Characteristics of Pectin Extracted from Cocoa Pod Husks

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PELITA PERKEBUNAN, Volume 37, Number 1, April 2021 Edition

Pelita Perkebunan 37 (1) 2021, 62—75 ISSN: 0215-0212 / e-ISSN: 2406-9574

Characteristics of Pectin Extracted from Cocoa Pod Husks

Nanti Musita1*)

1)Bandar Lampung Industrial Standardization and Research Center, Jl. Soekarno-Hatta (By Pass), Bandar Lampung, Indonesia*)Corresponding author: [email protected]

Received: 14 August 2020 / Accepted: 13 October 2020

Abstract

Cocoa plant husk is one of the source of pectin. Pectin in the food industryis used as thickener, gel agent and stabilizer. The aim of this study was to determinethe characteristics of the pectin from cocoa pod husks with variation in temperatureand extraction times. In this study the extraction of pectin from cocoa pod huskwas carried out with hydrochloric acid solvent, with 40, 60, and 80 minutesextraction times at 65oC, 80oC, and 95oC. The results showed that the extractionof temperature (65oC, 80oC, and 95oC) and extraction time (40, 60, and 80 minutes)had no significant effect on methoxyl content, galacturonic acid, equivalent weight,and pectin content, but the extraction time had a significant effect on the acetylnumber and the degree of esterification. The highest yield of pectin was obtainedat an extraction temperature of 80oC for 60 minutes. The pectin content in cocoapod husk is larger than the content in banana skin. The characteristics of cocoapod husk pectin powder are brown, moisture content is 10.56–11.96%, ash content6.82–8.97%, methoxyl content 3.51–4.86%, galacturonic acid content is 41.38–88.40%, esterification degree 10.76–19.96%, acetyl number 14.55–20.90%, equiva-lent numbers 663.83–1549.22, pectin content 9.52–19.51 and yield 5.55–7.70%. Therewas no difference in the functional groups between standard, commercial, and pectinextracted at different temperatures.

Keywords: characteristic, pectin, cocoa pod husk

Pectin is a polysaccharide compoundthat is soluble in water and is a pectinic acidthat contains methoxyl groups, and its mainfunction as a thickening and gelling agents.Beside in the food industry, pectin can beused in the cosmetics and pharmaceuticalindustries, such as in the manufacture ofcreams, soaps, hair oils and pastes. The qualityof pectin can be seen from the amount ofmethoxyl content. If the methoxyl content is2.3 to 4.5%, it is classified as low, while themethoxyl content is more than 7.12%, it isclassified high methoxyl content (Anonim,2014). The methoxyl content of pectin willeasily form jelly which is an important property

INTRODUCTION

Cocoa pod husk is one source of pectin(Susilowati et al., 2017). The use of cocoa plantshas been mostly for the beans, while other partssuch as cocoa pod husk and pulp are currentlyused for compost. The need for pectin forindustries in Indonesia in 2012 reached 2,277tons (equivalent to USD 2,133 thousands),all of which were imported (Anonim, 2012).To solve for pectin requirement, cocoa pod huskcan be used as raw material to be processedand extracted. Therefore, it is expected toreduce pectin imports and increase the addedvalue of cocoa pod husk.

DOI: 10.22302/iccri.jur.pelitaperkebunan.v37i1.428

Characteristics of pectin extracted from cocoa pod husks

63PELITA PERKEBUNAN, Volume 37, Number 1, April 2021 Edition

of pectin. The use of pectin in the foodindustry is determined by the methoxylcontent of the pectin. High methoxyl contentis usually used for jam, jelly, high-qualityconfectionery, thickening for drinks, flavoremulsions. Pectin with low methoxyl is usuallyused for jam and low calorie jelly for peoplewho avoid sugar, is also used for puddingand fruit gel in ice cream (Schemin et al.,2005).

Pectin can be obtained from the husksof cocoa by extraction. Extraction is theprocess of separating one or several materialsfrom a solid or liquid, the separation occurson the basis of the different solubility of eachcomponent in the mixture (McCabe & Warren,2000). The process of extracting pectin fromplant tissue depends on several factors,namely contact time, type of solvent, extrac-tion temperature, the ratio between the sampleand the solvent and the type of solvent used(Prasetyowati et al., 2009). Generally, thepectin extraction process uses acidic solvents(Nurhikmat, 2003).

