfor-
mance liquid chromatography; GC–MS, gas chromatography–mass spectrometry; MS, mass spectrometry.
citrus peels include reflux [14,41], shaking [49], stirring [50],
and ultrasonic extraction [51]. Scientists are focusing on
developing novel techniques for industries that can offer more
compact, safer, efficient, energy-saving, and sustainable
extraction processes [52–55]. Different extraction methods
and procedures involved in the extraction of value-added
products are shown in Figure 7.
Certain techniques for extraction, such as supercritical
fluid extraction, ultrasound extraction, controlled pressure
drop process, and subcritical water extraction, typically
consume less solvent and energy. A list of widely employed
extraction and analytical methods is displayed in Table 3
[56–68].
The extraction techniques, such as microwave-assisted extrac-
tion (MAE), ultrasonic extraction (USE), supercritical fluid extrac-
tion, and accelerated solvent extraction, are considered efficient
methods for dealing with environment problems as well as
meeting various consumer demands [69]. Recently, MAE became
popular as a potential alternative to conventional extraction
methods, mainly due to considerable savings in processing time,
solvent consumption, and energy [70]. This method uses micro-
wave energy to heat solvents in contact with solid samples fol-
lowed by partition separation of the compounds of interest from
the sample into the solvent. This method is considered better than
USE and rotary extraction methods, as the use of microwave energy
ensures ease, rapidity, less solvent consumption, higher extraction
rate, energy savings, and better product yield with lower cost.
Microwave hydrodiffusion and gravity (MHG) [67] is advanta-
geous in comparison to conventional methods because it requires
shorter extraction periods and consumes less solvent amounts. It is
a novel, environmentally friendly green technology, also employed
for the extraction of polyphenols from onion [67]. MHG appears as
an efficient and economical technology. It works just under the
effect of microwave and earth’s gravity at atmospheric pressure
without using any solvent [71]. This process includes heating a
mass of 500 g of fresh plant waste under microwave at a certain
temperature without addition of any solvent or water. The direct
interaction of microwaves with the biological water inside the cells
of the plant material sets off the release of compounds. These
compounds then diffuse out along with hot water or crude juice
and settle down naturally under the effect of gravity on a spiral
condenser outside the microwave cavity where it is condensed. The
crude juice thus collects continuously in a graduated cylinder. The
extraction process is continued until no more juice is obtained or
overheating is detected [67].
Generally, waste is sent to waste disposal plants, which
require substantial transportation costs and availability of suit-
able sites for waste disposal. In citrus industries, the centrifuged
pulp waste is generally treated with alkaline or enzymatic
methods for obtaining animal feed. Enzymatic treatment is
considered one of the most efficient methods for processing the
pulp. The product obtained by this method have shown high
protein content, but not as high as compared with other agro
industrial waste products currently used as components of ani-
mal feed. Furthermore, the processed citrus waste have shown
excellent digestibility in vivo.
Extraction of value-added products
Phenolic and flavonoids
Citrus fruit waste is rich in biologically active compounds
including natural antioxidants, such as phenolic acids and fla-
vonoids [57,72]. Flavonoids are an important class of bioactive
compounds because of their versatile antioxidant, anticarcino-
genic, and antiinflammatory properties and their ability for lipid
antiperoxidation effects [73–75]. The two groups of flavonoids
found in citrus fruits are glycosylated flavones (luteolin, apige-
nin, and diosmin glucosides) and polymethoxylated flavones
 K. Sharma et al. / Nutrition 34 (2017) 29–46 37

Fig. 8. Chemical structures of common citrus flavonoid. (A) Flavones and flavone aglycon, (B) flavanones, and (C) flavonols.
38 K. Sharma et al. / Nutrition 34 (2017) 29–46

Fig. 9. Chemical structures of common citrus limonoids.

[14]. The chemical structures of citrus flavonoids are presented in
Figure 8.
These two groups and their species-specific patterns make
them good markers for detecting adulteration in commercial
juices [76–78]. Some glycosylated flavanones can be easily
transformed into corresponding dihydrochalcones, which are
potent natural sweeteners [79,80]. Additionally, the main fla-
vonoids found in citrus species are hesperidin, narirutin, nar-
ingin, and eriocitrin [81]. Peels and other solid residues of
lemon waste contain mainly hesperidin and eriocitrin, whereas
naringin and eriocitrin are predominant in liquid residue [82].
