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J. Inst. Eng. India Ser. A (June 2021) 102(2):469–478 https://doi.org/10.1007/s40030-021-00514-3 ORIGINAL CONTRIBUTION Effect of Process Parameters on Extraction of Pectin from Sweet Lime Peels 1 2 1 • • Arshi Siddiqui Khan Chand N. C. Shahi Received: 30 October 2020 / Accepted: 25 January 2021 / Published online: 5 April 2021 The Author(s) 2021 Abstract Pectin is a heterogeneous polysaccharide found Introduction in the cell wall, middle lamellae of many fruits and veg- etables, and is widely used as gelling agent, emulsifier and Waste utilization is one of the major concerns in the food stabilizer in food industry. In keeping the importance of processing industry and it has a great potential to provide pectin in the food industry, ultrasound-assisted extraction economic, social and environmental benefits to a country of pectin from sweet lime peel was investigated. The [5]. The waste from households accounts for 42% while individual and interactive effect of solid-solvent ratio, food manufacturing industry adds 39%, 14% losses occur ultrasound power intensity and sonication time on the in food service sector and 5% food waste during distribu- pectin yield, equivalent weight and methoxyl content were tion chain [14]. The inadequate waste management can studied and analyzed using multiple regression analysis. cause several health hazards as well as environmental The maximum pectin yield (36.4 g/100 g), equivalent issues. Hence, necessary steps should be taken to reduce weight (740.3 mg) and methoxyl content (7.1%) was waste levels and finding the most sustainable solution to obtained under optimal condition (solid-solvent ratio of manage the remaining waste. Food waste can be converted 1:24.3 g/ml, ultrasound power intensity of 80 W/cm and into high-value products such as antioxidants, bioactive, sonication time of 18.4 min). Significant (p \ 0.05) effect bioethanol, industrial enzyme, films, nutraceuticals, pig- of process parameters was found in all responses of pectin ments, protein, sugar, etc. which would provide certain extracted from sweet lime peel. It was also revealed from economic benefit for the agri-food sector and a positive the present study that ultrasound-assisted extraction of environmental impact [23]. Citrus fruit is one of the most pectin from sweet lime peel is an efficient approach toward extensively consumed and processed fruit in the world waste valorization and extraction of pectin with high yield which constitute about 18% of total world fruit production and good quality attributes. [10]. Citrus fruits are highly consumed as fresh produce and juice worldwide, and most commonly its peel is dis- Keywords Sweet lime peel Pectin carded as waste [19]. Due to both economic and environ- Ultrasound-assisted extraction and pectin yield mental factors, the disposal of citrus peel waste has considerable constraints. Thus, the conversion of citrus peel waste into valuable products provides both economic and environmental benefits. Citrus peels can be used as a & Khan Chand great source for the retrieval of pectin, bioactive com- kcphpfe@gmail.com pounds, organic acids, enzymes and essential oils [13]. Department of Post Harvest Process and Food Engineering, Citrus limetta is a species of citrus, commonly known as College of Technology, G.B. Pant University of Agriculture mosambi, sweet lime, sweet lemon and sweet limetta. It and Technology, Pantnagar, Uttarakhand 253145, India belongs to the family of ‘‘Rutaceau’’ and is the third largest Department of Agricultural Engineering, School of fruits produced in India. Sweet lime contains active phy- Agricultural Sciences and Rural Development, Central tochemicals that can protect health. It is also a rich source University of Nagaland, Medziphema, Dimapur, Nagaland of various nutrients like vitamin C and minerals that make 797106, India 123 470 J. Inst. Eng. India Ser. A (June 2021) 102(2):469–478 it one of the important commercial citrus fruit crops used Materials and Methods by juice processing industries [20]. In India, sweet lime juice is a favorite citrus drink, while its peel discarded as Materials and Reagents waste can be utilized for extraction of various value-added products. Sweet lime peel is considered