Pectin is a type of carbohydrate derivedfrom polysaccharide compounds found inplant cell walls. Pectin is an important com-ponent in plant tissue because it providesflexibility and mechanical strength to plants.Pectin consists of -galacturonic acid residuesthat are partially esterified with a methylgroup and acetyl ester with a small portionof L-rhamnosa (Güzel & Akpýnar, 2019).

Pectin compounds consist of pecticacid, pectinic acid and protopectin. Pecticacid is a galactonic acid compound that iscolloidal without the content of methyl esters.Pectinic acid is polygalluraconic acid whichis colloidal and contains methyl ester, whileprotopectin is neither pectate substance norsoluble in water (Hanum et al., 2012).

In food product pectin is used as thickener,gel maker, and stabilizer in various product

such as jelly, jam, marmalade, candy, andjuice. In addition, pectin can also play a rolein the formation of texture and reduce totalcholesterol level (Habibati, 2017).

Pectin requirement in Asia, especiallyIndonesia, increased in 2000 to 2009. Untilnow, pectin used by industries in Indonesiais imported especially from Germany. Theamount of pectin imports in Indonesia in2008 was 147.6 tons and continued to increaseuntil in 2011 which reached 291.9 tons witha value of USD 2,977,498 (Injilauddin et al.,2015). Whereas Khendriani (2018) stated theneed for pectin in February to March 2013 was85,157 kg and it is estimated that in 2020 theneed for pectin will reach 1,320 tons.

This study was carried out to know thecharacteristics of pectin extracted fromcocoa pod husk with variations in tempera-ture and exctraction times.

MATERIALS AND METHODS

This research was conducted at the Pro-cessing Laboratory of the Industrial Standard-ization and Research Institute in BandarLampung. The main material used in thisstudy was cocoa pod husks of MCC 01 clonetaken from local plantation at Pesawaran,Lampung Province. The scope of this studywas to elaborate the technology of the processof making pectin flour from cocoa pod husks,and the treatment in this study were extrac-tion temperature (65ºC, 80ºC, and 95ºC) andextraction time (40 minutes, 60 minutes and80 minutes). The determination of the typeof treatment was based on the results ofprevious studies, including research on pectinfrom banana peels (Tuhuloula et al., 2013;Hanum et al., 2012), research on pectin frombrown skin (Susilowati et al., 2013). Thedata were analyzed using analysis of varianceto get error at 5% level.

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Pre-treatment

The cocoa pod husks were cleaned uponarrival from the plantation and put inside abasin with lime ash solution to remove thegums. The pod husk were cut into slices withdimension of approximately 2 cm x 2 cm x0.5 cm each and dried prior to size reduction.Drying was carried out for about 12 hours,consisted of sun drying for approximately 6–8 hours, and drying using a conventional ovenat temperature of 40oC for approximately 4–5 hours. The dried cocoa husk slices werethen reduced their size into 60-80 mesh usinga grinder (Fomac FCT Z200).

Pectin Extraction

Cocoa pod husk flour was extractedusing 0.1 N HCl concentration until the pHof the solution becomes 1.5–3. The mixturewas heated on the bath while stirring accordingto treatments. The extract was filtered usingfilter paper (Whatman No. 41) with the helpof a vacuum buchner to separate the filtratefrom the residue. The filtrate was cooledto room temperature, then added 70% tech-nical ethanol (1:1) and deposited for 12–16hours. The pectin precipitate was filteredand washed with technical ethanol severaltimes (at least 3 times). The final washingused technical methanol to achieve the maxi-mum pectin produced. The pectin chlorideprecipitate was dried in an oven at 40ºC for8 hours, then sieved with a 60 mesh sieve,weighed and the yield calculated.