Peels and seeds are important sources of phenolic compounds,
which include both phenolic acids and flavonoids. The content
is richer in peels than in seeds [83,84]. The composition of seeds
and peels is not always the same for a determined species. For
instance, lemon seeds contain principally eriocitrin and hes-
peridin, whereas the peel is rich in neoeriocitrin, naringin, and
neohesperidin [14]. The ratios of the concentrations of different
glycosylated flavanones also are different; neoeriocitrin and
naringin are found in similar concentrations in the peel,
whereas in the seeds, eriocitrin is 40 times more abundant than
naringin [14]. Four main phenolic acids, such as caffeic, p-cou-
maric, ferulic, and sinapinic acids, are found in the peel of citrus
fruits. Sour orange peels are richest source of ferulic and sina-
pinic acids [14]. The bergamot citrus contains a number of
additional minor flavones (apigenin, luteolin, and
diosmetin-derived) and flavanones (eriodictyol, naringenin,
and hesperetin-derived), but the concentrations of simple
 K. Sharma et al. / Nutrition 34 (2017) 29–46
Fig. 10. Chemical structures of common citrus carotenoids.
phenolic acids in peel samples are found to be less [85]. The
reason might be high concentrations of phenolic acids in the oil
prepared from bergamot, indicating that peel waste must be
essentially free of most of the oil-soluble components [86]. The
content of total phenolics, quercetin equivalent flavonoids and
flavonols, and antioxidant activity in citrus byproduct, peel,
pulp, and juice is summarized in Table 4 [38,50,85,87–92].
An optimized MAE method for the extraction of phenolic
acids from citrus mandarin peels has been developed by Hayat
et al. [93]. Their method focused on optimizing certain definite
parameters, namely, microwave power, extraction time, type
and composition of solvent, solvent-to-solid ratio, soaking time,
particle size of sample, and extraction cycles. The method
showed better performance in terms of higher yields and
confirmed by different antioxidant assay systems. Furthermore,
the results demonstrated practical feasibility of MAE over
traditional or conventional methods for extracting phenolic
compounds from citrus mandarin peels. It also has been re-
ported that traditional or conventional methods consuming
long procedural times cannot save some phenolic acids from
degradation. Therefore, the application of MAE for the extrac-
tion of biologically active compoundsdin particular, some un-
stable phytochemicalsdhas an edge over conventional
methods.
39
A new process for the simultaneous production of pectin and
hesperidin (flavonoid) from citrus waste has been proposed by
Lo Curto et al. [46]. In this process, orange peel residue is pre-
treated with chemical reagents, such as calcium hydroxide and
hydrochloric acid. Ethanolic extract of orange peels has larger
quantities of hesperidin compared to water extracts. The yield of
hesperidin from the pretreated and dried orange peels ranges
between 3.7 and 4.5%, respectively, and between 1.8 and 2.3%
when it is extracted from fresh orange peels. The better yield is
believed to be due to the solubilization of pectin during pre-
treatment. Alternately, Li et al. proposed an enzyme-assisted
extraction method for better extraction of phenolic compounds
and flavonoids from the citrus wastes [57]. The enzyme-assisted
extraction method has been reported for obtaining other bioac-
tive compounds, such as carotenoids from marigold flower
(Tagetessp.) [94], vanillin from vanilla green pods (Vanilla plani-
folia) [95], and phenols from black currant (Ribesnigrum) [96,97].
The efficacy of this method depends on the activity of cell wall
degrading enzymes (e.g., glucanases and pectinases), which have
the ability to break down the proteins and carbohydrates present
in the cell walls. This renders the intracellular materials exposed
and more accessible for the extraction. The enzyme concentra-
tion of 1.5% (w/w) of the peel sample size is reported to be op-
timum for the highest extraction [57].
