A TECHNICAL SEMINAR REPORT

ON

“SEPARATION OF OIL AND PECTIN FROM ORANGE PEEL AND STUDY OF

EFFECT OF PH OF EXTRACTING MEDIUM ON THE YIELD PECTIN ”

SUBMITED

TO

UNIVERSITY INSTITUTE OFCHEMICAL TECHNOLOGY,

JALGAON

In successful completion of

B.Tech( Chemical Engineering)

By

Mr. Mukesh Raju Agale

Under the guidance of

Dr.A.K.Goswami
(Assistant Professor)

UNIVERSITY INSTITUTE OF CHEMICAL TECHNOLOGY

UICT,NMU, Jalgaon Page 1
 NORTH MAHARASTRA UNIVERSITY, JALGAON.

NORTH MAHARASTRA UNIVERSITY, JALGAON

CERTIFICATE
This is to certify that the Technical seminar report entitled

“SEPARATION OF OIL AND PECTIN FROM ORANGE PEEL AND STUDY OF

EFFECT OF PH OF EXTRACTING MEDIUM ON THE YIELD PECTIN ”
Completed by,

Mr. Mukesh Raju Agale

Is completed as per the requirement of University Institute of
Chemical Technology, jalgaon in fulfilment of the degree of Bachelor of
chemical Technology for the academic year 2016-2017.

Dr.A.K.GoswamiDr.R.D.Kulkarni
(Assistant Professor,U.I.C.T) H.O.D
Internal Guide U.I.C.T. NMU,Jalgaon.

External Examiner
Date:
Place Jalgaon

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 Table of content
1 Abstract…………………………………………………………………………………………………………………3

2 Introduction…………………………………………………………………………………………………………..4

3 what is pectin……………………………………………………………………………………………………….5

4 Commercial classification………………………………………………………………………………………6

5 The role of pectin in plants…………………………………………………………………………………7

6 Natural and healthy pectin………………………………………………………………………………..8

6.1 Biology………………………………………………………………………………………………………………..9

6.2 Chemistry………………………………………………………………………………………………………….10

7 Sources and production……………………………………………………………………………………….11

8 General properties of pectin………………………………………………………………………………..12

9 Gel formation properties of pectin……………………………………………………………………….13

10 Natural and healthy pectin………………………………………………………………………………14

10.1 High methoxyl pectin……………………………………………………………………………………….14

10.2 Amidated low methoxyl pectin………………………………………………………………………..15

10.3 Conventional low methoxyl pectin………………………………………………………………….16

11 Material and Method………………………………………………………………………………………….17

11.1 Separation of oil from peels:Raw Material ,method………………………………………..18

11.2 Extraction of pectin from orange peels…………………………………………………………….19

11.2.1 Comparison of yield of pectin from the dry cake residue left after

simple distillation and leaching…………………………………………………………………………………19

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12 Characterization of extracted pectin………………………………………………………….....22

13 Qualitative tests…………………………………………………………………………………………….25
14 Quantitative Test……………………………………………………………………………………………25
15 Application of pectin…………………………………………………………….……………………….28
15.1 Pharmaceutical uses of pectin……………………………………………………………………29
15.2 Medicinal application of pectin………………………………………………………………….30
16 Result and discussion……………………………………………………………………………………31

17 Conclusion ……………………………………………………………………………………………………31

18 References…………………………………………………………………………………………………….32

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 LIST OF FIGURE
Fig. No Name Of Fig. Page No.
1 High Methoxyl 6
(HM)pectin

2 Amidated Low Methoxyl 7

pectin(LMA)

3 Amidated low Methoxyl 7

(LMA)
4 Pectin classification 8
5 Chemical formulae for 10
pectin
6 Process flow chart for 21
extraction of pectin from
orange peel sampl

7 Pectin yield at different 24

pH of extracting medium

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 LIST OF TABLE
Table No. Name Of Table Page No.

1 List of the key HM 17

pectins, produced by
Silvateam

2 A list of the key LMA 18

pectins, produced by
Silvateam

3 A list of the key LMC 19

pectins, produced by
Silvateam.

4 Experimental 23
observations of yield of
pectin at different pH

5 Experimentel observation 25
of comparision of yield
pectin from dry cake
residue left after bsimple
distillation and leaching

6 The results of the 26

qualitative test for the
three samples

7 The characterized 28
parameters for the three
samples

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1 ABSTRACT
Pectin is an important polysaccharide with applications in foods, pharmaceuticals, and a number of
other industries. Its importance in the food sector lies in its ability to form gel in the presence of Ca2+
ions or a solute at low pH. Although the exact mechanism of gel formation is not clear, significant
progress has been made in this direction. Depending on the pectin, coordinate bonding with Ca2+ ions
or hydrogen bonding and hydrophobic interactions are involved in gel formation. In low-methoxyl
pectin, gelation results from ionic linkage via calcium bridges between two carboxyl groups belonging
to two different chains in close contact with each other. In high-methoxyl pectin, the cross-linking of
pectin molecules involves a combination of hydrogen bonds and hydrophobic interactions between
the molecules. A number of factors--pH, presence of other solutes, molecular size, degree of
methoxylation, number and arrangement of side chains, and charge density on the molecule--
influence the gelation of pectin. In the food industry, pectin is used in jams, jellies, frozen foods, and
more recently in low-calorie foods as a fat and/or sugar replacer. In the pharmaceutical industry, it is
used to reduce blood cholesterol levels and gastrointestinal disorders. Other applications of pectin
include use in edible films, paper substitute, foams and plasticizers, etc. In addition to pectolytic
degradation, pectins are susceptible to heat degradation during processing, and the degradation is
influenced by the nature of the ions and salts present in the system. Although present in the cell walls
of most plants apple pomace and orange peel are the two major sources of commercial pectin due to
the poor gelling behavior of pectin from other sources. This paper briefly describes the structure,
chemistry of gelation, interactions, and industrial applications soft pectin.
KEYWORDS orange peel, pectin extraction, orange essential oil

An orange, specifically, the sweet orange (Citrus sinensis (L.)) is the most commonly grown tree fruit in
the world. The present work addresses to the development of the part of the process needed for the
extraction of value added products like orange oil and pectin from orange peel, which is the waste of
orange juice processing industry. The outcome of the present work highlighted that the sweet orange
peels are good source of orange oil and pectin and does have the potential to become important raw
material for food processing industries. Two methods namely simple distillation & leaching have been
explored for separation of oil from peels. The remains of cake in this part is further treated for
isolation of pectin. It is found from the experimental observations that the peel source, for extraction
of pectin, when taken after extracting orange oil through simple distillation gives higher yield than
leaching residue. It is concluded that the process in which orange oil is first extracted using technique
of simple distillation followed by acid extraction of pectin is most suitable for industrial production for
isolation of pectin. These results demonstrate the successful extraction of orange oil and pectin,
providing potential benefits for industrial extraction of pectin from an economic and environmental
point of view.