Observation

This research analyzed yield of pectin,methoxyl content, galacturonic acid content,degree of esterification, equivalent weight,pectin content, and functional group analysisusing FTIR instrument. Functional groupanalysis was also performed on commercialpectin. Several parameters observed were:

1. Yield of pectin. The yield percentage wasthe ratio g of pectin produced per g of dryraw material (Amin, 2007).Yeild (%) =

pectin total weight x 100raw material dry weight

2. Methoxyl content. The methoxyl content(MC) was determined by adding 25.0 mLNaOH 0.25 N into the neutral solutionfrom the determination of equivalentweight, then shaken properly and letstands for 30 minutes at room tempera-ture in an erlenmeyer closed. 25.0 mLHCl 0.35 N and phenol red indicator wereadded, later titrated with 0.1 N NaOH titrantuntil the solution turns pink (Ranganna,1977).MC (%) =

(ml.NaOH x 31 x N.NaOH) x 100

pectin weight (mg)

where 31 = molecular weight of methoxyl

3. Galacturonic acid content. Galacturonicacid content (GAC) were calculated frommilli equivalents of NaOH obtained fromdetermination of equivalent weight andmethoxyl content (Ismail et al., 2012).

GAC (%) = (A+B) x 176 x 100pectin weight (mg)

where a (meq of NaOH for free acid);B (meq of NaOH for methoxyl).

4. Degree of esterification. The degree ofesterification (DE) is the percentage ofthe amount of D-galacturonic acid residuein which the carboxyl group was esterifiedwith ethanol (Schultz cit. Hariyati, 2011)DE (%) =

metoxyl content x 176 x 100 galacturonate content x 31

5. Equivalent weight value. The equivalentweight (EW) value was used for calcu-lating the levels of galacturonic acid anddegree of esterification (Ranganna, 1977).



The equivalent weight was determined byweighing of 0.25 g pectin, put in a 250 mLenlenmeyer and moistened with 10 mLalcohol. Oxygen free distilled water asmuch as 50.0 mL and 6 drops of phenolred indicator added. The mixture was thenstirred rapidly for ensuring that all pectinsubstances have dissolved and there areno lumps attached to the side of erlenmeyer.Titration is carried out slowly with 0.1 Nstandard NaOH titrant until the color ofthe mixture turns pink (pH 7.5) and staythere for at least 30 seconds. The solutionneutralized which is then used for deter-mination of methoxyl content.EW (mg) =

pectin weight (mg) x 100 (ml NaOH x N NaOH)

6. Pectin content. Sample of 0.1 g is dissolvedin 40 mL distilled water while heating,then cooled. Continue to put in 100 mLvolumetric flask and added distilledwater to mark the limit. It is, then, filteredwith Whatman filter paper No. 4 andtaken 20 mL of the filtrate from the flask.Then added 25 mL distilled water and 2drops of PP indicator. The solution wastitrated with 1 N and NaOH in combina-tion with 1 mL of 1N NaOH then leaveit for overnight. Solution later added with5 mL of 1 N acetate until the color becomesclear. After 5 minutes, the solution wasadded 2.5 mL of 1N CaCl2 and stirredto homo-genize it, then filtered with hotwater moistened filter paper, dried in anoven at 102oC for 2 hours, cooled insidethe desiccator and weighed in a closedcontainer. In addition, the precipitate waswashed with almost boiling hot wateruntil it is free of chloride. The filter paperwhich contains the precipitate was trans-ferred to a weighing container, dried at100oC for overnight, cooled in a desic-cator and then weighed. Calculation ofpectin levels (Apriyantono et al., 1989)

using the following formula: Ca-pectate (%) =

calcium pectate weight (g) x 5 x 100 sample weight (g)

7. FTIR (Fourier Transform Infra Red)spectroscopy is an analytical method usedfor functional group analyzer (Kwon et al.,2013). For FTIR spectroscopic analysis,5 µl of the sample was placed in the containersilicon, which was then placed on a microreader unit. Then the infrared rays pass tothe sample at a wavelength of 4000 cm-1

to 400 cm-1. The waves transmitted by thesample is captured by a detector connectedto a computer which will provide an over-view of the spectrum of the sample beingtested. The functional group analysis ofa sample was carried out by comparingthe absorption bands formed in the infra-red spectrum.