40 K. Sharma et al. / Nutrition 34 (2017) 29–46

Table 3
Analytical methods to determine different phytochemicals from citrus fruits

Extraction and analysis methods Type of compounds Brief description

Heat treatment
Enzyme-assisted extraction
Hydrolysis with cellulase and
pectinase enzymes
Steam explosion and further
fermentation
Methanol extraction and HPLC
Subcritical water extraction
USAE
USAE with HPLC/DAD–MS
analysis
Traditional hydrodistillation, cold
pressing, and microwave-accelerated
distillation with GC–MS
Optimize method HPLC method
LC–DAD and LC–MS
Microwave hydrodiffusion and gravity
Water-based extraction such as
hand-pressure extraction,
microwave extraction, and combined
hand-pressure and microwave
extraction
Cinnamics, benzoics, FG
Total phenolic contents
Monomer sugars
Bioethanol, galacturonic acid,
D-limonene
Naringin, hesperidin, didymin,
tangeretin, and nobiletin
Total phenol contents,
polymethoxylated flavones
Phenolic compound (FGs)
Hesperidin and neohesperidin,
diosmin, nobiletin, tangeritin
Essential oil
Diosmin, hesperidin, and
naringin
Flavonoids (isoquercitrin)
Essential oil
Pectin
Amounts of benzoic and cinnamic acids significantly increase; FG content and
antioxidant capacity decreases after heat treatment [56]
Highest recovery was achieved at a temperature of 50 C using the enzyme
celluzyme
MX. Enzyme-assisted aqueous extraction did not give as high recovery as the
solvent extraction [57]
Cellulose, pectin, and hemicellulose to monomer sugars [58]
Steam explosion and enzymatic hydrolysis pretreatments on lemon (Citrus
limon L.)
peel waste to obtain bioethanol, galacturonic acid and other coproducts, such as
D-limonene and citrus pulp pellets [59]
Analytical method for the simultaneous determination of five major flavonoids
from
citrus fruit by HPLC-PDA [60]
Subcritical water extraction at 200 C for 60 min used for fast recovery of
phenolic
compounds [61]
Optimum particle size of 2 cm2 is considered best for ultrasonic waves and
appeared
very effective in comparison to conventional procedure [62]
USAE, frequency of 60 kHz, extraction time of 30 min, and temperature of 40 C,
citrus
peel-to-water ratio (g/mL) 1/10, Ca(OH)2 as basifying agent, and water as
solvent [63]
Essential oil obtained in concentrated form, free from any residual solvents,
contaminants [64]
A reverse-phase HPLC method for the simultaneous determination was simple,
specific, precise, and accurate and is successfully used for the quantitative
analysis [65]
Rapid sample preparation and flavonoid determination, can be used in quality
assurance
routine analysis for adulteration detection in citrus concentrates and juices [66]
Microwave heating with earth gravity to devise a fast and efficient extraction
technique;
without adding solvent, a higher purity of the final product can be obtained [67]
Extract twice as much pectin obtained by the Soxhlet method and has better
productivity [68]

FG, flavanone glycoside; GC–MS, gas chromatography–mass spectrometry; HPLC-PDA, high-performance liquid chromatography-photodiode array; LC–DAD, liquid
chromatography–diode array detector; LC–MS, liquid chromatography–mass spectrometry; USAE, ultrasound-assisted extraction

Essential oils
The oil present in oil sacs or oil glands is located at different
depths in the peel and the cuticles of the fruit. Essential oils are
released when oil sacs are crushed or broken during juice
extraction. These volatile oils are used for flavoring ingredients
in drinks, ice creams, and other food products. Additionally,
substantial quantities of these oils are used in the preparation of
toilet soaps, perfumes, cosmetics, and other home care products
[98]. The major component of the oil extracted from citrus peels

Table 4
Content of total phenolics (mg GAE/g DM), flavonoids (mg QE/g DM), and flavonols (mg/g DM) and antioxidant activity (mmol Fe2þ/g DM) in citrus byproduct, peel, pulp,
and juice

Citrus byproduct Peel Pulp Juice

Total phenolics 147.6  6.3* 57.7  4.1* 673.9  18.5z (mg/mL)
Total flavonoids 49.2  1.33y 1.15  0.06* 260.1  23.3z (mg/mL)
Hesperidin 258.38  7.27x 455.3,k 29.5  0.32y 4007  42* (mg/g) 33.09  0.26{ (mg/L)
Naringin – 1104.6,k 0.54  0.02y 22  1* (mg/g) 307  173yy (mg/L)
Neohesperidin 18.17  0.74x 919.6,k 0.11  0.00y 9.07  1.65# 2.01  0.19{ (mg/L)
Antioxidant activity – 656.18  10.91** 456.7  15.7** 46.35**

* From reference [87].