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2 Introduction
An orange, specifically, the sweet orange (Citrus sinensis (L.)) is the most commonly grown tree fruit in
the world. Orange trees are widely cultivated in tropical and subtropical climates for the sweet fruit,
which is peeled or cut (to avoid the bitter rind) and eaten whole, or processed to extract orange juice,
& also for the fragrant peel. Citrus fruits are at the top not only in total production, but also in
economic value. The albedo is the main source of pectin. Pectin includes all the esterified
polygalacturonic acids at different degree of neutralization. In the presence of saccharine and small
quantities of organic acids (usually citric acid), pectins gelatinized, and this property is exploited by the
agrochemistry and pharmaceutical industries for pectin isolation. Orange essential oil is present in
small ductless gland contained in the peel of the orange fruits. The main constituent of orange peel
essential oil is d-limonene (present to the extent of at least 90 %), which is the only hydrocarbon
present. The d-limonene is extracted from orange rinds or solids. The rinds and pulp are sent to an
evaporator and the d-limonene is steamed out. It is widely known for its pleasant scentand degreasing
properties. d-limonene is currently being used in many applications such as chlorinated solvents
replacements, hand cleaners and sewage treatments. The orange processing industry can get a
complete makeover if due importance is given for separation of useful ingredient from orange peel.
Researchers and Scientists have been working on the separation of oil and pectin from orange peel
and reporting their findings in journals of repute. A brief summary includes orange peel: organic waste
or energetic resource, Waste to wealth: Industrial raw materials potential of peels of Nigerian sweet
orange (Citrus sinensis), method of distilling a volatile constituent from liquid mixture, Optimization of
pectin acid extraction from passion fruit peel (Passifloraedulisflavicarpa) using response surface
methodology, Extraction and Qualitative Assessment of African Sweet Orange Seed Oil ,Comparisons
between different techniques for waterbased extraction of pectin from orange peels , microwave-
assisted Isolation of essential oil of CinnamomuminersReinw. exl: Comparison with Conventional
hydrodistillation), Microwave-assisted extraction of pectin from orange peel, microbial production of
pectin from Citrus peel, Optimization of Pectin Extraction from Peel of Dragon Fruit
(Hylocereuspolyrhizus)(10), Determining the Yield and Quality of Pectin from Fresh Peel & Pectin
Pomace and Microbial Production of Pectin from Citrus Peel.

The present work explored the possibility of separation of essential oils and pectin from the orange
peels. Nagpur is major orange producing centre in the subcontinent and even recognised in the name
of oranges as, Orange city.

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3 Peinct

What is pectin?

A natural ingredient for every application needs

Chemically, pectin consists of the partial methyl esters of polygalacturonic acid and their salts (sodium,
potassium, calcium and ammonia), with a molecular weight of up to 150,000 Daltons.

Pectin is obtained by aqueous extraction of the appropriate edible plant materials, mainly from citrus
peel and apple pomace, followed by a selective precipitation using alcohol or salts. The raw materials
used contain a large amount of pectin with superior quality and are available in sufficient quantities to
make the manufacturing process more cost effective.

Chemical Formulae - C6H10O7

Average molecular weight – 194.1394

Monoisotopic molecular weight – 194.042652674

IUPAC name – (2S,3R,4S,5R,6R) 3,4,5,6 –tetrahydroxyoxane 2-carboxylic acid.

Pectin is usually classified according to the degree of methoxylation (DM). The degree of
methoxylation is expressed as a percentage of esterified galacturonic acid units to total galacturonic
acid units in the molecule of pectin.

Pectin produced by the normal extraction process contains more than 50% of methoxyl groups and is
classified as high methoxyl (HM) pectin.

Fig no1: HM pectin

Modification of the extraction process, or continued acid treatment, will yield conventional low
methoxyl (LMC) pectin with less than 50% methoxyl groups.

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 Fig no 2: LMC pectin

Some pectin can be treated during manufacture with ammonia to produce amidated low methoxyl
(LMA) pectin with less than 50% methoxyl groups and from 5 to 25% of amidated groups.

Fig no 3:LMA pectin

4Commercial classification

Pectin is classified according to the degree of methoxylation (DM) as high methoxyl pectin (DM >50)
and low methoxyl pectin (DM <50).
The degree of methoxylation influences the properties of pectin, especially the solubility and the gel
forming characteristics.

HM pectins are capable of forming gels in aqueous systems with high contents of soluble solids and
low pH values.

LM pectins are characterised by their ability to form gels in the presence of bivalent salts, normally
Ca++ ions, in systems with low solids content and a wide pH range.

Pectin is classified by International Numbering System as E440(i) for high methoxyl pectin and
conventional low methoxylpectins and E440(ii) for amidated low methoxyl pectin.

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 Fig no 4: Pectin classification

(fromAncient Greek: πηκτικόςpēktikós, "congealed, curdled") is a structural heteropolysaccharide

contained in the primary cell walls of terrestrial plants. It was first isolated and described in 1825 by
Henri Braconnot.

It is produced commercially as a white to light brown powder, mainly extracted from citrus fruits, and
is used in food as a gelling agent, particularly in jams and jellies. It is also used in fillings, medicines,
sweets, as a stabilizer in fruit juices and milk drinks, and as a source of dietary fiber.

Pectin is a natural product which can be found in the cell walls of all higher plants and it has long been
used for its gel formation, thickening and stabilising properties in a wide range of applications from
food to the pharmaceutical and cosmetic industries.

Pectin was first isolated and described in 1825 by Henri Braconnot, though the action of pectin to
make jams was known long before this date. To make good jam from fruit that has poor quality pectin,
pectin-rich fruits or their extracts were mixed into the recipe. During industrialisation, the makers of
fruit preserves soon turned to producers of apple juice to obtain dried apple pomace that was then
cooked to extract pectin. In the 1920s and 1930s, factories were built that commercially extracted
pectin from dried apple pomace and later citrus peel.

At first pectin was sold as a liquid extract, but then as a dried powder which is easier to store and
handle than a liquid.

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5 The role of pectin in plants

Pectin has an important influence on the middle lamella between plant cells since protopectin,
insoluble pectin, and cellulose form the structure of the cell walls, binding cells together and
controlling the water in the plant. The amount of time needed for extraction, the structure and
chemical composition of the pectin differs between plants, within a plant over time and in different
parts of a plant.

During ripening, pectin is broken down by the enzymes pectinase and pectinesterase. In this process
the fruit becomes softer as the middle lamella breaks down and cells become separated from each
other.

6 Natural and healthy pectin

Pectin is a natural part of human diet, being present in fruits and vegetables, but does not contribute
significantly to nutrition. Pectin passes through the small intestine more or less intact. Pectin is
therefore a highly sophisticated stabiliserrecognised globally by consumers as label friendly and as one
of the most important sources of dietary fibre.

Consumption of pectin has been shown to reduce blood cholesterol levels. The mechanism appears to
be an increase of viscosity in the intestinal tract, leading to a reduced absorption of cholesterol from
bile or food. In the large intestine and colon, microorganisms degrade pectin and liberate short-chain
fatty acids that have a positive influence on health (prebiotic effect).

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Chemical Formula:

Fig no 5: Chemical formulae for pectin

Synonyms
Description

Pectin is a long chain of pectic acid and pectinic acid molecules. Because these acids are sugars,
pectin is a polysaccharide. It is prepared from citrus peels and the remains of apples after they are
squeezed for juice.
In the plant, pectin is the material that joins the plant cells together. When fungus enzymes break
down the pectin in fruit, the fruit gets soft and mushy.

6.1 Biology

In plant biology, pectin consists of a complex set of polysaccharides (see below) that are present in
most primary cell walls and are particularly abundant in the non-woody parts of terrestrial plants.
Pectin is a major component of the middle lamella, where it helps to bind cells together, but is also
found in primary cell walls.