RESULTS AND DISCUSSION

Yield of Pectin

According to Fitriani (2003), pectinproduced using the drying method in thepreparation of ingredients had a greater yieldthan those were not dried beforehand (freshraw materials). This was due to drying ofraw materials affected the diffusion of thesolution to the material better than in a freshstate, because fresh materials had high watercontent which makes it difficult to diffuseacid solution to extract pectin from the mate-rials. The cocoa pod husk powder can beused for the extraction process. The yieldof pectin flour can be seen in Figure 1.

The results of analysis of variance witha confidence level of 95% ( = 0.05) withindicates that the temperature and durationof extraction did not significantly affect theyield of pectin of cocoa pod husk in thisstudy. In Figure 3 it can be seen that thehighest yield of cocoa pod husk pectin is

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generally produced at extraction tempera-tures of 80ºC with a duration of 60 minutes,i.e. 7.70% (dry basis). At temperature of 65ºCthere is an increase in yield from 40 to 80minutes. However, at a temperature of 95ºC,the addition of extraction time actuallydecreases the yield of cocoa husk flour. Thisis because at higher extraction temperaturethere is an increase in the decompositionreaction of pectin compounds to galacturonicacid so that resulting in the yield decreasewith increasing extraction time.

The differences in the yield of pectinproduced depend on the type and part of theplant extracted. In the study of Sugiarto (2007),it was known that there was an increase inthe yield of pectin from carrots with increasingdegrees of acidity, where the highest yield waspH 2.0, i.e. 0.88% and the lowest yield wasextraction at pH 3.0, i.e. 0.74%. The highestyield of Kepok banana skin pectin was 5.21 g(from 10 g of banana powder), which wasobtained from extraction at 90ºC for 80 minutesusing HCl (Hanum et al., 2012).

In the process of pectin extraction usingacidic solvents there is a breakdown of insolubleprotopectin into soluble pectin. At a high levelof acidity, the process of protopectin hydrolysisof fruit skin tissue will increase rapidly.Protopectin does not dissolve easily because

it is in the form of calcium and magnesium salts.Hydrolysis of protopectin with acids causeshydrogen ions to replace calcium and magne-sium ions in the protopectin molecule. Thisis due to a pH of 1.5 which is more acidic andhas more hydrogen ions so it is likely thatmore calcium and magnesium are substituted(Prasetyowati et al., 2009). With the amountof calcium and magnesium substituted, theamount of pectin that occurs will also belarge. Gusti (2009) states that at a low aciditylevel, the pectin compound will decomposeinto galacturonic acid so that the yield ofpectin decreases.

Pectin Characteristics

The characteristics of pectin from cocoapod husk were analyzed compared withcommercial pectin with parameters accordingto the IPPA standard. The result of the analysiscan be seen in Table 1.

Pectin

The results of analysis of variance witha confidence level of 95% ( = 0.05) witha significant value (p value) > , showed thetemperature and extraction times have nosignificant effect on pectin content of cocoapod husk in this study. Figure 2 shows the

Figure 1. The effect of temperature and extraction time on pectin yield

9876543210

65oC 80oC 95oCY

ield

(%)

40 60 80

Extraction time (minutes)



tendency to increase pectin content withincreasing extraction temperature especiallyin the extraction time of 60 and 80 minutes.However, at the extraction of 40 minutesthere was a decrease in pectin levels. Theincreased extraction temperature causes anincrease in the kinetic energy of the solutionso that the diffusion of solvents into tissuecells increases as well. This results in pectinseparation from tissue cells so that the amountof pectin produced will be more. In addition,contact between particles also requires time,the longer the contact the greater the chanceof the solvent being contracted so that theweight of the pectin produced will be higher.Pectin content produced ranged from 9.52-19.51%.

Equivalent Weight

Equivalent weight is a measure of thecontent of free galactonic acid groups containedin the pectin molecular chain. Pure pecticacid has an equivalent weight of 176. Purepectic acid is pectic acid which is composedentirely of poly galacturonic acid which is freefrom the methyl ester group, so it does notundergo esterification. The less free acid groupsmeans the higher the equivalent weight. Theequivalent weight obtained from the resultsof this study can be seen in Figure 3.