y
From reference [50].
z
From reference [88].
x
From reference [38].
k
From reference [85].
{
From reference [89].
#
From reference [90].
** From reference [91].
yy
From reference [92].
 K. Sharma et al. / Nutrition 34 (2017) 29–46
is D-limonene, which is used as a green solvent for the deter-
mination of fats and oils instead of hazardous petroleum solvents
[99]. D-limonene is a very versatile chemical with a wide variety
of applications. Also, it is considered safer and more effective
than typical cleaning solutions.
The traditional method for extracting essential oils from the
citrus peels is cold pressing. In cold pressing, the peel and cuticle
oils are removed mechanically, yielding a watery emulsion,
which is then centrifuged to recover the essential oil [64]. Citrus
waste is required to be processed sufficiently before composi-
tional changes commence to occur. Murdock and Allen [36] re-
ported that the bacteria present in the citrus waste could convert
D-limonene in citrus oils to a-terpineol. Therefore, rapid
handling and management of cold-pressed peel oil is important
to maintain sanitation. Limonene is employed in medicine
manufacturing and as flavoring agent in food processing. It has
many applications in the chemical industry as well as in cos-
metics and domestic household purposes. A relatively simple
stream stripping and distillation method is effective for
removing oil components from oil-milled sludge. Both the oil
and aqueous distillate offer promising potential to recover flavor
enhancement materials from the citrus peel. In some countries,
distillation is considered an economical way to recover the oils,
with better yield of 0.21% compared with 0.05% from cold
pressing [64]. During distillation, the citrus peels, exposed to
boiling water or steam, release their essential oils through
evaporation. The steam and essential oil vapors are condensed
and collected in separate vessel called “Florentine flask.”
Compared with conventional steam distillation (SD), the new
distillation technique is effective in terms of saving time and
energy. Microwave steam distillation (MSD) is another technique
that highly accelerates the extraction process without causing
any changes in the volatile oil composition. The effectiveness of
MSD over SD is attributed to the more pronounced alteration of
cell structure, particularly the cell wall compartment by
microwaves.
Pectin and other fibers
Numerous attempts have been made to use citrus waste as a
source of dietary fiber [100], animal feed [101], polyphenols [57,
72], and biofuel [102]. Among these, pectin extraction is thought
to be one of the most reasonable ways [103]. Industrially, pectin
is produced from citrus waste under acidic conditions at an
elevated temperature of w100 C [104]. Recently, alternative
extraction methods including USE [105] enzymatic extraction
[106], MAE [107], and subcritical water extraction [108] have
been introduced for the extraction of pectin. Subcritical water
extraction has been found to be very effective for hydrolysis of
lignocellulosic material [109] and pectin extraction from citrus
peel waste [108,110]. The effect of extraction temperature on the
properties of pectins by using subcritical water has been inves-
tigated and reported by Wang et al. [111].
The processing of citrus fruits and the extraction methods
used for the recovery of its byproducts are very important in
order to obtain good yield at the end. For instance, maximum
performance was observed during the processing of citrus waste
with scalding, in terms of lipid-holding capacity (LHC); whereas,
the solubility of the dietary fiber and water-holding capacity
(WHC) of the final product was found to be reduced [31]. Simi-
larly, amounts of ascorbic acid and antioxidant activity of citrus
fibers are also reduced. Further research on the processing of
citrus waste is required to achieve an appropriate and optimized
method for complete valorization. The food and chemical
41
industries use different compositions of bioactive compounds.
The byproducts obtained from chemical industries showed lower
contents of pectin and flavonoids, and higher contents of lignin
and ash compared with the byproducts from food industries [31].