The amount, structure and chemical composition of pectin differs among plants, within a plant over
time, and in various parts of a plant. Pectin is an important cell wall polysaccharide that allows primary
cell wall extension and plant growth. During fruit ripening, pectin is broken down by the
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enzymespectinase and pectinesterase, in which process the fruit becomes softer as the middle
lamellae break down and cells become separated from each other.[4] A similar process of cell
separation caused by the breakdown of pectin occurs in the abscission zone of the petioles of
deciduous plants at leaf fall.[citation needed]

Pectin is a natural part of the human diet, but does not contribute significantly to nutrition. The daily
intake of pectin from fruits and vegetables can be estimated to be around 5 g (assuming consumption
of approximately 500 g fruits and vegetables per day).

In human digestion, pectin binds to cholesterol in the gastrointestinal tract and slows glucose
absorption by trapping carbohydrates. Pectin is thus a soluble dietary fiber.

Consumption of pectin has been shown to reduce blood cholesterol levels. The mechanism appears to
be an increase of viscosity in the intestinal tract, leading to a reduced absorption of cholesterol from
bile or food.[5] In the large intestine and colon, microorganisms degrade pectin and liberate short-
chain fatty acids that have positive influence on health (prebiotic effect).

6.2 Chemistry

Pectins, also known as pectic polysaccharides, are rich in galacturonic acid. Several distinct
polysaccharides have been identified and characterised within the pectic group. Homogalacturonans
are linear chains of α-(1–4)-linked D-galacturonic acid. Substituted galacturonans are characterized by
the presence of saccharide appendant residues (such as D-xylose or D-apiose in the respective cases of
xylogalacturonan and apiogalacturonan) branching from a backbone of D-galacturonic acid residues.
Rhamnogalacturonan I pectins (RG-I) contain a backbone of the repeating disaccharide: 4)-α-D-
galacturonic acid-(1,2)-α-L-rhamnose-(1. From many of the rhamnose residues, sidechains of various
neutral sugars branch off. The neutral sugars are mainly D-galactose, L-arabinose and D-xylose, with
the types and proportions of neutral sugars varying with the origin of pectin.

Another structural type of pectin is rhamnogalacturonan II (RG-II), which is a less frequent, complex,
highly branched polysaccharide. Rhamnogalacturonan II is classified by some authors within the group
of substituted galacturonans since the rhamnogalacturonan II backbone is made exclusively of D-
galacturonic acid units.

Isolated pectin has a molecular weight of typically 60–130,000 g/mol, varying with origin and
extraction conditions.

In nature, around 80 percent of carboxyl groups of galacturonic acid are esterified with methanol. This
proportion is decreased to a varying degree during pectin extraction. The ratio of esterified to non-
esterified galacturonic acid determines the behavior of pectin in food applications. This is why pectins
are classified as high- vs. low-ester pectins (short HM vs. LM-pectins), with more or less than half of all
the galacturonic acid esterified.

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The non-esterified galacturonic acid units can be either free acids (carboxyl groups) or salts with
sodium, potassium, or calcium. The salts of partially esterified pectins are called pectinates, if the
degree of esterification is below 5 percent the salts are called pectates, the insoluble acid form, pectic
acid.

Some plants such as sugar beet, potatoes and pears contain pectins with acetylated galacturonic acid
in addition to methyl esters. Acetylation prevents gel-formation but increases the stabilising and
emulsifying effects of pectin.

Amidated pectin is a modified form of pectin. Here, some of the galacturonic acid is converted with
ammonia to carboxylic acidamide. These pectins are more tolerant of varying calcium concentrations
that occur in use.

To prepare a pectin-gel, the ingredients are heated, dissolving the pectin. Upon cooling below gelling
temperature, a gel starts to form. If gel formation is too strong, syneresis or a granular texture are the
result, whilst weak gelling leads to excessively soft gels. Pectins gel according to specific parameters,
such as sugar, pH and bivalent salts (especially Ca2+).

In high-ester pectins at soluble solids content above 60% and a pH-value between 2.8 and 3.6,
hydrogen bonds and hydrophobic interactions bind the individual pectin chains together. These bonds
form as water is bound by sugar and forces pectin strands to stick together. These form a 3-
dimensional molecular net that creates the macromolecular gel. The gelling-mechanism is called a
low-water-activity gel or sugar-acid-pectin gel.

In low-ester pectins, ionic bridges are formed between calcium ions and the ionised carboxyl groups of
the galacturonic acid. This is idealised in the so-called “egg box-model”. Low-ester pectins need
calcium to form a gel, but can do so at lower soluble solids and higher pH-values than high-ester
pectins. Normally low-ester pectins form gels with a range of pH from 2.6 to 7.0 and with a soluble
solids content between 10 and 70%.

Amidatedpectins behave like low-ester pectins but need less calcium and are more tolerant of excess
calcium. Also, gels from amidated pectin are thermo-reversible; they can be heated and after cooling
solidify again, whereas conventional pectin-gels will afterwards remain liquid.

High-ester pectins set at higher temperatures than low-ester pectins. However, gelling reactions with
calcium increase as the degree of esterification falls. Similarly, lower pH-values or higher soluble solids
(normally sugars) increase gelling speed. Suitable pectins can therefore be selected for jams and for
jellies, or for higher sugar confectionery jellies.

Pectin is a natural product which can be found in the cell walls of all higher plants and it has long been
used for its gel formation, thickening and stabilising properties in a wide range of applications from
food to the pharmaceutical and cosmetic industries.

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Pectin was first isolated and described in 1825 by Henri Braconnot, though the action of pectin to
make jams was known long before this date. To make good jam from fruit that has poor quality pectin,
pectin-rich fruits or their extracts were mixed into the recipe. During industrialisation, the makers of
fruit preserves soon turned to producers of apple juice to obtain dried apple pomace that was then
cooked to extract pectin. In the 1920s and 1930s, factories were built that commercially extracted
pectin from dried apple pomace and later citrus peel.

7 Sources and production

Pears, apples, guavas, quince, plums, gooseberries, and oranges and other citrus fruits contain large
amounts of pectin, while soft fruits like cherries, grapes, and strawberries contain small amounts of
pectin.

Typical levels of pectin in plants are (fresh weight):

 apples, 1–1.5%
 apricots, 1%
 cherries, 0.4%
 oranges, 0.5–3.5%
 carrots approx. 1.4%
 citrus peels, 30%

The main raw materials for pectin production are dried citrus peel or apple pomace, both by-
products of juice production. Pomace from sugar beet is also used to a small extent.From these
materials, pectin is extracted by adding hot dilute acid at pH-values from 1.5 – 3.5. During several
hours of extraction, the protopectin loses some of its branching and chain length and goes into
solution. After filtering, the extract is concentrated in vacuum and the pectin then precipitated by
adding ethanol or isopropanol. An old technique of precipitating pectin with aluminium salts is no
longer used (apart from alcohols and polyvalent cations, pectin also precipitates with proteins and
detergents).

Alcohol-precipitated pectin is then separated, washed and dried. Treating the initial pectin with
dilute acid leads to low-esterified pectins. When this process includes ammonium hydroxide,
amidatedpectins are obtained. After drying and milling, pectin is usually standardised with sugar and
sometimes calcium salts or organic acids to have optimum performance in a particular application.

8 General properties of pectin

Pectins are soluble in pure water. Monovalent cation (alkali metal) salts of pectinic and pectic acids are
usually soluble in water; di- and trivalent cations salts are weakly soluble or insoluble. Dry powdered
pectin, when added to water, has a tendency to hydrate very rapidly, forming clumps. These crumps

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consist of semidry packets of pectin contained in an envelope of highly hydrated outer coating.
Further solubilisation of such crumps is very slow. Clump formation can be prevented by dry mixing
pectin powder with water-soluble carrier material or by the use of pectin having improved
dispersibility through special treatment duringmanufacturing .