The results of analysis of variance witha confidence level of 95% ( = 0.05) witha significant value (p value) > , showed thetemperature and extraction times have nosignificant effect on the equivalent weight

of cocoa pod husk in this study. Figure 3shows the varied equivalent values, namely664–1549 mg. The tendency is that thehigher the extraction temperature, theequivalent weight decreases and the longerthe extraction time will cause the processof de-esterification of pectin to pectic acid.This deesterification process will increasethe number of free acid groups. The increasein the number of free acid groups will reducethe equivalent weight.The results of this studyare similar to research conducted by Hariyati(2006) who used Kepok banana skins.

Equivalent weight according to IPPAStandards (International Pectin ProducersAssociation) (Anonim, 2014) namely 600–800 mg. The results of this study are mostlystill at standard conditions that have beenset. This is influenced by the molecular weightof pectin depending on the type of plant,quality raw materials, extraction methods andtreatment in the extraction process. Therewould be possible influences to the equiva-lent weight value, i.e. the property of pectinresulting from the extraction itself, as well asthe titration operational (Fitria, 2013).

Methoxyl Content

Methoxyl content is defined as the numberof moles of ethanol contained in 100 molesof galacturonic acid. These methoxyl pectincontent have a very important role in deter-mining the functional properties of pectinsolutions and can affect the structure andtexture of pectin gel. The levels of methoxyl

Table 1. Wave number (cm-1) results of FTIR analysis of pectin functional groupsWave number (cm-1)

Functional groups-OH

Stretching -C=O -C=O Bending Stretching R-O-R-CH3 (ester) (acid) -C-H -C-H (ester)

Standard 3446 2934 1698 1457 1369 1152Commercial pectin 3323 2937 1747 1632 1443 1377 1153Cocoa pod husk 65oC/40 minutes 3410 2926 1741 1634 1331 1147 80oC/40 minutes 3404 2926 1738 1635 1406 1331 1147 90oC/40 minutes 3391 2935 1746 1636 1441 1376 1153

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pectin obtained from the results of this studycan be seen in Figure 4

The results of analysis of variance witha confidence level of 95% ( = 0.05) showedthe temperature and extraction times haveno significantly effect on the methoxyl contentof cocoa pod husk in this study. Table 1 showedthe varied equivalent values, namely 664–1549 mg. The tendency was that the higherthe extraction temperature, the equivalentweight decreases and the longer the extractiontime will cause the process of de-esterificationof pectin to pectic acid. This de-esterificationprocess will increase the number of free acidgroups. This increase in the number of freeacid groups will reduce the equivalent weight.The results of this study was similar to researchconducted by Hariyati (2006) who used Kepokbanana peels.

Equivalent weight according to Interna-tional Pectin Producers Association (IPPA)Standards (Anonim, 2014) namely 600–800 mg.The result of this study are mostly still at stan-dard conditions that have been set. This is in-fluenced by the molecular weight of pectin,on the type of plant, quality raw materials, andextraction process. Possible influences on theequivalent weight value is the property of pectinresulted from the extraction (Fitria, 2013).

In this study the highest methoxyl contentwas 4.86% resulting from the extraction tem-perature of 65oC for 60 minutes and thelowest 3.51% from 95oC for 60 minutes.This shows that the higher the extractiontemperature, decreased in the level ofmethoxyl produced. This increase in methoxylcontent is due to the increase in esterifiedfree carboxyl groups.

25

20

15

10

5

0

Pect

in c

onte

nt (

%)

Figure 2. The effect of temperature and extraction time on pectin content

40 60 80Extraction time (minutes)

65oC 80oC 95oC

200018001600140012001000800600400200

0

Figure 3. The effect of temperature and extraction time on equivalent weight of pectin

65oC 80oC 95oC

Pect

in e

quiv

alen

t wei

ght (

mg)




The methoxyl content of pectin producedin this study ranging from 3.51–4.86%. Accordingto IPPA (Anonim, 2014) quality standard data,pectin with methoxyl levels of less than7.12% includes in low methoxyl pectin. Lowmethoxyl levels are thought to be due to anincrease in non-pectate compounds on the cellwall which are dissolved during the extractionprocess. Pectin which has a low methoxyl contentis more advantageous because low methoxylpectin can be directly produced without goingthrough the process of demethylation.

