Thammasat Int. J. Sc. Tech., Vol.

13 Special Edition, November 2008

Extraction of Pectin from Sugar Palm Meat

Pornpen Yujaroen, Udomsri Supjaroenkul and Supitcha Rungrodnimitchai* Department of Chemical Engineering, Faculty of Engineering, Thammasat University, Rangsit Campus, Pathum Thani, 12121, Thailand, *tsupitch@engr.tu.ac.th

Abstract
Not only is pectin recognized for its properties as natural gelling agents and thickener in a wide variety of products, it also offers both healthy and protective advantages for consumers. Pectin is known to have a unique property being a water soluble fiber. It has been known to help fight against many diseases such as diabetes, obesity and arteriosclerosis. In this paper, we used sugar palm as a raw material to extract pectin, for the reason that there are abundant sugar palms in Thailand and there is plenty of pectin in the meat of sugar palm shell. This paper investigates various factors that affect the yield of extraction of pectin from sugar palm, which are pretreatment of raw material, ratio of water in extraction, pH of solution, temperature of solution and time of heating to find the optimal condition to extract pectin from sugar palm. The highest extraction rates from our experiments occurred when pectin was in C2H5OH at 60oC for 30 min and extracted using a water: sugar palm ratio of 40:1 (wt: wt) a pH 4-6 at 80oC for 2 hrs. The above condition gave 20% of pectin per weight of sugar palm meat. Keywords: pectin, sugar palm, pretreatment, extraction, water soluble fiber

1. Introduction
Pectin is a polymeric carbohydrate which has a high molecular weight and is present in all plants, consisting mainly of galacturonic acid. The carboxyl groups of the polygalacturonic acid are partly esterified by methanol or are amidated [2]. Commercial pectin is obtained from the peel of citrus fruits (lemon, lime and orange) or from apple pomace. These raw materials are used because they produce pectin of superior quality, contain a relatively large amount of pectin and are available in sufficient quantities to make them commercially available. Pusaran investigated extraction of pectin from guava, papaya, pineapple, peel of lemon and orange. The peel of lemon was found to give the highest yield of 25.30% per dry weight [3]. Chang reported about extraction of pectin from sunflowers which have yield of pectin at 7.6% [4]. On the other hand, it was reported that pectin from peel of mandarin citrus had yield of pectin at 7.5 % [5]. Each year, Thailand has to import at least 200 million baht valued-pectin because it is not able to produce pectin in the country. In this paper we used sugar palm as a raw material to extract pectin, for the reason that there is abundant sugar palm in Thailand and is an industrial crop, whose every part can be utilized. In the past, people in local areas diluted ripe meat of sugar palm meat in water and added calcium hydroxide solution. The solution becomes solid gel, which is the phenomenon found in pectin. This gave us the idea that there would be plenty of pectin in meat of sugar palm shell. This paper aims to investigate various factors that affect the yield of pectin extraction from sugar palm meat such as pretreatment methods, soaked to water ratio, pH, temperature, extraction time, and to determine the optimal conditions for the extraction.

2. Experimental
2.1 Raw Material 2.1.1. Yellow sugar palm meat (from Saraburi province, Thailand) 2.1.2. Sodium hydroxide (Ajax Fine Chem) 2.1.3. Hydrochloric 37% (Carlo Erba) 2.1.4. Ethyl alcohol 95% (commercial grade A)

2.2 Methods
In this research, yellow ripe sugar palm meat was used as a raw material in the extraction of pectin. Extractions were

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performed in laboratory scaled by standard separation techniques. The apparatus was normal 1000 ml-beaker, filtration set, rotary evaporator, dry oven, etc. Generally, there are nine steps of pectin extraction as shown below. Step 1 pretreatment of raw material (20 g: 1 sample) Step 2 mixing sample with deionized water (ratio as shown in table 2) Step 3 adjusting pH of solution by 0.25 N HCl (aq) or 0.25 N NaOH (aq) Step 4 heating and stirring solution Step 5 filtering residue (cheesecloth) Step 6 removing water from the filtrate with rotary evaporator to give 100 ml solution Step 7 adding 300 ml of C2H5OH to recrystallize pectin from the solution Step 8 filtering gel (Whatman 41) and transfer to crucible Step 9 dry at 70oC for 26 hrs Figure 1. Flow diagram of pectin extraction from yellow ripen sugar palm meat. After the drying process the obtained yellow pectin was weighed. The effects of five factors were investigated. The first was the raw material pretreatment methods, in which 4 different methods (Method A-D) were tested as summarized in Table 1. The four studied variables are deionized water to sample weight ratio (10:1, 20:1, 30:1, 40:1 and 50:1), extraction temperature (30, 60, 80, and 100oC), pH (2, 4, 6 and 8), and time of extraction (0.5, 1, 2, and 3 hrs). The extraction conditions for different experimental runs are summarized in Table 2. 2.2.1 Effect of pretreatment of raw material (Method A-D) Raw material was sliced and weighed (20 g for one sample). The pretreatment of sugar palm meat was done in four groups (Method AD).

Table 1 Pretreatment methods

Methods Method A Method B Method C Method D pretreatment methods no pretreatment Sample was frozen at -20oC for 24 hrs. Sample was steamed for 20-30 min. Sample was soaked in 60 ml of C2H5OH for 30 min before removing C2H5OH.