Dilute pectin solutions are Newtonian but at a moderateconcentration, they exhibit the non-Newtonian,
pseudoplasticbehaviour characteristics. As with solubility, the viscosity of a pectin solution is related to
the molecular weight, DE, concentration of thepreparation, and the pH and presence of counterions in
thesolution. Viscosity, solubility, and gelation are generally related. Forexample, factors that increase
gel strength will increase the tendencyto gel, decreasesolubility, and increase viscosity, and vice
versa.These properties of pectins are a function of their structure, which isthat of a linear polyanion
(polycarboxylate). As such, monovalentcation salts of pectins are highly ionised in solution, and
thedistribution of ionic charges along the molecule tends to keep it in anextended form by reason of
coulombicrepulsion .Furthermore, this same coulombic repulsion between thecarboxylate anions
prevents aggregation of the polymer chains. (Thenumber of negative charges is, of course, determined
by the DE.) Inaddition, each polysaccharide chain, and especially eachcarboxylate group, will be highly
hydrated. Solutions of monovalent salts of pectins exhibit stable viscosity because each polymer chainis
hydrated, extended, and independent.

As the pH is lowered, ionisation of the carboxylate groups issuppressed, and this results in a reduction
in hydration of thecarboxylic acid groups. As a result of reduced ionisation, thepolysaccharide
molecules no longer repel each other over theirentire length, and as a result, they can associate and
form a gel.Apparent pK-values (pH at 50% dissociation) vary with the DE ofthepectin a 65% DE pectin
has anapparent pK of 3.55, while a 0% DE pectic acid has an apparentpK of 4.10. However, pectins
with increasingly greater degrees ofmethylation will gel at somewhat higher pH, because they have
fewercarboxylate anions at any given pH.
Dissolved pectins are decomposed spontaneously bydeesterification as well as by depolymerisation;
the rate of thisdecomposition depends on pH, on water activity, and on thetemperature. In general,
maximum stability is found at pH 4. Thepresence of sugar in the pectin solution has a certain
protective effect while elevated temperatures increase the rate of degradation. At low pH-values and
elevated temperatures degradation due tohydrolysis of glycosidic linkages is observed.
Deesterification is alsofavoured by low pH. By deesterification a HM-pectin becomes slower setting or
gradually adapts LM-pectin characteristics. Atnear-to-neutral pH (5-6), HM-pectin is stable at room
temperatureonly. As the temperature (or pH) increases, a so-called âeliminationstarts which results in
chain cleavage and very rapid loss of viscosity and gelling properties. LM-pectins show a
somewhatbetter stability at these conditions. At alkaline pH values pectin israpidly deesterified and
degraded even at room temperature.
Powdered HM-pectins slowly lose their ability to form gels if stored under humid or warm conditions
while LM-pectins are morestable and loss should not be significant after one year storage atroom
temperature .

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9 Gel formation properties of pectin

The most important use of pectin is based on its ability to form gels. HM-pectin forms gels with
sugar and acid. This can be seen as a partial dehydration of the pectin molecule to a degree where it is
in a state between fully dissolved and precipitated. The particular structure of pectin imposes some
specific constraints. HM-pectin, unlike LM-pectin, does not contain sufficient acid groups to gel or
precipitate with calcium ions, although other ions such as aluminium or copper cause precipitation
under certain conditions. It has been suggested by Oakenfullthat hydrogen bonding and hydrophobic
interactions are important forces in the aggregation of pectin molecules. Gel formation is caused by
hydrogen bonding between free carboxyl groups on the pectin molecules and also between the
hydroxyl groups of neighbouring molecules. In a neutral or only slightly acid dispersion of pectin
molecules, most of the unesterified carboxyl groups are present as partially ionised salts. Those that
are ionised produce a negative charge on the molecule, which together with the hydroxyl groups
causes it to attract layers of water. The repulsive forces between these groups, due to their negative
charge, can be sufficiently strong to prevent the formation of a pectin network. When acid is added,
the carboxyl ions are converted to mostly unionised carboxylic acid groups. This decrease in the
number of negative charges not only lowers the attraction between pectin and water molecules, but
also lowers the repulsive forces between pectin molecules. Sugar further decreases hydration of the
pectin by competing for water. These conditions decrease the ability of pectin to stay in a dispersed
state. When cooled, the unstable dispersing of less hydrated pectin forms a gel, a continuous network
of pectin holding the aqueous solution. The rate at which gel formation takes place is also affected by
the degree of esterification. A higher DE causes more rapid setting. Rapid-set pectins (i.e. pectin with a
DE of above 72%) also gel at lower soluble solids and higher levels than slow-set pectins (i.e. pectin
with a DE of 58-65%).
LM-pectins require the presence of divalent cations (usually calcium) for proper gel formation. The
mechanism of LM-pectin gelation relies mainly on the well-known ‘egg-box’ model. The mechanism
involves junction zones created by the ordered, side-by-side associations of galacturonans, whereby
specific sequences of GalA monomer in parallel or adjacent chains are linked intermolecularly through
electrostatic and ionic bonding of carboxyl groups .
It is generally accepted that the junctions consist of dimers in 21 helical symmetry, similar to the 21
model proposed for alginates . The oxygen atoms of the hydroxyl groups, the ring oxygen atoms, and
the bridging oxygen atoms of the component sugar units participate in the bonding process through
their free-electron pairs. The life of the junction depends on the strength of the electrostatic bonds.
The bonds are stable when there are at least seven consecutive carboxyl groups on the interior of each
participating chain (Powell et al., 1982). The occurrence of methyl ester groups in the primary
backbone limits the extent of such junction zones leading to formation of the gel. Other models for
LM-pectin gelation (e.g. 32 helical model) have been proposed , but they are currently unconfirmed by
experimentation. Nevertheless, all
LM-pectin gels seem to develop similar, if not identical, junction zones.
Furthermore, amidation increases or improves the gelling ability of LM-pectin: amidatedpectins need
less calcium to gel and are less prone to precipitation at high calcium levels Racape and coworkers
suggested that the gelation of amidatedpectins could not be explained by the ‘egg-box’ model alone,
as blocks of amide groups along the chain promote association through hydrogen bonding. As
UICT,NMU, Jalgaon Page 18
expected for any polymer, the lower the molecular weight, the weaker the gel.The role of pectin in
plants

Pectin has an important influence on the middle lamella between plant cells since protopectin,
insoluble pectin, and cellulose form the structure of the cell walls, binding cells together and
controlling the water in the plant. The amount of time needed for extraction, the structure and
chemical composition of the pectin differs between plants, within a plant over time and in different
parts of a plant.During ripening, pectin is broken down by the enzymes pectinase and pectinesterase.
In this process the fruit becomes softer as the middle lamella breaks down and cells become separated
from each other.

10 Natural and healthy pectin

Pectin is a natural part of human diet, being present in fruits and vegetables, but does not contribute
significantly to nutrition. Pectin passes through the small intestine more or less intact. Pectin is
therefore a highly sophisticated stabiliserrecognised globally by consumers as label friendly and as one
of the most important sources of dietary fibre. Consumption of pectin has been shown to reduce
blood cholesterol levels. The mechanism appears to be an increase of viscosity in the intestinal tract,
leading to a reduced absorption of cholesterol from bile or food. In the large intestine and colon,
microorganisms degrade pectin and liberate short-chain fatty acids that have a positive influence on
health (prebiotic effect).