The reason for this might be that the kind of solvent used for the
extraction process in food industries must be safe for human
health. On the other hand, in chemical industries, hydro-
alcoholic solvents are used during the processes, which are
able to extract both, flavonoids and pectins but are not as friendly
as water alone. The byproducts from the food industry showed 3-
to 10-fold higher amounts of total flavonoids compared with the
byproducts from the chemical industry. Solvents play an
important role in the extraction of value-added products from
waste. Different solvents are associated with various issues that
have to be managed, such as inherent health or environmental
hazards. Health hazard information was derived from human
case reports or animal studies [112]. Manufacturers using organic
solvents must confirm the absence of risk during extraction. Also,
to demonstrate the safety of ingredients regarding solvent traces.
Most organic solvents are flammable, volatile, and often toxic,
and are responsible for environmental pollution and the green-
house effect. Safety, environmental, and economic aspects are
forcing the processing industries to turn toward greener sol-
vents. Among green solvents, the agro- or biosolvents play an
important role for the replacement of petrochemical solvents
and have high solvent power, are biodegradable, nontoxic, and
are not flammable.
Ethanol is one of the most common biosolvents obtained
from different sources, such as fermentation of sugar-rich ma-
terials (e.g., sugar beet and cereals). Although it is flammable and
potentially explosive, ethanol is used in large scale because it is
easily available with high purity, has a low price, and is
completely biodegradable.
In addition to ethanol, water is used in large amounts in
extraction processes. The polar nature of water makes it a ver-
satile solvent for the natural water-soluble products, such as
proteins, sugars, and organic acids, as well as for inorganic sub-
stances. Pressurized hot water extraction or subcritical water is
one of the most promising modern green extraction techniques
for rapid extraction. Furthermore, it is easy to manipulate the
dielectric constant (εr) of water that varies over a wide range just
by changing the temperature and pressure. Thus, at ambient
temperature and pressure, water has an εr of w80, which makes
it an extremely polar solvent. This value can be drastically low-
ered by raising the temperature under moderate pressure. For
instance, subcritical water at 250 C and a pressure just over
4 MPa has an εr value of 27, which is close to ethanol, and is
suitable for extraction of low-polarity compounds [113]. In this
direction, solvent-free techniques are gaining more attention.
MHG has been used for extraction of essential oils, colors, and
antioxidants. It is an original “upside-down” microwave alembic
combining microwave heating and earth gravity at atmospheric
pressure. Based on a relatively simple principle, this method also
involves placing the plant material in a microwave reactor,
without adding any solvent or water. The internal heating of the
water within the plant material distends the plant cells and leads
to the rupture of glands and oleiferous receptacles. The heating
action of microwaves thus frees essential oils and water in situ,
and separates dropwise down the gravity and out of the micro-
wave reactor [114].
In canning industries, generally hot chemical peeling with
sodium hydroxide is employed, which may lead to lower
flavonoid content in the extracts because this treatment leads
to the opening of the flavonoid skeleton to the chalcone form,
42 K. Sharma et al. / Nutrition 34 (2017) 29–46
making it more soluble in the solvent phase. Similarly, the
pectin content in the food industry byproducts is w2- to 10-
fold higher than that obtained from the chemical industry
byproducts.
Limonoids
Limonoids are classified into two main groups, limonoid
aglycones and limonoid glucosides (LGs). Limonoid aglycones
primarily include limonin and nomilin, which impart bitterness
to citrus juices and reduce the juice quality. Therefore, it is a
negative aspect for the citrus juice industry. This has been
researched for some time in effort to find a solution to this
problem. Limonoid aglycones present in seeds are water insol-
uble. On contrary, LGs abundant in citrus juice and tissues are
water soluble and tasteless, but safe to consume [115]. Structures
of typical limonoids are displayed in Figure 9. In general, limonin
is present in all citrus fruits but the amounts vary depending on
the variety, stage of fruit growth, and fruit part [60,83].
