Indian Journal of Natural Products and Resources

Vol. 5(2), June 2014, pp. 184-189

Optimization of method for extraction of pectin from apple pomace

PC Sharma1, Anil Gupta2* and P Kaushal2
1
Horticultural Crop Processing, CIPHET-Abohar, Punjab, India
2
Department of Food Science and Technology, Dr Y S Parmar University of Horticulture and Forestry,
Nauni, Solan–173 230, Himachal Pradesh, India
Received 7 June 2013; Accepted 24 July 2014

Method for extraction of pectin from apple pomace-waste generated from apple juice processing industries for
commercial adoption was optimized. Fresh pomace yielded 13.3% pectin on dry weight basis (dwb). Blanching of pomace
(boiling at 95oC for 5 minutes followed by cooling) and drying (at 50±2oC) was found to be a necessary pretreatment before
pectin extraction. Among different methods of pectin extraction and precipitation, extraction of apple pomace by using
0.05N HCl at 95oC for one hour followed by precipitation in 95% ethanol was found optimum with pectin yield of 10.5% on
dry weight basis. The resultant pectin was characterized by 59.1% anhydrogalacturonic acid content, 71.2% degree of
esterification (DE) and 110 jelly grade. Water and Ammonium Oxalate-oxalic acid extractions on the other hand yielded
very low 3.4 and 8.0% pectin, respectively. Sequential combination extractions, viz. water and acid or water and ammonium
oxalate-oxalic acid though yielded slightly higher amount of pectin yet the addition of a unit operation along with
comparatively low increase in pectin yield was found to limit their use for pectin extraction. Among precipitation methods,
precipitation of extract in 95% ethanol resulted in higher pectin yield with comparable quality of the pectin obtained by
using aluminium chloride precipitation. The cost of production of pectin calculated on the basis of input used and after
adding labour and processing charges worked out to be Rs. 808.30 per kg. The standardized method of pectin extraction and
precipitation can be used commercially by the processing industries for utilization of apple pomace.

Keywords: Apple pomace, Blanching, Pectin extraction, Waste utilization.

IPC code; Int. cl. (2014.01)−A61K 36/00

Introduction and crude fibre (16.16%)1 with a very high biological

Apple (Malus x domestica Borkh.) is an important oxygen demand i.e. 240-19000 mg/L2. Apple pomace
fruit crop of the world. In India, it is predominantly reported to contain about 18-19% pectin on moisture
grown in Jammu and Kashmir, Himachal Pradesh and free basis3. Pectin extraction from apple pomace is
Uttarakhand and has a large contribution towards the considered a reasonable way of utilizing it in the
economy of these hill states. A substantial quantity of technologically developed countries of the world3,4.
the apple produce is processed into juice, pulp, Pectin is a plant polysaccharide present in the middle
concentrate and other processed products and apple lamella of all plant primary cell walls including apple.
pomace is the major by-product left after extraction of It is used as a gelling agent, thickener, emulsifier and
apple juice. It is estimated that more than 10,000 stabilizer in a large number of food products such as
tonnes of apple pomace is being generated as a waste jams, jellies, fruit conserves, bakery and
in India. Since apple pomace is highly biodegradable, confectionary products, beverages, etc5,6 as well as in
its disposal near the processing units leads to pharmaceuticals and cosmetics besides possessing
environmental pollution besides causing a huge some medicinal benefits7. Various studies conducted
economic loss to the processing industry. Although on extraction of pectin from apple pomace3,4,8,10,11
efforts have been made to utilize apple pomace for mainly focused on fresh apples as the raw material
making edible products, but have not yet proven which are also suitable for table purpose. While in
fruitful for its commercial utilization. Apple pomace India very small, deformed and pitoo sized fruits (not
is a rich source of sugars (17.35%), pectin (16.95%) otherwise fit for fresh market) are used for processing.
——————
A huge quantity of pomace produced during
*Correspondent author processing goes waste due to non availability of
E-mail: [email protected] literature on feasibility of such raw material (pomace)
 SHARMA et al: OPTIMIZATION OF EXTRACTION METHOD OF PECTIN FROM APPLE POMACE 185