10.1 High methoxyl pectin

Suitable for high sugar jams, jellies and beverages

High methoxyl pectin has a relatively high portion of the carboxyl groups as methyl esters, greater
than 50%. HM pectin can be divided into rapid set, medium rapid set and slow set pectin depending
on the setting time and temperature.

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Gels made with HM pectins have a firm and short structure, and are clear, with a good flavour release.
These gels are not heat reversible.

Apart from the setting time, HM pectins are standardised with respect to SAG grade, gel strength,
setting temperature, viscosity and protein stability depending on the final application.

The table below no 1: shows a list of the key HM pectins, produced by Silvateam.

Gel DM
Product name Description Applications
strength (%)

 High sugar jams and marmalades

Aglupectin HS-R Rapid 145 - 155 67 - 70

Medium rapid  High sugar jams

Aglupectin HS-MR 145 - 155 64 - 67
set
 Single portion jams
Aglupectin HS-S Slow set 145 - 155 58 - 64

 Confectionery jellies
Aglupectin HS-ES Extra slow set 145 - 155 50 - 58  Jams and marmalades

 High viscosity fruit beverages

Aglupectin HS-RV Rapid set N.a. 64 - 67

Aglupectin HS-  Acidic protein beverages

Rapid set N.a. 70 - 72
RAM
 Confectionery jellies
Aglupectin HS-SB Buffered slow set N.a. 58 - 64

The determination of gelling strength according to the USA-Sag method (Committee for Pectin
Standardisation, 1959).

DM: Degree of Methoxylation

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10.2 Amidated low methoxyl pectin

Suitable for low sugar jams, fruit preparations and reversible jellies in hot and cold conditions

Amidated pectin (LMA) is a low methoxyl pectin obtained from high methoxyl pectin when ammonia is
used in the alkaline de-esterification process. The degree of methoxylation (DM) and the degree of
amidation (DA) determine the calcium reactivity of this pectin. LMA pectin form spreadable, shear
reversible gels in hot and cold conditions.

The degree of amidation (DA) is expressed as a percentage of amidatedgalacturonic acid units to total
galacturonic acid units in the molecule of pectin:

 Typical DA level is from 2 or 3% to 25% (max 25% by law);

 Typical DM level is from 25% to 48%.

LMA pectins are typically standardised according to the gel strength, setting temperature and calcium
reactivity.

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 The table no 2: below shows a list of the key LMA pectins, produced by Silvateam.

Product name Description DM (%) DA (%) Applications

 Cold spreadable jellies

Aglupectin LA-S03S Amidated 40 - 48 8 - 12

 Yoghurt fruit preparations

Aglupectin LA-S05 Amidated 35 - 45 12 - 16

 Low sugar jams

 Jellies
Aglupectin LA-S10 Amidated 30 - 40 16 - 20
 Yoghurt fruit preparations

 Reversible jellies
Aglupectin LA-S10S Amidated 30 - 40 16 - 20

 Low sugar jams and jellies

Aglupectin LA-S20 Amidated 25 - 35 20 - 25  Yoghurt fruit preparations

DM: Degree of Methoxylation and DA: Degree of Amidation

10.3 Conventional low methoxyl pectin

Suitable for organic jams and bakery jams

Conventional pectin (LMC) is a low methoxyl pectin that contains less than 50% of the carboxylic acid
units esterified and forms gels only with polyvalent ions (Ca++, Mg++). LMC pectin permits to produce
brittle thermally irreversible gels.

LMC pectins are typically standardised according to the gel strength, setting temperature and calcium
reactivity

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The table no 3: below shows a list of the key LMC pectins, produced by Silvateam.

Product name Description DM (%) Applications

 Jams
Aglupectin LC-S12 Conventional 31 - 35  Yoghurt fruit preparations

 Yoghurt fruit preparations

Aglupectin LC-S18 Conventional 35 - 41  Organic jams and jellies

 Jams
 Jellies
Aglupectin LC-S22 Conventional 46 - 50
 Yoghurt fruit preparations with high solids

 Bakery jams
Aglupectin LC-BF Conventional 35 - 41

DM: Degree of Methoxylation

11 Material and Method:The present work is divided into following parts:

I. Separation of oil from peels.

a) Using the method of simple distillation

b) Using ethanol as solvent in the method of leaching

II. Extraction of pectin from oil peels

a) From fresh peels, the leftover

b) From dried cake remained after simple distillation and leaching as in part I

11.1 Separation of oil from peels:

 Raw Material:
The raw material taken under examination for the extraction of orange oil (d-limonene) and pectin
is orange peel. Orange peels are removed from fresh oranges which are procured from local market
and which were harvested in the month of December 2011 to January 2012

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  Methods:
Simple distillation is employed for removal of essential oil from orange peel. Dried and fined ground
orange peel powder is added with known quantity of water which is simple distilled off for
approximately one hour. The solid remains of the residue are dried to obtain the dry cake.

The distillate resulted in to two phases, oil and water. Two phases are separated and orange oil is
obtained. For 350 gm of orange powder taken, 8 ml of oil and 126.3 gm of dried cake is obtained. The
method of leaching is also explored for removal of oil from peels. 380 gm of fresh orange peel are
extracted with 225 ml of ethanol. After adequate contacting, two phases, solid and liquid are
separated, 198 gm of wet slurry resulted into 150 gm of dry cake. However oil could not be recovered
following this method. The dried cake obtained is further treated for separation of pectin in next part
of present work.

11.2 Extraction of pectin from orange peels:

The objective of this part of work is extraction and isolation of pectin from fresh orange peel sample
and the dry cake sample left after extraction of oil using simple distillation as in part I. The objective
includes the study of the effect of pH of the medium on the yield of pectin extracted. The process flow
chart is as shown in the figure 6.

Fig no 6 : Process flow chart for extraction of pectin from orange peel sampl

 Citric acid in distilled water solutions of desired pH values 1, 1.5, 2, 3, 4 and 5 are prepared.
UICT,NMU, Jalgaon Page 24
  Orange peel samples weighing 10 gm each are dipped in to the solution and heated at 800C for
10 minutes.
 After cooling the solution,
 it is filtered using cloth filter and Whatman filter paper under vacuum.
 Ethanol is added to the filtered solution to facilitate filtration of pectin.
 The solution is filtered using fine filter cloth or centrifuge at 8000 rpm for 15 min at 100C to
separate jelly pectin which is dried under vacuum at 500C and -100 mmHg gauge for two
hours.
 Dried pectin is thus obtained.
 The observations are given in table no 1. Yield % of pectin is based on the gram of peel sample
taken, and is calculated by formula as given below;

Y pec (%)=100×(p/BL)

whereYpec (%) is the extracted pectin yield in per cent (%), P is the amount of dry pectin in g and Bi is
the initial amount of orange peel in gram.

 Results and discussion:

The yield of pectin obtained is highest in turbid extract, but this might be due to some suspended
impurities present in the extract. The maximum overall yield of the pectin is obtained from orange
peel residue sample through simple distillation. Therefore, in the process of orange oil and pectin
extraction from orange peel, it is recommended on basis of results obtained, that to first extract oil
using simple distillation and then isolate pectin with acid hydrolysis technique.

The maximum yield of pectin is obtained at extraction medium pH of 1. However negligible yield is
obtained at pH of 4 and 5 as can be seen from graph plotted between pectin yield % obtained for
various values of pH of medium as shown in fig no 7.