as a rich and Sweet lime peel (10 kg, IMC 80%) was procured from the important pectin source. Pectin is the most widely used local market of Pantnagar, Uttarakhand. It was cleaned, polysaccharide in food industry, which can be extracted washed and dried using tray drier at 60 C for 48 h. The from peels of fruits. It is also used in pharmaceutical dried peel (2–3 kg) was ground using hammer mill (Make: industries as antitumor, antioxidant, antidiabetic and anti- Butex Engineering Company, Kanpur) and sieved into fine cancer drug [8]. Pectin is used as a good additive in jams, powder of size 300 microns. The obtained powder (1–2 kg) soft drinks and milk products [26]. Pectin is also used as fat was stored in sealed plastic bags prior to experiments. substitute in emulsified meat products, spreads, ice cream Citric acid was mixed in deionized water to prepare acidic and salad dressing [7]. Pectin is considered as an effective medium of pH 1.8 for pectin extraction. biomaterial film due to its biodegradability, biocompati- bility and non-toxicity [22]. Extraction is one of the Ultrasound-assisted Extraction of Pectin essential techniques which is used to recover pectin from various organic and inorganic wastes. Extraction technique Ten (10) grams dried sweet lime peel powder was weighed can be carried out by both conventional and non-conven- and mixed with the solvent (Citric acid) in the solid-solvent tional methods. However, the conventional extraction ratio (1:18, 1:24 and 1:30 g/ml) in the beaker. The mixture methods have numerous limitations like long processing solution was then placed under probe (20 mm diameter) of time, high energy requirement and high solvent consump- ultrasonication apparatus (Electronic industries model— tion with high amount of waste water generation. Thus EI—250, 230 VAC Single phase, 250 watts ultrasonic various novel approaches like microwave-assisted extrac- power) at ultrasound power intensity (48, 64 and 80 W/ tion, ultrasound-assisted extraction and enzyme-assisted cm ) and time (15, 25 and 35 min) combinations for extraction were developed for the extraction process [20]. extraction of pectin given in Table 1. After completion of Among various extraction techniques, ultrasound-assisted the set time of extraction, the suspension was filtered using extraction technique is considered more beneficial due to muslin cloth and centrifuged (8000 rpm for 15 min). The low energy consumption, shortened treatment time, less supernatant was precipitated with equal volume of ethanol solvent usage, increased safety of the operators, and and was left untouched for an hour. The coagulated pectin increased yield [2]. It is a non-thermal extraction technique was washed 2–3 times with ethanol to remove mono and in which sound waves, having frequencies higher than disaccharides. Extracted wet pectin was then dried in hot 20 kHz travel in matter and induce expansion and com- air oven at 45 C until it attains a constant weight. After pression cycles, leading to the formation of cavitation drying, the dry pectin mass was milled to powdered pectin bubbles. The collapse of cavitation bubbles near cell walls form and stored for analysis. induced by ultrasound produces cell disruption, thus causing stronger and enhanced solvent entrance into the Quantitative and Qualitative Analysis of Pectin cells and intensification of the mass transfer [24]. Ultra- sound-assisted extraction is widely used in food industry Yield Estimation due to its capability to induce chemical and physical changes of food components. Also, ultrasound processing The extraction yield is the amount of extract recovered in has some of the improvements on foods such as increased mass compared with the initial amount of whole plant. It is emulsifying capacity, release and diffusion of cell material a measure of efficiency of the solvent to extract specific and enhanced foaming [6]. Several authors already repor- components from the original material. The dry extract ted the extraction of pectin from various citrus fruits. obtained after filtration was weighed to get the extraction However, none research report has been found on the yield [21]. The yield of the extract calculated using ultrasound-assisted extraction of pectin from waste sweet formula: lime peel. Weight of Pectin Pectin Yieldðg=100gÞ¼ 100 Weight of drypowder Equivalent Weight Equivalent weight is an important physical property of pectin. It is the most important characteristic in 123 J. Inst. Eng. India Ser. A (June 2021) 102(2):469–478 471 Table 1 Box-Behnken design with the observed values for pectin yield, equivalent weight and methoxyl content of ultrasound-assisted extraction of pectin from sweet lime peel Factors Unit Levels -10 1 Solid-solvent ratio (X ) g/ml 1:18 1:24 1:30 Ultrasound power intensity W/cm 48 64 80 (X ) Sonication time (X ) Min 15 25 35 Exp. Solid-solvent Ultrasound power Sonication Pectin Yield (g/ Equivalent Weight Methoxyl Content no ratio intensity time 100 g) (mg) (%) (X , g/ml) (X , W/cm ) (X , min) 1 2 3 1 1:24 48 35 34.3 722.7 6.9 2 1:30 64 35 36.8 750.4 6.9 3 1:24 64 25 30.8 671.1 7 4 1:24 80 35 36.9 795.2 7.1 5 1:24 64 25 32.5 691.1 7 6 1:24 48 15 31.5 677 6.9 7 1:24 64 25 31.1 671.4 7 8 1:24 80 15 38.8 770.3 7.1 9 1:24 64 25 31.3 671.6 7 10 1:18 80 25 26.2 582.3 7 11 1:30 64 15 27.9 583.6 6.8 12 1:24 64 25 30.6 671.2 7 13 1:18 64 35 28.1 599.5 6.8 14 1:30 80 25 36.5 731.7 7 15 1:18 64 15 31.2 671.4 6.8 16 1:18 48 25 29.2 609.5 6.7 17 1:30 48 25 25.2 566.2 6.9 determining the functional behavior of pectin. 0.5 g sample the end point [21]. Methoxyl content was calculated using was taken in a 250 ml conical flask, and 5 ml ethanol was the equation: added. 1 g of sodium chloride to sharpen the end point and Volume of alkali Normality of alkali 3:1 Methoxyl contentðÞ % ¼ 100 ml of distilled water were added. Finally, 6 drops of Weight of sample phenol red were added and titrated against 0.1 N NaOH. Titration point was indicated by pink color [21]. Equivalent Statistical Design weight was calculated by the given formula: Three factors, three levels (-1, 0, 1) Box-Behnken design of response surface methodology was employed to inves- Weight of sample 1000 Equivalent weightðÞ mg ¼ tigate and optimize the effect of process variables on the Volume of alkali Normality of alkali yield and quality of pectin extracted from sweet lime peel, shown in Table 1. A total 17 experiments with 5 center Methoxyl Content points were designed using Design Expert software 10.0.1. The data collected were subjected to regression analysis to Methoxyl content was determined by saponification of the determine the existing relationship between independent pectin and titration of the liberated carboxyl groups. The and dependent variables. Each response was represented by neutralized solution obtained during the determination of a mathematical equation that correlates the response sur- equivalent weight was collected, and 25 ml of 0.25 N faces. The response was then expressed as second-order NaOH was added. The mixture was stirred thoroughly and polynomial equation kept at ambient temperature for 30 min. Then, 25 ml of 0.25 N HCl was added and titrated against 0.1 N NaOH to 123 472 J. Inst. Eng. India Ser. A (June 2021) 102(2):469–478 X X n n ultrasound power intensity at 80 W/cm and sonication Y= b þ b X þ b X 0 i ii i i¼1 i¼1 X X n n time at 35 min might be due to higher ultrasound power þ b X X ii i j i¼1 j¼i¼1 intensity which facilitates the release of higher amount of pectin. However, the lower equivalent weight was obtained where, under experimental conditions of solid-solvent ratio of Y = response, b b b are regression coefficients and 0, i, ii 1:30 g/ml, ultrasound power intensity at 48 W/cm and n = number of independent variables (n = 3). X and X i j- sonication time at 25 min. This reduction could be due to = independent variables (where, i =1, 2, …n and j =1, 2 higher partial degradation of pectin during extraction. …n). Similarly, the methoxyl content of extracted pectin varied from 6.7 to 7.1%, as experiment no. 4 and 16 had the maximum and minimum value of methoxyl content, Results and Discussion respectively. The maximum methoxyl content was obtained under experimental conditions of solid-solvent Analysis of Pectin Yield, Equivalent Weight ratio of 1:24 g/ml, ultrasound power intensity at 80 W/cm and Methoxyl Content and sonication time at 35 min. The higher value of meth- oxyl content might be because of the presence of more free As results given in Table 1, Box-Behnken design was esterified