NATIONAL UNIVERSITY OF TRUJILLO

FACULTY OF AGRICULTURAL SCIENCES

PROFESSIONAL SCHOOL OF AGROINDUSTRIAL ENGINEERING

PRACTICE: PECTIN EXTRACTION

TEACHER:
ING. ASCON DIONICIO, GREGORIO MAYER

AUTHORS:
Carranza Roman, Sarita
Montenegro Balarezo, Nuria
Portilla Quiroz, Antonela
Quispe Huamán, Yennifer
Vásquez Quiroz, Wendy

CYCLE:
VII

GUADELOUPE - 2019
PECTIN EXTRACTION

INDEX

INTRODUCTION............................................................................................................................2
AIM...................................................................................................................................................2
BASIS................................................................................................................................................3
TYPES OF PECTIN ACCORDING TO THE DEGREE OF ESTERIFICATION................3
a. High Methoxyl Pectins.....................................................................................................3
b. Low Methoxyl Pectins......................................................................................................4
EVALUATION OF EXTRACTED PECTIN.............................................................................4
1. Performance (%)..............................................................................................................4
Physicochemical characterization...........................................................................................4
2. Free acidity (AL) and equivalent weight (PE) of pectin................................................4
3. Methoxyl percentage........................................................................................................5
4. Esterification degree.........................................................................................................5
5. Percentage of galacturonic anhydride acid (GAA)........................................................6
6. Apparent viscosity test.....................................................................................................6
7. Statistic analysis................................................................................................................6
USE IN INDUSTRY.....................................................................................................................6
MATERIALS AND METHODS.....................................................................................................7
1. Materials...............................................................................................................................7
1.1 Materials.......................................................................................................................7
1.2 Equipment.....................................................................................................................8
2. Methods.................................................................................................................................8
RESULTS.........................................................................................................................................9
DISCUSSIONS.................................................................................................................................9
CONCLUSIONS............................................................................................................................10
BIBLIOGRAPHIC REFERENCES.............................................................................................10
ANNEXES......................................................................................................................................11

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INTRODUCTION
Pectin is a carbohydrate (that is, a biopolymer consisting mainly of galacturonic acid), it
belongs to the family of plant hydrocolloids, therefore, it has a high molecular weight and
is present in all plants, it manifests itself in form of protopectin, accompanied by cellulose,
make up the structure of cell walls, which makes them important in terms of the influence
on plant cells, mainly in the primary wall and in the mesenchymal and parenchymatic
tissues, thus fulfilling, the function of intercellular cement.

Pectin was made known in 1825, derived from the Greek pektikos , which means to freeze
or solidify; was known as a soluble substance, which we could find in fruit juices, it is
found naturally, the amount that can be contained in each of them depends on the state of
ripeness, that is, the more ripe it is, the less Pectin contains, in general, the fruits with the
highest amount of pectin are quinces, apples (obtained from their peel and seeds) and citrus
fruits. This fiber works as a natural thickener, since when sugar joins with the acids present
in fruits, it forms gels; We have as an example, quince candy, which is noticeable when it
acquires its characteristic texture.

According to the FAO (Food and Agriculture Organization of the United Nations), pectin is
considered a food additive, it is considered essential in food processing, being the best
known in the production of jams.

The present work is based on the "Extraction of pectin from mandarin peel", where the
experimental tests aimed at the production, characterization and analysis of the quality of
pectin are analyzed and described, following some parameters already established for its
obtaining, in addition to this, we will calculate the performance obtained for its application
in a specific product.

AIM
 Know the processing flow for pectin extraction.
 Extract pectin from mandarin peel.

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 Determine the yield of pectin.

BASIS
Peptic substances are considered linear polymers of galacturonic acid, since they have a
wide range of carboxylic groups esterified by methyl radicals. We can find them in the cell
walls and in the intercellular spaces of plant tissues. The 100% methylated galacturonic
chain is called pectin, and peptide acids are those that had a methylation ratio of less than
100%; the term peptic acids refers to methyl-free polygalacturonic acids (Braverman, J.,
1987).