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 Table no 4: Experimental observations of yield of pectin at different pH

Solution of pH pH 1 pH 1.5 pH 2 pH 3 pH 4 pH 5

Volume taken 100 100 100 100 100 100

for extraction
(ml)

Amount of 10 10 10 10 10 10
peel sample
added (g)

Extraction 80 80 80 80 80 80
temperature
(0C)

Extraction 5 5 5 5 5 5
Time (minute)

Volume 89 50 70 73 88 70
obtained after
filtration (ml)

Volume of 44.5 25 35 37 44 35
ethanol
added(ml)

Centrifuge rpm 8000 8000 8000 8000 8000 800

Centrifuge 15 15 15 15 15 15
time (minute)

Weight of 4.55 2.21 1.15 0.28 - -

dried pectin
obtained (g)

25% yield of 45.5 22 11.5 2.8 - -

pectin
obtained

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 pectin yeild (%) vs. pH
45.5

22

11.5

2.8

1 2 3 4 5 6

Fig no 7 : Pectin yield at different pH of extracting medium

11.2.1 : Comparison of yield of pectin from the dry cake residue left after simple
distillation and leaching:
Same procedure is applied for separation of pectin in this part of present work, as followed in part
1.2.2.the observations are tabulated in table 2 & pictorial details & output of process are depicted in
fig no 8:

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Fig no 8 : Pictorial presentation of the process for comparison of yield of pectin from the dry cake residue
left after
simple
distillation
and leaching

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Table no.5: Experimentel observation of comparision of yield pectin from dry cake residue left after bsimple
distillation and leaching

Peel sample Simple distillation residue Leaching residue

Amount (g) 31 86
Volume of citric acid solution ,pH 360 940
2 added (ml)
Heating Temerature (0C) 80 80
Heating time (minute) 10 10
Filtrate Extract through simple Clear pectin Turbine pectin
distillation extract extract
Filtrate volume (ml) 480 700 1100
Volume taken precipitation of 400 300 300
pectin (ml)
Equivalent amount of orange 25.83 14.33 14.33
peel for the pectin extract (g)
Volume of ethanol added (ml) 200 150 150
Weight of jelly pectin added (g) 183.6 60.8 123.8
Weight of dry pectin obtained 12 3.8 7.4
Yeild of pectin 46.46 26.52 51.64
Total pectin yield (%) 46.46 39.08

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12 Characterization of extracted pectin:The dried pectin obtained from the various peels of
the three fruits was subjected to the following qualitative and quantitative test to characterize them.

13 Qualitative tests:
• Colour:This was done by visual observation

• Solubility of dry pectin in cold and hot water:(0.25%) of the pectin samples were separately placed
in a conical flask with 10 mL of 95% ethanol added followed by 50 mL distilled water. The mixture was
shaken vigorously to form a suspension which was then heated at 85-95°C for 15 min (Fishman et al.,
1984).

• Solubility of pectin solution in cold and hot alkali (NaOH):To 1 mL and 0.1 N NaOH was added 5ml
pectin solution and then heated at 85-90°C for 15 min, (Joslyn, 1980).

• Sugar and organic acids:One gram of the pectin sample was placed separately in 500 mL flask each
and moisture with 5 mL ethanol, 100 mL water poured rapidly, shaken and allowed to stand for 10
min. To this solution, 100 mL ethanol containing 0.3 mL hydrochloric acid was added, mixed and
filtered rapidly, 2.5 mL of the filtrate was measured into a conical flask (25 mL), the liquid has
evaporated on a steam bath and the residue dried in an oven at 50°C for 2 h.

• pH determination:The choice of the pH was made by preparing a buffer at pH 7.0 and the
temperature adjusted to 28°C, the glass electrode standardized with standard buffer solution with the
electrode rinsed with distilled water before inserting into the pectin solution and pH determined read
off.

14 QUANTITATIVE TEST
• Equivalent weight determination: Pectin sample (0.5 g) was weighed into a 250 mL conical flask and
moistened with 5 mL ethanol, 1.0 g sodium chloride was added to the mixture followed by 100 mL
distilled water and few drops of phenol red indicator. Care was taken at this point to ensure that all
the pectin had dissolved and that no clumping occurred at the sides of the flask before the solution
was then slowly titrated (to avoid possible de-esterification) with 0.1 M NaoH to a pink colour at the
endpoint.

Equivalent weight was calculated using the equation below: Equivalent Weight = (Weight of Pectin
Sample / Volume of Alkali (cm3) × Molarity of Alkali) × 100%

• Methoxyl content determination: This was done by using the neutralized solution obtained during
the equivalent weight determination by the saponification of the pectin followed by titration of the
liberated acid i.e., 25 mL of 0.25 M NaOH was added to the neutralized solution used in the equivalent
weight determination. The mixture was stirred thoroughly and allowed to stand for 30 min at ambient
temperature. The percentage content was calculated using the equation below :

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 Methoxyl content % = (Volume of alkali (cm3) × Alkali × Weight / Weight of Pectin Sample (mg)) × 100

• Ash content determination:Five grams of each of the sample was accurately weighed into a
weighed empty crucible separately. The crucible was transferred to a furnace set at 60°C to burn off
all the organic matter. The carbon charred and then burnt off as carbon dioxide, leaving a dark ash;
this process lasted for 24 h. The crucible was taken out of the furnace and placed in a desiccator to
cool. The crucible after cooling was reweighed again. This was calculated using:
Ash Content (%) = (Weight of Ash / Weight of Sample) × 100
• Moisture content determination: A dried empty petri dish was dried in an oven, cooled in a
dessicator and weighed. Five grams of the pectin

samples was transferred into the crucibles in the oven which was set at 130°C for 1 h thereafter the
petri dish was removed, cooled in a dessicator and weighed. This process was repeated once. The
moisture content was calculated using:

Moisture Content (%) = (Weight of the Residue / Weight of the Sample) × 100%

Table no 6: Showing the results of the qualitative test for the three samples

Parameter Lemon Grape Sweet orange

Color Brown Brown Brown

Solubility in cold Insoluble, inubides Insoluble, inibibes, Dissolved slightly and
water smells after vigorous swells after vigorous form suspension
shaking and forms shaking, form after vigorous
suspension. suspension shaking
Solubility at 85-90°C The mixture The mixture The mixture dissolve
for 15 min dissolves dissolves
Solubility of pectin The pectin The pectin The pectin
suspension in cold suspension forms suspension forms suspension forms
alkali yellow precipitated yellow precipitate yellow precipitate
Solubility of pectin The pectin The pectin The pectin
suspension in hot suspension dissolve suspension dissolve suspension dissolved
alkali and turned milky and turned milky
Sugar and organic % % %
acid

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 Table no 7: Showing the characterized parameters for the three samples

Table 2:
Showing the
characterized (%) Lemon Orange Grape
parameters for
the three
samples S/No
1 Percentage yield 16.71 15.92 15.70
of pectin in wet
basis
2 Percentage yield 2.760 1.680 2.310
of pectin in dry
basis
3 Equivalent 694.44 534.00 293.60
weight
(mg/mol)
4 Methoxyl 4.460 5.790 3.900
content
5 Moisture 66.60 95.25 80.95
content
6 Ash content 30.00 35.00 34.50
7 pH 4.100 3.600 4.000

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15 Application of pectin-

(1) Pectin is traditionally used as a gelling agent in a wide range of fruit-based products,such
as jams, marmalades, jellies, fruit preparations for yoghurts and desserts and fruit filling for
bakery products.

(2) Pectin can be used to improve the mouth-feel and the pulp stability in juice based
drinks and as a stabiliser in acidic protein beverages.

(3) Pectin also reduces syneresis in jams and marmalades and increases the gel strength of
low calorie jams.

(4)Pectin is used in confectionery jellies to give a good gel structure and a clean bite.