Galacturonic Acid Content

Galacturonic acid content and pectinmolecular charge have an important role indetermining the functional properties of pectinsolution. Galacturonic acid content can affectthe structure and texture of pectin gel. Thehigher the level of galaturonic acid, thehigher the purity of the pectin. In pectins otherthan D-galacturonic as the main component,pectin also has D-galactose, L-arabinose,and L-rhamnose in high amounts, whichvaries depending on source and conditionsused in its insulation (Willats et al., 2006).

The results of analysis of variance witha confidence level of 95% ( = 0.05) witha significant value (p value) > , showedthe temperature and extraction times have

no significant effect on the galacturonic contentof cocoa pod husk in this study. Table 1shows that galacturonic content increase withincreasing temperature then decreases atincreasing extraction temperatures (95oC).Galacturonic content obtained ranged from41.38–88.40%. The acquisition of galactu-ronic content is already included in the pectinquality standards set by IPPA (Anonim,2014), with the minimum content is 35%.The highest level of galacturonic acid wasobtained at pectin extraction at 95oC for 80minutes. The results of galacturonic acid testshowed that the temperature and concen-tration of the solvent affected the content ofgalacturonic pectin produced. Galacturonicacid content tend to increase along with theincrease in hydrolysis of the protopectin topectin, whose basic component is D-galac-turonic acid

Degree of Esterification

The degree of esterification is the percentageof the amount of D-galacturonic acid residuein which the carboxyl group is esterified withethanol. The degree of esterification is obtainedfrom a comparison between methoxyl andgalacturonic acid content.

The results of analysis of variance witha confidence level of 95% ( = 0.05), showed

6

5

4

3

2

1

0

Met

hoxy

l con

tent

(%

)


65oC 80oC 95oC

Figure 4. The effect of temperature and extraction time on methoxyl content

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that the extraction time did not significantlyaffect the degree of esterification, but theextraction temperature has a significanteffect to the degree of esterification of cocoapod husk. The range of degrees of esteri-fication obtained in this study was 10.76–16.96%. The highest degree of esterificationwas obtained at the extraction of pectin at65oC for 40 minutes and the lowest at 95oCfor 60 minutes. According to the pectin qualitystandard set by IPPA (Anonim, 2014), thepectin produced in this study is a low pectinester because it has an esterification degreeof less than 50%.

The esterification degrees in Figure 6show a decrease with increasing extractiontemperature. The degree of esterification tendsto decrease with increasing time due to theglycosidic group of methyl esters of pectinwhich tends to be hydrolyzed to producegalacturonic acid. If the extraction temperatureis too high, pectin will turn into pectic acid,which is galacturonic acid free from the methylester group. The number of methyl estergroups indicates the number of unesterifiedcarboxyl groups or degree of esterification.

FTIR Analysis

FTIR analysis was performed to seethe composition of the extraction of pectinflour extracted from cocoa pod husk. Theresults of the analysis were compared withthe results of the FTIR analysis of the stan-dard pectin (Table 1).

Pectin has hydroxy (-OH), methoxy(CH3), carbonyl (C=O), and ether (C-O-C)functional groups, where the main functionalgroups in pectin usually occur at wavenumberof 1000–2000 cm-1, and carbonyl bond esteri-fied at 1740–1760 cm-1 (Ismail et al., 2012).The stretching spectrum of -OH is at wave-number of 3100–3700 cm-1, the -OH bendingspectrum is located at 1600–1700 cm-1

(Hongping et al., 2004), and spectrum of theC-H alkane (CH3) group is at 2700–3050 cm-1

(Hadri et al., 2012). The carbonyl group islocated at 1630–1850 cm-1, the bond -C-H isat 1450–1375 cm-1, the ether functional group(R-O-R) is in the spectral range of 1050–1260 cm-1. Based on the results of FTIRanalysis on each sample, it shows that it hasconformity to the standard pectin structure(Pavia et al., 2009).