Figure 1. Pectin structure

In fruits, most of the acid groups of galacturonic acid are esterified by methanol; this can be
lost relatively easily by acid and enzymatic hydrolysis, thus leaving a free acid group.
Depending on the percentage of esterified galacturonic acid residues, pectins are classified
as high methoxyl when their percentage is greater than 65% and low methoxyl, when it is
lower (Carbonell, E.; Costell, E. and L. Durán., 1990).

TYPES OF PECTIN ACCORDING TO THE DEGREE OF ESTERIFICATION

a. High Methoxyl Pectins
It has a methoxyl degree of at least 70%, they form gels when adding acids and
sugars between a pH of 3.0 to 3.4 and at relatively high temperatures. The amount
of acid is proportional to the percentage of carboxyls

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b. Low Methoxyl Pectins

Those that have a methoxyl degree of at least 50%. They do not form gels in the
presence of sugar and acid but do form with calcium ions and other polyvalent
cations, the strength of the esterification bound gels. (Braverman, 1965).
EVALUATION OF EXTRACTED PECTIN
1. Performance (%)
The yield of extracted pectin is calculated on a dry basis of raw material, thus
applying the method of Seggiani et al. (2009):

Pectina pura ( g)
% de Rend= × 100 %
Peso prom . de cáscaras en base seca(g)

Where, the amount of “pure pectin” was calculated free of moisture and ash. To
determine the average moisture content, 100g of peel are dried at 100°C until
constant weight is obtained, while the ash content is obtained by calcining one gram
of pectin at 500°C for 24 hours (Chan & Choo , 2013). These determinations were
performed in quintuplicate.

Physicochemical characterization
Based on the methodology planned by Owens et al. (1952), applying it to the
treatment with higher extraction yield and to commercial pectins with slow and
rapid gelation in triplicate.

2. Free acidity (AL) and equivalent weight (PE) of pectin

It is determined by performing a titration with 0.1 mol/L NaOH. These are
calculated by relating the weight of the sample (mg) and the milliequivalents of
NaOH spent in the titration, according to the following expressions (Owens et
al. 1952):

mg componente ácido
Peso equivalente ( Pe ) =
meq ( A ) NaOH

Where:
 Meq A (NaOH): meq of NaOH used in the titration
 Acid component: mg pectin

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meq A (NaOH )
Acidez libre ( A )=
g componente ácido

Where:
 Meq A (NaOH): meq of NaOH used in the titration
 Acid component: mg pectin

3. Methoxyl percentage
It is determined with the solution used to determine the equivalent weight and
acidity, in which 0.25mol/L sodium hydroxide is added to deesterify the pectin;
The solution is neutralized with 0.25mol/L hydrochloric acid and titrated with
0.1mol/L sodium hydroxide, to determine the percentage of methoxyl, until the
color changes to reddish, which is calculated by the equation:

meq B∗31∗100
%Metoxilo ( Me )=
mg componente ácido

Where:
 31: molecular weight of methoxyl (CH 3 O) expressed in mg/meq
 Meq B: meq of NaOH used in the titration
 Acid component: Sample weight (mg)

4. Esterification degree
It is calculated by relating the meq B spent in the titration to determine the
methoxylation percentage and the sum of the total of the meq A spent in the
titration to determine the equivalent weight and meq B, according to the
equation:

meq B
%Grado de esterificacion ( ¿ )=
meq A+meq B

Where:
 Meq A: milliequivalents used in the first titration NaOH 0.1 mol/L.
 Meq B: used milliequivalents of 0.1 mol/L NaOH in the second titration to
determine the methoxyl content

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5. Percentage of galacturonic anhydride acid (GAA)

It allows us to know the degree of purity of the pectic substance, because pectin
is a polysaccharide made up not only of D-galacturonic acid, but also, in its
structure, 10% or more of the chain can represent other sugars, such as
arabinose. , glucose and rhamnose. Its determination is the free acidity and
methylated units, relating them in the equation:

176∗100∗(meq A +meq B)
%AAG=
mgcomponente ácido

Where:
 176: Molecular weight of galacturonic anhydride acid expressed in mg/meq
 meq A: milliequivalents used in the first titration with 0.1 mol/L NaOH
 meq B: milliequivalents used of 0.1 mol/L NaOH in the second titration, to
determine the methoxyl content
 Acid component: sample weight (mg)

6. Apparent viscosity test

Components are prepared, weighed and mixed with constant stirring, brought to
boiling temperature (98°C) for 45 minutes and left to rest until cooling. The
measurements are carried out in a rotational viscometer, recording 3 viscosity
measurements, every 2 minutes, at each deformation speed used.