(5)The typical dosage of pectin in food applications is between 0.5 - 1.0%.

(6) Besides its use in the food industry, pectin is also used in pharmaceutical and cosmetic
products.

Pectin is one of the most versatile stabilizers available. Its gelling, thickening and stabilizing
attributes makes is an essential additive in the production of many food products.

Traditionally, pectin was primarily used in the production of jams and fruit jellies -
industrially as well as domestically and in low as well as high sugar products. It secures the
desired texture, limits the creation of water/juice on top of the surface as well as an even
distribution of fruit in the product. With the change in lifestyle pectin is primarily sold for
industrial use. In some European markets it is still sold to the consumers as an integrated
component in gelling sugar, though.
Product and application development by the major pectin producers has over the years
resulted in a large expansion of the opportunities and applicability of pectin. Pectin is a key
stabilizer in many food and organic food products as well.

 Fruit applications
- Jams, jellies, and desserts

 Bakery fillings and toppings

- Fruit preparations for dairy applications

 Dairy applications
- Acidified milk and protein drinks
- Yoghurts (thickening)

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  Confectionery
- Fruit jellies
- Neutral jellies

 Beverages

 Nutritional and Health Products

 Pharmaceutical and Medical Applications

Over the years the positive public connotation of pectin has proven helpful in its widespread
use, and this may be a contributing factor to the growing interest in investigating pectin for
possible direct health benefits and thus applications in regulated non-food segment as well
as in functional foods and nutraceuticals. Pectins also find medical and pharmaceutical
applications.

This wide range of applications explains the need for many different types of commercial
pectins, which are sold according to their application, for example:

 Rapid Set pectin - traditionally used for jams and marmalades

 Slow Set Pectin - used for jellies and for some jams and preserves, especially using
vacuum cooking at lower temperatures. Also important for higher sugar products
like bakery and biscuit jams, sugar confectionery, etc.

 StabilisingPectins - used for stabilising acidic protein products such as yoghurts,

whey and soya drinks against heat processing.

 Low methyl ester and amidatedpectins - used in a wide range of lower sugar
products, reduced sugar preserves, fruit preparations for yoghurts, dessert gels and
toppings, and savoury applications such as sauces and marinades. Can also be used
in low acid high sugar products such as preserves containing low acid fruits (figs,
bananas) and confectionery.

15.1 Pharmaceutical uses of pectin

Pectin has applications in the pharmaceutical industry. Pectin favaorably influences

cholesterol levels in blood. It has been reported to help reduce blood cholesterol in a wide
variety of subjects and experimental conditions as comprehensively reviewed (Sriamornsak,
2001). Consumption of at least 6 g/day of pectin is necessary to have a significant effect in
cholesterol reduction. Amounts less than 6 g/day of pectin are not effective (Ginter et al.,
1979). Mietinnen&Tarplia (1977) reported a 13% reduction in serum cholesterol within 2
weeks of treatment.
Pectin acts as a natural prophylactic substance against poisoning with toxic cations. It
has been shown to be effective in removing lead and mercury from the gastrointestinal tract
and respiratory organs (Kohn, 1982). When injected intravenously, pectin shortens the
coagulation time of drawn blood, thus being useful in controlling hemorrhage or local

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bleeding (Joseph, 1956). Pectin and combinations of pectin with other colloids have been
used extensively to treat diarrheal diseases, especially in infants and children. Although a
bactericidal action of pectin has been proposed to explain the effectiveness of pectin
treating diarrhea, most experimental results do not support this theory. However, some
evidence suggests that under certain in-vitro conditions, pectin may have a light
antimicrobial action toward Echerichia coli (Thakur et al., 1997).
Pectin reduces rate of digestion by immobilising food components in the intestine. This
results in less absorption of food. The thickness of the pectin layer influences the absorption
by prohibiting contact between the intestinal enzyme and the food, thus reducing the
latter’s availability (Wilson &Dietschy, 1974; Dunaif&Schneeman, 1981; Flourie et al., 1984).
Due to its large waterbinding capacity, pectin gives a feeling of satiety, thus reducing food
consumption. Experiments showed a prolongation of the gastric emptying half-time from 23
to 50 minutes of a meal fortified with pectin (Holt et al., 1979). These attributes of pectin
are used in the treatment of disorders related to overeating (Di Lorenzo et al., 1988).
Pectin hydrogels have been used in tablet formulations as a binding agent (Slany et al.,
1981a,b) and have been used in controlled-release matrix tablet formulations (Krusteva et
al., 1990; Naggar et al., 1992). Recently, Sungthongjeen et al. (1999) have investigated HM-
pectins for their potential value in controlledrelease matrix formulations. The application of
a binary polymer system, i.e. HM-pectin and hydroxypropyl methylcellulose, in drug release
rate modulation for oral administration was studied by Kim &Fassihi (1997a,b,c). Pectin
beads prepared by the ionotropic gelation method (Aydin &Akbuga, 1996) were used as a
sustained release drug delivery system. However, the use of these beads has some
drawbacks due to their rapid in-vitro release. By changing the DE of LM-pectin,
Sriamornsak&Nunthanid (1998) modified the drug release pattern from calcium pectinate
gel beads.
Since pectin can react with calcium ions, calcium pectinate has been investigated as an
insoluble hydrophilic coating for sustained release delivery by interfacial complexation
process (Sriamornsak 1996; Sriamornsak et al., 1997a,b). The spherical pellets, which
contain calcium acetate, were prepared using an extrusionspheronisation method and then
coated in a pectin solution. An insoluble and uniform coating of calcium pectinate gel was
formed around the pellets. The use of pectin to develop other oral controlled release drug
delivery systems has been reported by some authors (Table 1).
Pectin has a promising pharmaceutical uses and is presently considered as a carrier
material in colon-specific drug delivery systems (for systemic action or a topical treatment
of diseases such as ulcerative colitis, Crohn’s disease, colon carcinomas), as indicated by the
large number of studies published over the last few years (Table 2). The potential of pectin
or its salt as a carrier for colonic drug delivery was first demonstrated by two studies, i.e.
Ashford et al. (1993) and Rubinstein et al. (1993). The rationale for this is that pectin and
calcium pectinate will be degraded by colonic pectinolytic enzymes (Englyst et al., 1987), but
will retard drug release in the upper gastrointestinal tract due to its insolubility and because
it is not degraded by gastric or intestinal enzymes (Sandberg et al., 1983). Rubinstein et al.
(1992) demonstrated that pectin-degrading bacteria, Klebsiellaoxytoca, could adhere to a
film casted of low methoxylated pectin. The ability of the bacteria to adhere to the films,
however, was not correlated with their ability to degrade pectin. When the dissolution of
pectin matrix tablets was analysed with and without K. oxytoca, a significant retardation in
the dissolution rate was observed in the presence of K. oxytoca, suggesting the formation of
a biofilm on the matrix or sedimentation of insoluble pectin salts.

UICT,NMU, Jalgaon Page 35

 Pectin is an interesting candidate for pharmaceutical use, e.g. as a carrier of a variety of
drugs for controlled release applications. Many techniques have been used to manufacture
the pectin-based delivery systems, especially ionotropic gelation and gel coating. These
simple techniques, together with the very safe toxicity profile, make pectin an exciting and
promising excipient for the pharmaceutical industry for present and future applications.