for pectin extraction. Further, the pectin extraction ethanol and dried in an oven at 50oC. The dried pectin
methods12,13 are quite generalized for direct from both the methods of precipitation was packed in
application in apple pomace utilization. The huge polythene pouches and stored in a cool dry place until
demand for pectin in the processed food industry in further analysis. For optimization of pretreatment of
developing countries including India is met mainly by apple pomace, acid extraction followed by alcoholic
importing it from Europe and USA. Although precipitation method was followed.
substantial amount of raw material is available in
India, industries for production of pectin from apple Physico-chemical analysis
pomace have not yet been established mainly due to Apple pomace was analyzed for different
lack of proper technology in this direction. physico-chemical attributes such as moisture, ash,
The present study was therefore, conducted to total soluble solids (TSS), titratable acidity, sugars,
investigate the effect of various extraction variables, ascorbic acid, crude fibre and pectin content
viz. pretreatment of raw material, extraction and (as calcium pectate) as per method described by
precipitation methods on the yield and quality of Ranganna15. The extracted pectin was analyzed for
pectin in order to develop a method for the moisture, ash, acid insoluble ash, equivalent weight,
commercial extraction of pectin from apple pomace. methoxyl content, anhydrogalacturonic acid content,
acetyl value and jelly grade15. Equivalent weight of
Materials and Methods the pectin was determined by titrating a known weight
Fresh pomace left after extraction of apple juice of pectin against standardized 0.1N NaOH solution to
from processable grade fruits at HPMC (Himachal a faint pink end point and expressed as under:
Pradesh Horticultural Produce Marketing and Weight of Sample×1000
Processing Corporation Ltd) Fruit Processing Plant, Equivalent Weight=
Parwanoo, Dist. Solan (H.P.) was utilized to carry out Titre× Normality of alkali
these studies. Apple pomace after different Methoxyl content was determined by
pretreatments such as blanching (boiling at 95oC for 5 saponification of extracted pectin and titrating the
minutes followed by cooling) and drying (in liberated carboxyl group against standardized 0.1 N
mechanical dehydrator at 50±2oC) was used for NaOH solution using phenol red as indicator to a faint
extraction of pectin using different extraction and pink end point. Methoxyl content was calculated as
precipitation methods. Method for extraction of pectin per expression:
consisted of boiling the apple pomace in distilled
Titre× Normality of alkali×3.1
water, 0.05N HCl (acid extraction) and 0.75% Methoxylcontent,% =
ammonium oxalate-oxalic acid (1:1) for one hour at Weight of sample
95oC(Ref. 3). On the basis of preliminary observations it Degree of esterification was calculated from the
was found that the ratio of 1:2 of fresh apple pomace observed value of methoxyl content and
to extraction medium was the most suitable and was anhydrogalacturonic acid content as per the following
followed in all the extraction methods. After expression given by Schultz16:
extraction, the extract was separated from the solid
residue by filtration through a muslin cloth prior to its Degree of esterification,% (DE)
176 ×methoxylcontent×100
use for pectin precipitation. Sequential combination =
31×Anhydrogalacuronic acid content
extractions such as two-stage sequential water-acid
and water-oxalate extraction were carried out in Jelly grade of extracted pectin was measured by
which the pomace was extracted first with boiling making test jellies with assumed jelly grade and
water for one hour to separate the water soluble comparing them with a standard jelly of 150 grade
fraction, and the remaining residue was again pectin. Each attribute was determined in triplicate.
extracted for one hour with the corresponding Alkalinity of ash of pectin was determined for the
extractant. The pectin extract obtained from different subsequent calculation of acid insoluble ash and
extractions after cooling to room temperature was anhydro-galacturonic acid contents15. The ash
used for precipitation of pectin either with 95% obtained after determination of ash contents was
ethanol (alcoholic precipitation)3 or precipitating by dissolved in standardized 0.1N HCl solution, heated
using aluminium chloride14. The precipitates were to boiling and cooled and titrated against standardized
then separated, washed successively with 70 and 95% 0.1N NaOH solution using phenolphthalein as
186 INDIAN J NAT PROD RESOUR, JUNE 2014