6

5

4

3

2

1

0Gal

actu

roni

c ac

id c

onte

nt (

%)


65oC 80oC 95oC

Figure 5. The effect of temperature and extraction time on galacturonic acid content



65oC 80oC 95oC

201816141210

86420E

ster

ific

atio

n de

gree

(%

)

Extraction time (minutes)

Figure 6. The effect of temperature and extraction time on esterification degree

40 60 80

Extraction time (minutes)40 60 80

65oC 80oC 95oC

From the FTIR spectrum data above(Table 1, Figure 7), the absorption of eachfunctional group from standard, commercialpectin and extraction results shows a difference.In the standard pectin (Figure 7) there is anabsorption peak at wavenumber of 3446 cm-1,in commercial pectin appear absorption peakat wavenumber of 3323–3417 cm-1, and at theextraction pectin the absorption peak appearsat 3394–3410 cm-1 on cocoa pod husk, whichshows the absorption of the -OH group fromcarboxylic acids (Gnanasambadam & Proc-tor, 2000).

Uptake of element -CH3 appears at wavenumber of 2934 cm-1 on standard pectin(Figure 7), while commercial pectin appearsat wavenumber of 2937 cm-1 on cocoa pod husk,and on pectin resulting from contraction.There is a shift in the wavenumber at 2926–2935 cm-1. This indicates the presence ofa methoxy group which indicates the methylester group of galacturonic acid.

The wavenumber of 1747 cm-1 indicatesthe presence of carbonyl groups of esters(C=O) in commercial pectin (Figure 7 (d)),whereas in the pectin resulted from the extrac-tion has a shift at wavenumber of 1738–1746cm-1 for cocoa pod husk (Figure 7 (a-c)).

The carbonyl group of carboxylates incommercial pectin is characterized by theappearance of absorption peaks at wavenumber 1632 cm-1, whereas in pectin resultingfrom the extraction of cocoa pod husk appearsat wavenumber 1634–1636 cm-1 (Table 1),according Gnanasambadam & Proctor(2000) that carbonyl from ester appears atwavenumber of 1760–1745 cm-1 and carbonylfrom carboxylate appears at wavenumber1640–1620 cm-1.

According to Coates (2000), FTIR spectrawith their peak absorption indicated somefunctional group in pectin sample such ashydroxyl group (O-H), carboxyl group (C=O)and C-O. The peak between 3500 and 3300cm-1 is due to stretching of hydroxyl group,while peaks lies between 1850 and 1500 cm-

1 are associated with the vibrational modesof a carboxyl group that indicates doublebond from the carboxylic acid methyl ester.Other band lies between 1320 and 1210 cm-1

is associated with C-O.

C-H bond interactions appear in wave-numbers between 1460-1300 cm-1, which isfound in each sample. The stretching vibra-tion of C-O-C appears at wavenumber of1000-1140 cm-1. Based on the description

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Figure 7. FTIR spektra of (a) cocoa pod husk pectin production by 65oC/40 minutes, (b) cocoa podhusk pectin production by 80oC/40 minutes, (c) cocoa pod husk pectin production by 65oC/40 minutes, and (d) commercial pectin

(a)

(b)

(c)

(d)

Wavenumber cm-1

Wavenumber cm-1

Wavenumber cm-1

Wavenumber cm-1

Tran

smitt

ance

(%

)Tr

ansm

ittan

ce (

%)

Tran

smitt

ance

(%

)Tr

ansm

ittan

ce (

%)



above, it can be concluded that there is nodifference in functional groups amongstandard, commercial pectin and extractionresults with different temperatures.

CONCLUSIONS

The extraction temperature (65oC, 80oC,and 95oC) and extraction time (40, 60, and80 minutes) had no significant effect onmethoxyl content, galacturonic acid, equiva-lent weight, and pectin content, but the ex-traction time had a significant effect on theacetyl number and the degree of esterifica-tion. The highest yield of pectin was obtainedat extraction temperature of 80oC for 60minutes. The characteristics of cocoa podhusk pectin powder are brown, moisturecontent 10.56–11.96%, ash content 6.82–8.97%, methoxyl content 3.51–4.86%, galac-turonic acid content 41.38–88.40%, esteri-fication degree 10.76–19.96%, acetylnumber 14.55–20.90%, equivalent numbers664–1549, pectin content 9.52–19.51% andyield 5.55–7.70%. IR spectrum showed thatthere was no difference in the functionalgroups between standard, commercial, andpectin extracted at different temperatures.

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Characteristics of Pectin Extracted from Cocoa Pod Husks

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