15.2 Medicinal application of pectin

Insufficient Evidence for :

 Diarrhea in young children. Pectin seems to shorten bouts of diarrhea

andvomiting and lessen the need for replacement fluids in children aged 5-12
months from developing nations who experience ongoing diarrhea.
 Prostate cancer. Early research suggests that taking a specific modified citrus pectin
product (Pectasol by Econugenics) after prostate surgery or radiationmight
lengthen the time to prostate cancer recurrence.
 Colon cancer.
 Diabetes.
 Infection.
 Mouth and throat sores.
 Damage from radiation.
 Heartburn.
 Other conditions.
More evidence is needed to rate pectin for these uses.

16 Result and discussion:

The yield of pectin obtained is highest in turbid extract, but this might be due to some
suspended impurities present in the extract. The maximum overall yield of the pectin is
obtained from orange peel residue sample through simple distillation. Therefore, in the
process of orange oil and pectin extraction from orange peel, it is recommended on basis of
results obtained, that to first extract oil using simple distillation and then isolate pectin with
acid hydrolysis technique.

17 Conclusion
Over the years the positive public connotation of pectin has proven helpful in its
widespread use and this may be a contributing factor to the growing interest in investigating
pectin for possible direct
health benefits and thus applications in regulated non-food segment as well as in functional
foods and nutraceuticals. Dealing with various sources, it has been found that pectin can
easily be obtained from various natural sources but good and high grade of yield depends
upon some major sources. Conventionally, various extraction procedures used have

UICT,NMU, Jalgaon Page 36

reported different percentage yield, but still the most reliable remains Soxhlet water based
extraction. Pectin finds enormous number of applications such as mucoadhesive polymer,
gelling agent and also in medical and pharmaceutical field. This wide range of applications
explains the need for many different types of commercial pectins, which are sold according
to their application, grade and quality.

Nagpur region is well known in central Asia as largest orange producing region.It is also
known as the California of India, producing excellent quality oranges in large
number.Though it has great production of oranges, the downstream processing and value
added product manufacturing technology is not yet developed.The present work is
dedicated for the development of the part of the process technology needed for the
extraction of value added products i.e. orange oil and pectin from orange peel, which is the
waste of orange juice processing industry.

The present work revealed that the sweet orange peels are good source of orange oil and
pectin and does have the potential to become important raw material for food processing
industries.It is found from the experimentation that the peel source, for extraction of pectin,
when taken after extracting orange oil through simple distillation gives higher yield than
leaching residue.So it can be concluded that the process in which orange oil is first extracted
using technique of simple distillation followed by acid extraction of pectin is most suitable
for industrial production.These results demonstrate the successful extraction of orange oil
and pectin, providing potential benefits for industrial extraction of pectin from an economic
and environmental point of view.

Acknowledgement
Authors are highly thankful to Department of Pharmaceutical Technology, Meerut Institute of
Engineering and Technology, Meerut and Advance Group of Pharmacy Colleges, Kanpur for
providing necessary facilities.

UICT,NMU, Jalgaon Page 37

18 References

1. Martín M.A, Siles J.A.1, El Bari H, Chica A. F, Université Ibn Tofail. Faculté dos Sciences.
Kenitra (Maroc) .(2008). Orange Peel: Organic Waste or Energetic Resource?

2. Tobias I. NdubuisiEzejiofor, N. V. Eke, R. I. Okechukwu, R. N. Nwoguikpe and C. M. Duru.

(2011) Waste to wealth: Industrial raw materials potential of peels of Nigerian sweet orange
(Citrus sinensis). African Journal of Biotechnology Vol. 10(33), pp. 6257-6264.
3. Gorden P. Gerow, Davenport, Fla.(1982). Method Of Distilling A Volatile Constituent From
Liquid Mixture.
United States Patent, 4,326,926.

4. Erika Kliemann, Karina Nunes de Simas, Edna R. Amante, ElaneSchwindenPrudeˆncio,

Reinaldo F. Teo´ filo, Ma´ rcia M. C. Ferreira & Renata D. M. C. Amboni. (2009). optimisation
of pectin acid extraction from passion fruit peel (Passifloraedulisflavicarpa) using response
surface methodology. International Journal of Food Science and Technology, 44, 476–483.
5. Nwobi BE, Ofoegbu O & O B Adesina. (2006). Extraction And Qualitative Assessment Of
African Sweet Orange Seed Oil
. African Journal of food agriculture nutrition and development. Vol. 6 ISSN 1684-5374.

6. S. Yeoh, J. Shi, T.A.G. Langrish. (2008). Comparisons between different techniques for
water-based extraction of pectin from orange peels. Elsevier, Desalination 218, 229–237.

7. WeerachaiPhutdhawong, RungthipKawaree, SamartSanjaiya,

WayaSengpracha&DuangBuddhasukh.(2007). Microwave-Assisted Isolation of Essential oil
of innamomuminersReinw. ex Bl.: Comparison with Conventional Hydrodistillation.
Molecules ISSN 1420-3049

8. Zheng Jie, Yang Ting, Wu Qiang, Li Jing, Wang Ya- Na. (2009). Microwave-assisted
Extraction of Pectin from Orange Peel. Vol. 30, No. 20, p. 134-137.

9. P.Y. Tang, C.J. Wong and K.K. Woo. (2011). Optimization of Pectin Extraction from Peel of
Dragon Fruit (Hylocereuspolyrhizus). Asian Journal of Biological Sciences, ISSN 1996-3351,
Knowledgia Review, Malaysia, 4 (2): 189-195.

10. P. G. Crandall, R. J. Braddock, and A. H. Rouse. (1978). Determining The Yield And Quality
Of Pectin From Fresh Peel And Pectin Pomace. Proc. Fla. State Hort. Soc. 91:109-111.

11. Takuo Sakai & Minoru Okushima. (1998). Microbial Production of Pectin from Citrus
Peel.Applied and Environmental Microbiology, Vol. 39, No. 4, p. 908- 912.

12. HarshalMakode (2012).Project report submitted for B Tech to

RashtrasantTukadojiMaharaj Nagpur University,Nagpur.

13. Pektikos, Henry George Liddell, Robert Scott, "A Greek-English Lexicon", at Perseus

UICT,NMU, Jalgaon Page 38

14.Braconnot, Henri (1825) "Recherches sur un
nouvelacideuniversellementrépandudanstous les vegetaux" (Investigations into a new acid
spread throughout all plants), Annales de chimie et de physique, series 2, 28 : 173-178.
From page 178: … je propose le nom pectique, de πηχτες, coagulum, … ( … I propose the
name pectique, from πηχτες [pectes], coagulum [coagulated material, clot, or curd], … ).

15. Keppler, F; Hamilton, JT; Brass, M; Röckmann, T (2006). "Methane emissions from
terrestrial plants under aerobic conditions". Nature 439 (7073): 187–91.
doi:10.1038/nature04420. PMID 16407949.

16. Grierson, D; Maunders, MJ; Slater, A; Ray, J; Bird, CR; Schuch, W; Holdsworth, MJ;
Tucker, GA; Knapp, JE (1986). "Gene expression during tomato ripening". Philosophical
Transactions of the Royal Society, London,B 314: 399–410.

17. Sriamornsak, Pornsak (2003). "Chemistry of Pectin and its Pharmaceutical Uses: A
Review". Silpakorn University International Journal 3 (1–2): 206.

18. "Galacturonans". Complex Carbohydrate Research Centre, University of Georgia, US.

Retrieved 2010-07-23.

19. Buchanan, B. B.; Gruissem, W.; Jones, R. L. (2000). Biochemistry and Molecular Biology
of Plants. Rockville, MD USA: American Society of Plant Biologists. ISBN 0-943088-37-2.

UICT,NMU, Jalgaon Page 39