indicator to a faint pink end point. Alkalinity of ash Optimization of pre-treatments of pomace
was calculated as per the following expression: Fresh pomace (13.3% pectin on dry weight basis)
(Table 2) was found to be a good source of pectin
Alkalinity of ash, % (as carbonate) followed by blanched pomace (13.0%) with a jelly
Titre× Normality of alkali×60×100 grade of 120-125. Substantial losses in yield as well
=
Weight of ash×1000 as quality of pectin were observed during drying of
pomace. However, these losses were reduced when
Cost of production
drying was preceded by blanching. Since drying is
The cost of production of pectin was calculated by
necessary to facilitate raw material handling,
taking into consideration various input costs such as
blanching of pomace prior to drying was optimized as
cost of raw material, labour and electricity, processing
pretreatment before pectin extraction. The yield and
costs, packaging and other charges. The cost of
jelly grade of pectin obtained from dried pomace
recovered raw material like alcohol was subtracted
after blanching and drying was recorded as 10.5%
from cost of production for calculation of cost of
and 110 respectively. The likely causes of lower
pectin per kg.
pectin yield from unblanched dried pomace are
degradation of pectin by the action of inherent or
Statistical analysis: The data were analyzed
added pectinolytic enzymes18 which are inactivated by
statistically by following Completely Randomized
blanching, non-enzymatic degradation at high
Design (CRD)16.
temperature19, and insolubilization of pectin due to
enzymatic browning20. Thus, drying of pomace
Results and Discussion
after blanching has been optimized for extraction of
Physico-chemical composition of apple pomace
pectin.
The pomace was found to contain 8.87 % total
soluble solids consisted of sugars (6.18%), acid Standardization of extraction and precipitation methods
(0.29% as malic acid) and ascorbic acid (3.45 Single acid extraction resulted in higher pectin
mg/100g); while insoluble material constituted about yield (6.3-10.5%) than single oxalate (4.0-8.0%) or
2.33% pectin (as calcium pectate) and 5.39% crude water extraction (1.8-3.4%) methods (Table 3).
fibre (Table 1). The mineral matter, represented by Sequential extractions in which the water soluble
total ash content amounted to 0.87%. Thus, the fraction removed before extraction with either acid or
pomace besides being a rich source of sugars, acid oxalate, were found to improve yields by 13.1 and
and minerals, also contained appreciable amount of 20.7%, respectively when the collective yield from
pectin, which can be utilized in the food industry. water and extractant soluble fractions was considered.
Thus two-stage sequential water-acid extraction
Table 1—Physico-chemical composition of apple pomace yielded the highest amount of pectin. The pectin yield
Attributes Mean ± S.E. from apple pomace after precipitation by using 95%
ethanol was found to range between 3.4 to 10.5%
Fresh weight basis Dry weight basis
which was significantly higher than the yield obtained
Moisture, % 84.07± 0.16 –
Total solids, % 15.93 ± 0.16 – Table 2—Effect of various pre-treatments of apple pomace on the
TSS, oBrix 8.87 ± 0.20 – yield and quality of pectin
Titratable acidity/%
0.29 ± 0.01 1.84 ± 0.08 Pectin
malic acid
Pre-treatment Yield, % AGA, % DE, % Jelly Grade
Total sugars, % 6.18 ± 0.40 38.78 ± 2.05 (dwb)
Reducing sugars, % 2.20 ± 0.05 13.85 ± 0.30 Unblanched
Non reducing sugars, % 3.77 ± 0.29 23.68 ± 1.81 13.3 59.9 74.9 125
fresh
Ascorbic acid, mg/100g 3.45 ± 0.28 21.87 ± 1.80 Blanched fresh 13.0 59.7 72.1 120
Crude fibre, % 5.39 ± 0.29 33.86 ± 1.81 Unblanched
7.3 57.9 61.0 100
pHc 4.17 ± 0.12 – dried
Ash content, % 0.87 ± 0.03 5.48 ± .19 Blanched dried 10.5 59.1 71.2 110
Pectin, % calcium CD(0.05) 0.74 1.57 1.82 9.41
2.33 ± 0.19 14.66 ± 1.21
pectate AGA= Anhydrogalacturonic acid content, DE= Degree of
c
dilution 1:3 esterification, dwb= dry weight basis
 SHARMA et al: OPTIMIZATION OF EXTRACTION METHOD OF PECTIN FROM APPLE POMACE 187

Table 3— Effect of different extraction and precipitation methods on the yield and quality characteristics of pectin from
blanched dried pomace