carboxyl group in the pectin. On the other hand, employed to optimize the variables of ultrasound-assisted the minimum methoxyl content was obtained at experi- extraction process (UAE) and examine their effects on the mental conditions of solid-solvent ratio of 1:18 g/ml, responses (pectin yield, equivalent weight, methoxyl con- ultrasound power intensity at 48 W/cm and sonication tent). The results indicated that the pectin yield was in the time at 25 min. The lesser solid-solvent ratio and ultra- range 25.2–38.8 g/100 g, as experiment no. 17 and 8 had sound power intensity leads pectin having less free esteri- the lowest and highest yield, respectively. The maximum fied carboxyl group present in the pectin chain and thus pectin yield was found under the experimental conditions lower the methoxyl content. Therefore, optimal process of solid-solvent ratio of 1:24 g/ml, ultrasound power 2 conditions were investigated in order to obtain the maxi- intensity at 80 W/cm and sonication time 15 min. The mum extraction yield, equivalent weight and methoxyl maximum pectin yield might be due to the maximum level content of pectin extracted from sweet lime peel using of ultrasound power intensity and the low pH extracting ultrasound-assisted extraction technique. The maximum solvent used in the extraction process. At sufficiently production of pectin was obtained at solid-solvent ratio of higher ultrasound power intensity, UAE increases rupture 1:24.3 g/ml, ultrasound power intensity of 80 W/cm and of sweet lime cell wall matrix, leading to better interactions sonication time of 18.4 min as shown in Fig. 1 and 2. between solvent and extracted material and thus increased the pectin yield. Also, the lower acidic extraction solvent Statistical Analysis of Pectin Yield, Equivalent has the ability to contact directly with the insoluble pectin Weight and Methoxyl Content and favored the hydrolysis of the insoluble pectin con- stituents into soluble pectin, thus increasing the pectin The statistical significance of the proposed quadratic model yield [12]. However, the minimum pectin yield was for pectin yield, equivalent weight and methoxyl content obtained under the experimental conditions of solid-solvent ratio of 1:30 g/ml, ultrasound power intensity at 48 W/cm and sonication time at 25 min. This might be due to the higher solid-solvent ratio and lower ultrasound power intensity levels. The higher solid-solvent ratio affects the extraction yield negatively and also it complicates the recovery of pectin during the further extraction step by alcohol precipitation. Thus, further increment in solid-sol- vent ratio leads to decrement in pectin yield. Similar effect was observed for ultrasound-assisted extraction of pectin from pomegranate peel [16]. The equivalent weight of extracted pectin was found to be ranged from 566.2 to 795.2 mg. The maximum and minimum value of equiva- lent weight was found in experiment no. 4 and 17, respectively. The higher equivalent weight obtained at experimental conditions of solid-solvent ratio of 1:24 g/ml, Fig. 1 Extracted wet pectin in jelly form 123 J. Inst. Eng. India Ser. A (June 2021) 102(2):469–478 473 Pectin Yield ¼ 31:26 þ 1:46X þ 2:28X þ 0:84X þ 3:57X X 1 2 3 1 2 100g 2 2 2 þ 3:00X X 1:17X X 3:18X þ 1:19X þ 2:92X 1 3 2 3 1 2 3 ð1Þ Equivalent weightðÞ mg ¼ 675:28 þ 21:15X þ 38:01X 1 2 þ 20:69X þ 48:18X X 3 1 2 þ 59:68X X 71:46X 1 3 2 2 þ 18:61X þ 47:41X 2 3 ð2Þ Methoxyl contentðÞ % ¼ 7:04 þ 0:040X þ 0:11X þ 0:023X 0:042X X 1 2 3 1 2 2 2 2 þ 0:018X X 0:016X X 0:15X þ 0:033X 0:053X 1 3 2 3 1 2 3 ð3Þ The sign and magnitude of the coefficients in above Fig. 2 Dried pectin in powder form Eqs. (1, 2 and 3) indicate the effect of the significant independent variables on the responses. From the above was evaluated by ANOVA, and the results were listed in equations, it was observed that the positive coefficient of Table 2. In this analysis, the F value of model for the pectin solid-solvent ratio (X ), ultrasound power intensity (X ) and yield, equivalent weight and methoxyl content was 32.75, 1 2 sonication time (X ) signified the increase in the pectin 79.70 and 1173.89, which was associated with p value yield, equivalent weight and methoxyl content, of \ 0.0001 in all the responses. The high F value and low