7. Statistic analysis
The pectin extraction process is carried out in quintuplicate and is subjected to
the Kolmogorov-Smirnov test to verify its normality. Subsequently, a one-way
analysis of variance (ANDEVA) and Tukey's mean comparison tests will be
applied, at a 95% confidence level.

USE IN INDUSTRY
For industrial purposes, the sources of obtaining pectins are mainly restricted to the peels of
citrus fruits (20-35%), sunflower infructescence (15-25%), beet (10-20%) and apple pulp
( 10-15%). (Chasquibol Silva, et al, 2019)

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It is considered a functional ingredient and a source of dietary fiber, due to its ability to
form aqueous gels. These gels allow us to create or modify the texture of products, such as:
compotes, jellies, sauces, ketchup, mayonnaise, candies; In the dairy industry it is used in
the manufacture of fruity yogurts and low-fat dairy products; in the diet beverage industry
for the preparation of soft drinks, due to its low carbohydrate content, its stabilizing
properties and increasing viscosity; In the pharmaceutical industry, it is used as an
ingredient for antidiarrheals and detoxifiers and some drugs are encapsulated with a pectin
film to protect the gastric mucosa and thus allow the active component to be released into
the blood circulation. (Yamada, 1996: 173-190)

They are also used as lipoprotein absorbing agents, especially in weight loss
pharmaceuticals; His latest research is based on the application as healing biopolymeric
membranes. In addition, it reduces glucose intolerance in diabetics and even lowers the
level of blood cholesterol and the low-density lipoprotein fraction. On the other hand, it
helps in the potential inhibition of cancer and its metastasis. Specifically, studies are being
carried out on the effect of different types of pectin in inhibiting the growth of prostate
cancer and leading to dietary recommendations to combat this incidence (Heitman, D, et al,
1992).

In the case of the cosmetic industry, pectin is used in formulas for toothpastes, ointments,
oils, creams, deodorants, hair tonics, bath lotions and shampoo, due to its softening and
stabilizing properties. It is also used in the production of plastics, in the manufacture of
foaming products, as a clarifying agent and binders, and as a material for the absorption of
contaminants from liquid industrial effluents, this demonstrates its great potential
(Gierselmer, K, 1997).

MATERIALS AND METHODS

1. Materials
1.1 Materials
 Raw material: Tangerine peels (400g)
 600 ml Industrial alcohol
 1 L Distilled water

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 1N HCl (40 drops)

 Filter paper
 Pots, spoons, knives

1.2 Equipment
 Balance
 Stove
 pH-meter
 Electric kitchen
 Thermometer

2. Methods
The processing flow to obtain pectin from mandarin industrial waste is described
below.

FLOW OF OPERATION FOR OBTAINING PECTIN

PREPARATION OF RAW MATERIALS

BLEACHED
(90-95°C, t: 20 min)

EXTRACTION
(pH: 1.8, T: 70°C, t: 70 min)

FILTRATION

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COOLED
(25°C)

PRECIPITATION
(60% alcohol)

WASHED

DRYING
(T: 60°C, t: 18h)

GRINDING

SIEVED

PECTIN POWDER
Figure 2. Operation flow for the extraction of pectins from mandarin industrial
waste
RESULTS
According to our laboratory experimentation, we found the performance that our raw
material obtained at the end of the practice. For this, two formulas were used, which are
described in the Annexes.

Table 1
Experimental data from practice
Shell weight (g) Pectin weight (g) % Humidity Performance (%)
400g 3g 99.25 % 0.75 %

Source: self made

DISCUSSIONS
According to Herbstreith & Fox (2001), it tells us that the highest yield is obtained when
acidulated water with HCl is used, whose values can be obtained when the fruit is in a state
of green ripening, the most common is to extract it from the apple or other citrus peels, this
may vary depending on the degree of maturity of the fruit, the extraction process and
storage conditions of the pectin obtained are also taken into account. This agrees with our
result, we can notice that the degree of maturity of the fruit had a great influence on the
calculation of the results, the pH range was 1.8 and the extraction temperature was 70°C,

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thanks to this we managed to obtain a acceptable result in terms of the amount of pectin
obtained, thus avoiding non-enzymatic browning processes due to the Maillard reaction.