Recent researches reveal various health benefit and phar-
macologic aspects of limonoids, such as antibacterial, antifungal,
antiviral, antioxidant, and anticancer properties [116]. Limonoids
have been reported to induce detoxification of the enzyme
glutathione S-transferase in the liver cells of mice and rats [117].
It also has been found to inhibit the formation of chemically
induced neoplasia in the oral cavity, forestomach, small intestine,
colon, lung, and skin of animals [118]. Additionally, it inhibits the
proliferation of breast cancer cells grown in vitro [119]. Citrus
peel contains very small amounts of limonin; however, citrus
molasses, a major byproduct of citrus processing, is an attractive
source for LGs [120]. Furthermore, because molasses is liquid it is
the best potential source for industrial-scale extraction of LGs.
However, because it is not available commercially, extraction and
purification from the byproducts of juice processing plants could
increase its commercial value. It has been reported that the
method of extraction with supercritical fluids has an edge over
the method of traditional extraction with liquid organic solvents
due to its environmental compatibility [121]. Additionally, su-
percritical fluids have several other advantages, such as
nontoxicity, nonflammability, inability to leave residual
chemicals, and low to moderate operating temperatures and
pressures [122].
Carotenoid
The abundance of carotenoids in citrus fruits makes them an
important source of dietary nutrients. Carotenoids are usually
classified in two main classes: hydrocarbon carotenoids, known
as carotenes (e.g., b-carotene, lycopene); and oxygenated carot-
enoids, known as xanthophylls (e.g., b-cryptoxanthin, lutein,
violaxanthin). Chemical structures of common citrus carotenoids
are shown in Figure 10. Mono- or dihydroxylated carotenoids
often occur in esterified form and are more stable than the free
carotenoids. More than 115 carotenoids have been discovered in
citrus, contributing to various colors ranging from yellow to
red [123].
Carotenoids possess various health benefits. These are mainly
synthesized by bacteria, algae, fungi, and green plants from
acetyl-coenzyme A [124]. Natural colorants (carotenoids) are
preferred over synthetic coloring materials. In developed coun-
tries, carotenoids are widely used as natural colorants for foods
instead of artificial colorants. The latter have shown harmful
effects on human health. Industrially produced foods, such as
beverages, dairy products, confectionery margarine, and pasta,
contain b-carotene as colorant. The carotenoid content is higher
in the peel than in the pulp [125]. The quantitative detail of ca-
rotenoids is shown in Table 5 [50,126,127].
The orange from the navel variety contains zeta-carotene,
which indicates the presence of abundant amount of phytoene
in orange peel waste [128]. This is a commercial source of phy-
toene. Other carotenoids (e.g., b-cryptoxanthin) convert into
vitamin A, and therefore, are considered as provitamin A. b-
cryptoxanthin is a strong antioxidant and prevents free radicals
from damaging body cells and DNA. Many organic solvents are
used for the extraction of carotenoids from orange flavedo. Badr
[129] suggested that carotenoid could be extracted with a
mixture of isoproanol using petroleum ether. Furthermore, Ting
and Hendrickson [130] used acetone for extraction of caroten-
oids followed by hexane. Weissenberg et al. [131] reported
diethyl ether and methanol to be good solvents for extracting
carotenoids from sour orange. To evaluate the toxicity of carot-
enoids derived from natural sources, oral toxicity of carotenoids
extracted from citrus peel was studied [132]. Results showed that
there was no adverse effect of the mixture of carotenoids
extracted from citrus peel.
Citrus byproduct in pharmaceuticals, cosmetics, and food
Citrus processing generates a huge amount of waste, largely
converted in the form of press cakes (flavedo, albedo, seeds, and
remains of juice vesicles). It is very difficult to dispose of the
press cakes appropriately because of the high cost of handling
and transport. Alternatively, these wastes are being researched
for production of consumer products, such as novel whitening
phytochemicals from natural sources, compounds of pharma-
ceutical importance, and so on. The pigment melanin is the end
product of melanogenesis and it determines the color of human
skin, hair, and eyes. Also, it has photoprotective role. It is
absorbed in the cells and protects the skin from ultraviolet light.