Table 2 Experimental plan for pectin extraction from sugar palm meat
Ratio of water to palm meat by weight 20 : 1 Temperature (oC) 30 Time (hrs.) 0.5

Pretreatment Method A Method B Method C Method D Method D1 Method D2 Method D3 Method D4 Method D5 Method D6 Method D7 Method D8 Method D9 Method D10 Method D11 Method D12 Method D13 Method D14 Method D15 Method D16 Method D17

pH

4-6

10:1 20:1 30:1 40:1 50:1 30:1

60

30 60 80 100 80

30:1

2 4 6 8 8

30:1

80

0.5 1 2 3

2.2.2 Effect of deionized water to sugar palm meat weight ratio (Method D1-D5) The samples were mixed with deionized water into five ratios (10, 20, 30, 40 and 50 times of weight of samples). 2.2.3 Effect of temperature of solution (Method D6-D9) The samples were mixed with deionized water and were heated at room temperature, 60, 80 or 100oC. 2.2.4 Effect of pH of solution (Method D10D13) The samples were mixed with deionized water and pH was adjusted to 2, 4, 6 or 8. 2.2.5 Effect of heating and stirring time (Method D14-D17) The pH of palm meat solutions was adjusted to 8 and were heated at 80oC for 0.5, 1, 2 or 3 hrs.

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The yield calculated by

of

pectin

extraction

was

% pectin = weight of obtained pectin x 100 weight of dry sugar palm meat .

3. Results and discussions

3.1 Effect of pretreatment methods (Method A-D)

From Fig. 3, it can be concluded that as the ratio of water in the extraction increased, percent of pectin was also increased. However, since the yield of extraction by using 40 times and 50 times of deionized water had no significant difference, to use 40 times of water, or lower water might be better because of ease of operation. 3.3 Effect of temperature of solution (Method D6-D9)

Figure 2 Effect of pretreatment methods on performance of pectin extraction. According to Figure 2, pretreatment by adding ethanol to raw material and heating at 60oC for 30 minutes gave the highest percent of pectin (10.04%). The percent of pectin for nontreatment condition and steaming raw material for 20-30 minutes were 9.74 and 9.29%, respectively. The lowest percent of pectin was found by using freezing condition (5.74%). Washing by C2H5OH has an advantage in that the yellow color can be removed without leaching out of pectin. Therefore, the optimal condition of pretreatment of raw material was done by adding ethanol and heating at 60oC for 30 minutes. 3.2 Effect of the weight ratio of deionized water to sample (Method D1-D5)

D 6

D 7

D 8

D 9

Figure 4 Effect of the temperature of solution on performance of pectin extraction. From Fig. 4, it can be concluded that the optimal temperature of solution for extraction is 80oC. It is considered that if temperature of solution for extraction is higher than 80oC the percent of pectin decrease because of decomposition, which would be discussed later. On the other hand, lower temperature might not be enough to assist dissolution of pectin. 3.4 Effect of pH of solution(Method D10-D13)

D 10 D 1 D 2 D 3 D 4 D 5

D 11

D 12

D 13

Figure 5 Effect of pH of solution on performance of pectin extraction. It can be seen from Fig. 5 that base solution (pH 8) yielded the highest percent of pectin (14.15%) but pectin gel was not viscous. In acid solution pH 2 yielded the highest percent of pectin (11.77%) but after drying process, color of pectin turned into black and became

Figure 3 Effect of the weight ratio of deionized water to sample on performance of pectin extraction.

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dissoluble in water. It seems that too strong acid or basic condition would destroy the nature of pectin. Consequently, the optimum pH for pectin extraction should be around pH 4-6. The percent of pectin at pH 4 and 6 were 9.81 and 11.35 % respectively. 3.5 Effect of heating and stirring time (Method D14-D17)

4. Conclusion
We succeeded in extraction of pectin from sugar palm. The best condition for extraction of pectin is to immerse the raw material in C2H5OH at 60oC for 30 min and extract by 40 times of water to the weight of sugar palm meat at pH 46 at 80oC for 2 hrs, which gave a yield of 25.30% per weight of dry sugar palm meat. We found that too high temperature or too long extraction time in acid or basic condition was not appropriate for pectin extraction. The results suggest that sugar palm has potential as a new pectin industrial source.

D 14

D 15

D 16

D 17

5. References
[1] Roy L.Whister and James N.BeMiller, Carbohydrate Chemistry for Food Scientists, Eaganpress St. Paul, Minnesota, USA, 1997. [2] Severian Dumitriu, Polysaccharides Structural Diversity and Functional Versatility, Marcel Dekker; Inc. New York. [3] Puosaran,T., Extraction of Pectin from Guava, Papaya, Pineapple, Peel of Lemon and Orange, Master thesis, Kasetsart University, 2520. [4] Chang, Extraction and Physicochemical Characterization of Pectin from Sunflower Head Residues, Journal of Food Science. Vol.57, No.6, pp.1439-1442, 1992. [5] Kim, D.H. and others, Physiochemical Characterization of pectin Extracted from Cheju Mandarin (Citrus unshiu) Peels with Citric Acids, Food Science and Biotechnology. Vol.9, No.2, pp.95-98, 2000.

Figure 6 Effect of time of heating and stirring on performance of pectin extraction. From fig. 6, it can be estimated that the optimal time of heating is 2 hrs. If the time is longer than 2 hrs pectin will decompose. On the other hand, lower time might not be enough to assist dissolution of pectin. Too high temperature and too long extraction time would lead to decomposition of pectin. Since pectin is composed of -(1-4) linked units of galacturonic acid or methyl ester as shown Figure 7. The glycosidic bond is one kind of ether bond, so that it can go through hydrolysis reaction at the right conditions (at high temperature of pH 2, or at pH 8 for a long time). In this case, it is considered that by hydrolysis of high polymer of pectin molecules to low polymer leads to an increase of solubility in water, which makes it more difficult to separate pectin as a solid compound by addition of C2H5OH.

Glycosidic bond Figure 7 Chemical structure of pectin.

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