respectively, with increase in level of these parameters. p value indicated that all the proposed models are extre- However, the larger coefficient of ultrasound power mely significant and the responses were significantly intensity (X ) showed the higher effect on all the affected by the extraction factors. Also, lack of fit value for 2 responses in comparison with other independent regression models was not found significant, which indi- variables. In Eq. 1, the positive coefficient of combined cated that the model equation was adequate to describe the effect of solid-solvent ratio and ultrasound power intensity pectin yield, equivalent weight and methoxyl content. In (X X ) and solid-solvent ratio and sonication time (X X ) addition, R value for pectin yield, equivalent weight and 1 2 1 3 on the pectin yield suggests that pectin yield increases methoxyl content was 0.9768, 0.9903 and 0.9993, respec- when high level of solid-solvent ratio was used with high tively, which implies that the model could account for level of ultrasound power intensity and when high level of 97.68%, 99.03% and 99.93% data, respectively. For better solid-solvent ratio was used with high level of sonication suitability of the model, the difference between the pre- time, respectively. However, the negative coefficient of dicted and adjusted coefficient of determination should be combined effect of ultrasound power intensity and less than 0.2, the adequate precision should be greater than sonication time (X X ) on the pectin yield suggests that it 4 and whereas coefficient of variation should not exceed 2 3 decreases when high ultrasound power intensity was used 10%. In this case, ‘‘Pred R ’’ of 0.7603, 0.9067 and 0.9911 with increased sonication time. At quadratic level, the was in reasonable agreement with the ‘‘Adj R ’’ of 0.9470, negative coefficient of solid-solvent ratio (X ) showed that 0.9779 and 0.9985, respectively for pectin yield, equivalent pectin yield decrease with increase in level of this weight and methoxyl content. The adequate precision parameter. However, at quadratic level, the positive values of 19.038, 30.683 and 111.632 and the coefficient of coefficient of ultrasound power intensity (X ) and variation of 2.83%, 1.50% and 0.066% were calculated for 2 sonication time (X ) signified that when its level pectin yield, equivalent weight and methoxyl content, increased the pectin yield also increased. Similarly, in respectively, thereby verifying the accuracy suitability of Eq. 2, at interactive level, the positive coefficient of X X model. The coefficient of determination (R ) and adjusted 1 2 and X X suggests that the equivalent weight increases determination coefficient (Adj R ) were reasonably close to 1 3 when solid-solvent ratio was used with high level of 1, indicating a high degree of correlation between the ultrasound power intensity and when high level of solid- observed and predicted values. solvent ratio was used with high level of sonication time, Based on these results, the surface models for yield, respectively. At quadratic level, the negative coefficient of equivalent weight and methoxyl content of pectin extracted solid-solvent ratio (X ) showed that equivalent weight from sweet lime peel using ultrasound-assisted extraction 1 decrease with increase in level of this parameter. However, technique were formulated as given below at quadratic level, the positive coefficient of ultrasound 2 2 power intensity (X ) and sonication time (X ) signified 2 3 123 474 J. Inst. Eng. India Ser. A (June 2021) 102(2):469–478 Table 2 Analysis of variance (ANOVA) for the regression model of pectin yield, equivalent weight and methoxyl content Source Pectin yield Equivalent weight Methoxyl content Sum of Df Mean F Value p value@Prob [ F Sum of Df Mean F Value p value@Prob [ F Sum of Df Mean F Value p value@Prob [ F Square Square Square Square Square Square Model 237.25 9 26.36 32.75 \ 0.0001** 73,009.99 9 8112.22 79.70 \ 0.0001** 0.22 9 0.025 1173.89 \ 0.0001** Solid-solvent 17.11 1 17.11 21.26 0.0025** 3578.58 1 3578.58 35.16 0.0006** 0.013 1 0.013 608.28 \ 0.0001** ratio (X ) Ultrasound 41.41 1 41.41 51.44 0.0002** 11,559.60 1 11,559.60 113.58 \ 0.0001** 0.089 1 0.089 4231.46 \ 0.0001** power intensity (X ) Sonication 5.61 1 5.61 