However, its overproduction and accumulation in the skin may
cause skin disorders and aesthetic problems, such as hyperpig-
mentation and dark spots [133]. One of the popular uses of citrus
waste is to exploit the antimelanogenic effects of ethanolic ex-
tracts of the press cakes [134]. The ethanolic extract of citrus
press cakes was tested for its capacity to inhibit melanin content,
tyrosinase activity, and the protein expression profile of TRP-1,
TRP-2, and MITF in murine B16 F10 melanocytes in the skin
[134]. It has been reported that citrus press cake extracts
significantly reduce the cellular melanin content, through inhi-
bition of tyrosinase activity and transcription factors TRP-1 and
TRP-2 in a dose-dependent manner. Furthermore, in vivo
assessment of the biological activity of citrus press cake extracts,
suggests that citrus byproduct is a promising candidate for
treating skin pigmentation disorders [134]. Essential oils ob-
tained from citrus wastes are well known due to their strong
Table 5
Content of carotenoids in citrus byproduct, peel, pulp, and juice
mg/g DW Citrus byproduct Peel Pulp Juice
Total carotenoid – 2.04  0.0* – –
Lutein – 1.2  0.0y 2.9  0.0y 0.76  0.05z
Zeaxanthin – 0.8  0.0y 4.5  0.0y 0.71  0.09z
Cryptoxanthin – 1.2  0.0y 5.3  0.0y 4.70  0.30z
b-Carotene – 0.3  0.0y 1.1  0.0y 0.76  0.04z
* From reference [50].
y
From reference [126].
z
From reference [127].
 K. Sharma et al. / Nutrition 34 (2017) 29–46
antimicrobial, antioxidant, and antiinflammatory properties and
have a number of potential applications, such as ingredients in
food additives, preservatives against spoilage, pharmaceuticals,
and cosmeceuticals [135]. The potential use of essential oils from
citrus waste as antiinflammatory and antimicrobial agents in
cosmetics has been reported by Yang et al. [136]. The essentials
oil has strong antibacterial activity that destroys the cellular
integrity of microbial cells and inhibits its respiration. It also
downregulates the synthesis of nitric oxide (NO), an endogenous
free radical species. It is synthesized in various animal tissues by
NO synthase (NOS), which activates the inflammatory process
[137]. NO production induced in various cells can trigger a
transduction cascade leading to tissue damage and inflammation
[138]. Citrus extracts have been observed to initiate strong in-
hibition of NO synthesis in lipopolysaccharide-treated
RAW264.7 cell line (macrophages of the immune system), sug-
gesting that it could be a valuable antiinflammatory ingredient
for use in cosmetic formulas [136].
The functional dietary fibers and antioxidants extracted from
citrus byproducts are used as ingredients in various food pro-
cessing to obtain health products. Citrus waste, especially albedo,
is a good source of fiber (i.e., pectin). It is a white, spongy,
cellulosic tissue right beneath the peel and is rich in fibers of
better quality than other sources of dietary fibers. Pectin as an
ingredient has been found to be very useful in improving cooking
yield, reducing formulation cost, and enhancing texture in food
products [139]. Fiber is suitable for meat products to increase the
cooking yield due to their water and fat-binding properties and
to improve texture [140]. Various types of fibers have been
studied alone and are combined with other food ingredients for
formulations of reduced-fat or low-calorie meat products [141]
and meat emulsions [142]. The albedo fibers are incorporated
either in different percentage in the cooked or raw state in dried
cured sausages [143]. Various enzymes and microorganisms are
used for the extraction of various value-added products from
citrus waste, such as flavonoids, alkaloids, coumarins, limonoids,
carotenoids, phenolic acids, and essential oils. A list of commonly
used enzymes and microorganisms for the extraction of value-
added products from citrus wastes is provided in
Table 6 [144–152].