According to Espinal et al (2005), the yield of pectin in the orange seed is 6%, in the peel it
is around 30% and in the juice 25%, all of the mentioned being obtained on a dry basis and
in comparison With the results obtained in our practice (determined on a wet basis), we can
say that the extraction of pectin from mandarin peels is considerable, since the highest
concentration of pectin is found at that point, this can be used as an additive for the
production of various products belonging to the food industry.

CONCLUSIONS
We were able to determine the yield of pectin from the tangerine peel, the result was
0.75%; We must take into account that it has the ability to form gels, which is why it is
used as a thickening agent.

For the extraction of pectin we must take into account: quality control of the raw material,
acid hydrolysis, evaporation, drying and grinding. Therefore, according to bibliographic
sources, they tell us that the extraction of pectin with low pH and low temperature will have
a higher yield, and at high pH, the yield will be lower. This is because pectin is susceptible
to enzymatic degradation, and this means that it can be extracted more easily and in a
greater proportion.

BIBLIOGRAPHIC REFERENCES
BRAVERMAN, J.B.S. (1987). “Introduction to Food Biochemistry” Ed. Acribia. Zaragoya
– Spain.

CARBONELL, E.; COSTELL, E. And L. DURAN. “Determination of pectin content in

vegetable products.” Rev. Agroquím. Technol. Feed 30, 1990.

CHAN, S.-Y.; CHOO, W.-S. 2013. Effect of extraction conditions on the yield and
chemical properties of pectin from cocoa husks. Food Chemistry. (UK).
141(4):3752-3758.

CHASQUIBOL SILVA, N., ARROYO BENITES, E., & MORALES GOMERO, J. (2019).
Extraction and characterization of pectins obtained from fruits of Peruvian

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biodiversity. Retrieved from

http://revistas.ulima.edu.pe/index.php/Ingenieria_industrial/article/view/640/621.

ESPINAL CF, MARTÍNEZ HJ, PEÑA Y. The citrus chain in Colombia: A global look at
its structure and dynamics 1991-2005. Bogotá: Ministry of Agriculture and Rural
Development, Agrocadenas Colombia Observatory. [Internet site]. Available at:
http://www.agrocadenas.gov.co. Consulted: March 15, 2005.

GIERSELMER, K. “Pectin and pectin enzymes in fruits.” Vegetables technology 118,

1997.

HEITMAN, D. W.; HARDMAN, W. AND. And I. L. CAMERON. “Dietary

supplementation with pectin and guar gum on 1,2-dimethylhydrazine-induced colon
carcinogenesis in rats.” Carcinogenesis 13, 1992.

HERBSTREITH & FOX. (2001). The Specialists for Pectins. http://www.herbstreith-

fox.de/produkte/ englisch/einstant.htm (Feb 10 2001).

OWENS, HS; MCCREADY, RM; SHEPHERD, AD; MIERS, JC; EARLANDSED, RF;
MACLAY, W.D. 1952. Methods used at western regional research laboratory for
extraction and analysis of pectic materials. Book, Albany, California: AIC-340,
Western, Regional Research Laboratory

SEGGIANI, M.; PUCCINI, M.; PIERINI, M.; GIOVAndo, S.; FORNERIS, C. 2009. Effect
of different extraction and precipitation methods on yield and quality of pectin. Int.
J. Food Sci. Technol. (UK). 44(3):574- 580.

YAMADA, H. Contributions of pectins on health care. Pectins and pectinases: proceedings

of an international symposium. Wageningen, Netherlands, December 3-7, 1995.
Edited by Visser J, Voragen AGJ. Amsterdam: Elsevier, 1996.

ANNEXES
Calculation of yield (%) of pectin:
Pf
Rendimiento= ×100
Pi

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3
Rendimiento= ×100=0.75 %
400

Where:
Pf : Final weight of dry pectin
Pi : Initial sample weight

Calculation of moisture (%) of tangerine peel:

P i−Pf
Humedad (% )= ×100
Pi
400−3
Humedad ( % )= ×100=99.25 %
400

Figure 2. Pectin extraction after precipitation

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Figure 3. Pectin obtained after drying.

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