6.97 0.0334* 3423.78 1 3423.78 33.64 0.0007** 0.0043 1 0.0043 205.51 \ 0.0001 time (X ) X X 51.12 1 51.12 63.51 \ 0.0001** 9283.32 1 9283.32 91.21 \ 0.0001** 0.0069 1 0.0069 327.38 \ 0.0001** 1 2 X X 36.00 1 36.00 44.72 0.0003** 14,244.42 1 14,244.42 139.95 \ 0.0001** 0.0013 1 0.0013 58.21 0.0001** 1 3 X X 5.52 1 5.52 6.86 0.0344* 108.16 1 108.16 1.06 0.3369 0.001 1 0.001 48.66 0.0002** 2 3 X 42.58 1 42.58 52.90 0.0002** 21,504.19 1 21,504.19 211.28 \ 0.0001** 0.090 1 0.090 4256.42 \ 0.0001** X 6.01 1 6.01 7.47 0.0292* 1458.24 1 1458.24 14.33 0.0068** 0.0045 1 0.0045 213.30 \ 0.0001** X 35.90 1 35.90 44.60 0.0003** 9464.03 1 9464.03 92.99 \ 0.0001** 0.012 1 0.012 558.88 \ 0.0001** Residual 5.63 7 0.80 712.46 7 101.78 0.00015 7 0.000021 Lack of Fit 3.42 3 1.14 2.06 0.2478 399.47 3 133.16 1.70 0.3035 0.00012 3 0.00004 6.00 0.0582 Pure Error 2.21 4 0.55 312.99 4 78.25 0.000027 4 0.0000067 Cor Total 242.88 16 73,722.44 16 0.22 16 R 0.9768 0.9903 0.9993 Adj R 0.9470 0.9779 0.9985 Pred R 0.7603 0.9067 0.9911 Adeq 19.038 30.683 111.632 Precision C.V. % 2.83 1.50 0.066 **Significant at 1% level of significance, *Significant at 5% level of significance J. Inst. Eng. India Ser. A (June 2021) 102(2):469–478 475 that when its level increased, the equivalent weight also weight could be due to higher partial degradation of pectin increased. Additionally, in Eq. 3, the positive coefficient of during extraction [11]. Fig. 3e showed that the equivalent X X suggests that the methoxyl content increases when weight increased rapidly when solid-solvent ratio increased 1 3 high level of solid-solvent ratio was used with high level of from 1:18 to 1:24 g/ml with the increase in sonication time sonication time. However, the negative coefficient of X X from 15 to 35 min, while it decreased further at the highest 1 2 and X X suggests that the methoxyl content decreases value of solid-solvent ratio along with the lower value of 2 3 when high level of solid-solvent ratio was used with sonication time. In this study, the equivalent weight of increased ultrasound power intensity and when high pectin ranged almost in the range of International Pectin ultrasound power intensity was used with increased Producers Association standard of 600–800 mg [9]. sonication time, respectively. At quadratic level, the The methoxyl content in pectin has important role in 2 2 negative coefficient of X and X showed that methoxyl determining the functional properties of pectin and the 1 3 content decrease with increase in level of solid-solvent structure and texture of the pectin gel. Methoxyl content is ratio and sonication time, respectively. However, at the number of moles of methyl alcohol in 100 mol galac- quadratic level, the positive coefficient of X signified turonic acids. Methoxyl content is an important factor in that when the level of ultrasound power intensity increased, controlling the setting time of pectin and the ability of the the methoxyl content also increased. pectin to form gels [3]. Methoxyl content of the extracted pectin in the present study ranged between 6.7 and 7.1%, Analysis of 3 D Graphs of pectin Yield, Equivalent which almost meet the standard of 2.5–7.2% [9]. It was Weight and Methoxyl Content observed that the methoxyl content of the extracted pectin in the present study was higher than the methoxyl content For better understanding, the effect of processing param- reported as 4.11% for lime, 3.9% for orange and 4.2% for eters (solid-solvent ratio, ultrasound power intensity and grapefruit by Mohamed [15]. Figure 3f–h) shows the sonication time) on the pectin yield, equivalent weight and behavior of solid-solvent ratio, ultrasound power intensity methoxyl content was evaluated and illustrated by three- and sonication time on the methoxyl content value. Fig- dimensional plots (3D) in Fig. 3. Ultrasound power inten- ure 3f represents that the higher methoxyl content was sity was one of the effective factors in ultrasound-assisted found at the higher levels of ultrasound power intensity extraction technique since the maximum pectin yield was (80 W/cm ) and solid-solvent ratio of 1:24 g/ml. Also, observed at higher level of ultrasound power intensity with pectin with higher methoxyl content values could be increase in solid-solvent ratio (Fig. 