Future directions for citrus byproduct
The purpose of the present review was to encompass various
strategies and methods that aim to maximize the reuse of citrus
wastes. Reuse will help to minimize environmental stress. By
implementing different comprehensive methods of citrus waste
reuse, it is possible to improve processing efficiencies and in-
crease profitability, which can set an example for achieving
cleaner production of various valuable compounds. The
Table 6
Microorganism involved in the production of value-added products from citrus
wastes
Microorganism Substrate Value-added product
Cellulase, Pectinase Citrus peel Flavonoids
Endo-polygalacturonase Citrus peel Oligosaccharides
Aspergillus niger Citrus peel Citric acid
Aspergillus terreus Citrus peel Limonene
Trichosporon penicillatum Citrus peel Pectin
Aspergillus niger Citrus peel Soluble sugar
Aspergillus sp. Juice sacs Protease
Saccharomyces cerevisiae Citrus waste Bioethanol
Penicillium sp. Citrus peel Protein
43
exploitation of citrus byproducts as a source of functional com-
pounds and their application in food and beverages, pharma-
ceuticals, and cosmetic units is promising. This requires
collaborative and interdisciplinary research of food technologists
and chemists, nutritionists, and toxicologists. As we achieve this
goal, several important factors must be considered, including an
efficient infrastructure; internal resources; identification of the
best alternatives for waste streams; a systematic, rigorous, and
quantitative approach; and efficient analytical tools. Complete
use of citrus waste practices can be a catalyst for organizations to
realize that reducing waste not only helps to decrease costs and
improve processing efficiencies but also reduces the environ-
mental pollution load. Moreover, certain requirements must be
met to reuse the waste economically and effectively. In the near
future, the following needs must be met when considering the
complete use of citrus waste:
1. An adequate source of recyclable material needs to exist with
continuous supply and well-established system for extract-
ing the value-added compounds from the same.
2. A readily accessible facility or analytical method should be
available for complete characterization and quantification of
micronutrients and other functional compounds from citrus
byproducts.
3. Systematic use of citrus waste and maintaining a product
quality from the same is a significant barrier in the food-
processing industry, where shelf life, tamper resistance,
and food safety issues are paramount concerns. Further-
more, some phytochemicals, such D-limenon, and nitrates,
which have an adverse effect on the processing methods,
must be excluded by efficient quality control systems.
4. Active participation of the food and allied industries with
respect to sustainable production and waste management is
required.
5. Future investigations on the bioactivity, bioavailability, and
toxicology of citrus waste phytochemicals, their stability, and
interactions with other food ingredients should be carried
out with careful assessment of in vitro and in vivo studies.
If all of these components, such as technical and economically
feasibility challenges, product quality, and health safety, are not
in place, recycling will be incomplete.
Conclusion
Citrus crops are among the most widely cultivated,
commercially beneficial in tropical and subtropical regions. Their
combined annual production is w88 million tons. With high
demands for low-fat carbohydrates, low-sodium minerals, di-
etary fibers, vitamins (especially B complex and C), citrus fruits
have become an important as well as inseparable part of our diet.
In addition to essential nutrients, citrus fruits are a good source
of biologically active phytochemicals, i.e., carotenoids and fla-
vonoids, which provide provitamin A as well as antioxidant
benefits, respectively. More than 80% of the citrus is used for
Reference manufacturing processed items, such as juice, jams, jellies,
[144] marmalades, and so on. The waste produced in citrus processing
[145] industries is >40 million tons worldwide. The present review
[146]
focuses on the extraction of various beneficial value-added
[147]
[148] compounds or phytochemicals, such as flavonoids, carotenoids,
[149] pectin, sugars, limonoids, hesperidin, naringin, and essential oils,
[150] from these wastes, which are otherwise very expensive and
[151]
time-consuming to synthesize from conventional chemical
[152]
routes. Flavonoids, pectin, essential oils, and sugars are actively
44 K. Sharma et al. / Nutrition 34 (2017) 29–46
used in pharmaceutical applications and as natural additives for
functional foods. With progress in advanced techniques for the
extraction of beneficial compounds from citrus, it has been
possible to eliminate contamination of land and water. The an-
tioxidants and compounds present in the waste kill microbial
flora present in the soil and increase acidity. Microwave hydro-
diffusion and gravity technique for extraction of important
compounds has an edge over other conventional methods
because it consumes less solvent amounts. Other techniques,
such as ultrasonic extraction, supercritical fluid extraction, and
accelerated solvent extraction, also are considered efficient
methods for obtaining better yields of value-added compounds
and dealing with environment problems.
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