Pectin Acetyl
Precipitation Moisture, Ash, AIA, AGA, DE, Jelly
Extraction method yield, EW value,
method % % % % % grade
% dwb %
Boiling water, 1 h E 3.4 8.5 0.70 0.61 1271.4 51.7 60.8 0.46 40
A 1.8 9.0 0.70 0.60 1000.3 57.8 60.5 0.44 40
Boiling with 0.05N HCl, 1 h E 10.5 10.0 0.63 0.55 1239.8 59.1 71.2 0.37 110
A 6.3 11.7 0.67 0.57 872.2 64.4 69.0 0.45 120
Boiling with 0.75% ammonium
E 8.0 11.2 0.73 0.64 1316.4 56.3 74.9 0.44 100
oxalate-oxalic acid (1:1), 1 h
A 4.0 11.6 0.67 0.58 1035.2 61.5 70.7 0.48 105
Boiling water, 1 h + boiling with
E 9.8 10.0 0.60 0.52 1111.5 60.3 71.7 0.34 120
0.05N HCl, 1h*
A 4.1 11.5 0.63 0.54 877.4 64.9 69.8 0.39 130
Boiling water, 1h + boiling with 0.75%
E 6.1 9.5 0.70 0.60 1230.7 57.9 69.7 0.4 80
ammonium oxalate-oxalic acid (1:1), 1h*
A 3.8 10.2 0.67 0.57 961.8 61.3 68.7 0.41 90
CD(0.05)
Precipitation method (P) 0.58 0.43 0.172 0.148 19.80 0.48 0.69 0.047 3.61
Extraction method (E) 0.91 0.68 0.272 0.235 31.31 0.75 1.08 0.074 5.71
PxE 1.29 0.96 0.385 0.332 44.28 1.06 1.53 0.105 8.08
AIA= Acid insoluble ash, EW= Equivalent weight, AGA= Anhydrogalacturonic acid content, DE= Degree of esterification
E = Alcoholic precipitation, A = Aluminium chloride precipitation;
* Data given for extractant soluble fraction

from aluminium chloride precipitation method (1.8- extraction (60.3-64.9%) which was higher than that of
6.3%). This could be due to precipitation of pectin pectin from single oxalate extraction. Further, the
with high degree of esterification in alcoholic pectin obtained from water extraction was found to
precipitation21 and/or purification of pectin by have the lowest value of anhydrogalacturonic acid
elimination of neutral polysaccharides and further content. Precipitation of pectin by the use of
removal of neutral sugar side chains during acid alumimium chloride resulted in a purer pectin with
alcohol washing process22. higher anhydrogalacturonic acid content as compared
The level of moisture in the pectin extracted from to the precipitation by using ethanol. A minimum
apple pomace ranged from 8.5-11.7% with the highest value of 65% AGA for commercial pectins has been
amount of moisture recorded in pectin obtained after specified by FAO24. Thus the pectin obtained from
oxalate extraction (Table 3). The difference in apple pomace by using different extraction and
moisture content of various pectin samples could be precipitation methods, was found close to the range of
due to the difference in hygroscopic nature of pectin anhydrogalacturonic acid content for standard pectin.
with different degrees of esterification23. The total ash The pectin was also found of high methoxyl type with
content in the pectin extracted from apple pomace by degree of esterification ranging between 60.5-74.9%.
using different extraction and precipitation methods Among the extraction methods, pectin produced by
ranged from 0.63 to 0.73%, while the values of acid single oxalate extraction has highest degree of
insoluble ash ranged from 0.52 to 0.64%. The ash esterification, which was closely followed by single
content of the pectin extracted in the present study acid extraction. Lower degree of esterification was
was well below the Food and Agriculture obtained in the pectin precipitated by aluminium
Organization (FAO) specifications of not more than chloride as compare to pectin precipitated with
1% acid insoluble ash for commercial pectins24. The ethanol. The acetyl value was found to range between
anhydrogalacturonic acid (AGA) contents ranged 0.34-0.48% in pectin extracted from apple pomace.
from 51.7-64.9% with the highest value recorded in High degree of acetyl esterification of about 21 to
pectin obtained from two-stage sequential water-acid 25 moles per 100 moles of galacturonic acid in sugar
188 INDIAN J NAT PROD RESOUR, JUNE 2014

beet pectin has been considered to inhibit jelly by two-stage sequential water-acid extraction was
formation25. In apple pectin acetyl esterification value highest followed by acid extraction. Aluminium
is reported to range between 4.0-8.7mol/100 moles of chloride precipitation resulted in pectin with higher
galacturonic acid4 but is too low to inhibit jelly jelly grade in comparison to alcoholic precipitation.
formation. With respect to the extraction and Thus two-stage sequential water-acid extraction is
precipitation methods, the pattern of degradation of found to give high yield of pectin with best quality
acetyl and methyl esters (degree of esterification) was characteristics. However, the use of single acid
found to be similar with high acetyl value in pectin extraction was found more appropriate as two-stage
obtained from oxalate and water extractions and lower sequential water-acid extraction add one extra unit
values in the pectin from acid extraction and operation for pectin extraction without increasing the
sequential water-acid as well as water-oxalate yield in equivalent proportion,. The optimized method
extractions. Jelly grade of pectin was found to range for extraction of pectin from apple pomace is
from 40 to 130. The jelly grade of the pectin extracted presented in Figure-1.

Fig. 1–Flow sheet for extraction of pectin from apple pomace

 SHARMA et al: OPTIMIZATION OF EXTRACTION METHOD OF PECTIN FROM APPLE POMACE 189

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