3a). This increase in obtained around the central values of solid-solvent ratio pectin yield might be because of the disruption of cell wall and sonication time (Fig. 3. However, the further increase and release of cellular material at sufficient higher ultra- in both the variables reduced the methoxyl content due sound power intensity by De Oliveira et al. [4]. Fig. 3b likely to chain cleavage into smaller fragments of pectin showed that the pectin yield increased with increase in molecule [1]. Fig. 3h displayed that the methoxyl content solid-solvent ratio and sonication time. This increase might increased with the increase in ultrasound power intensity be because of the increasing time that offers more reaction and sonication time. This increase might be due to the opportunity with the solvent. Longer contact time between higher effect of ultrasound power intensity. Ultrasound the extractor and the plant materials provide greater mass power intensity plays an important role in breaking up the transfer from the solid particles into the solution. In addi- vegetal tissue and thus enhanced the extraction yield which tion, higher solid–liquid ratio favors the yield by increasing in turn increase the quality attributes [25]. the contact surface of the plant material with the solvent and enhances the swelling of the material, leading to cell disruption and thereby facilitates the solubilization of Conclusion pectin [18]. Equivalent weight is an important response to check out As per the current scenario of production of sweet lime the quality characteristics of the sweet lime peel pectin. peel at small juice extraction units and household, most of Equivalent weight of pectin is the total content of free the peel is discarded as waste without the knowledge of the galacturonic acid (not esterified) in the molecular chains of extraction of pectin from the waste. It is apparent from the pectin [21]. The increased or decreased equivalent weight present study that pectin was extracted from the sweet lime might be dependent upon the amount of free acid [17]. The peel using ultrasound-assisted extraction technique which higher equivalent weight might be due to higher ultrasound is proved to be an efficient extraction technique because of power intensity which facilitates the release of higher its reduced extraction time, lower use of solvent, less amount of pectin, which will increases the equivalent consumption of power and improved yield of extraction. weight of pectin (Fig. 3d). However, the lower equivalent The best optimum conditions were obtained as solid- 123 476 J. Inst. Eng. India Ser. A (June 2021) 102(2):469–478 Fig. 3 3D plots showing the effect of processing variables on pectin yield, equivalent weight and methoxyl content 123 J. Inst. Eng. India Ser. A (June 2021) 102(2):469–478 477 Fig. 3 continued food and natural products. Mechanisms, techniques, combina- solvent ratio of 1:24.3 g/ml, ultrasound power intensity of tions, protocols and applications: a review. Ultrason. Sonochem. 80 W/cm and sonication time of 18.4 min to produce 34, 540–560 (2017) maximum pectin. Under these conditions, the maximum 3. D. Constenla, J.E. Lozano, Kinetic model of pectin demethyla- pectin yield, equivalent weight and methoxyl content were tion. Latin Am. Appl. Res. 33(2), 91–95 (2003) 4. C.F. De Oliveira, D. Giordani, R. Lutckemier, P.D. Gurak, F. 36.4 g/100 g, 740.3 mg and 7.1%, respectively. Cladera-Olivera, L.D.F. Marczak, Extraction of pectin from passion fruit peel assisted by ultrasound. LWT-Food Sci. Tech- Acknowledgements We, the authors would like to thank Dean nol. 71, 110–115 (2016) College of Technology and Head, Department of PHPFE, 5. G. Garcia-Garcia, J. Stone, S. Rahimifard, Opportunities for GBPUA&T, Pantnagar, India for providing research facilities, waste valorisation in the food industry–A case study with four financial support and technical assistance for extraction of pectin from UK food manufacturers. Journal of Cleaner Production 211, sweet lime peel. Also thank to Coordinator, Technical Education 1339–1356 (2019) Quality Improvement Programme (TEQIP-III) College of Technol- ˇ ´ ´ ´ 6. A.N. Grassino, M. Brncic, D. Vikic-Topic, S. Roca, M. Dent, ogy, Pantnagar for sanctioning the grant for conducting the research ˇ ´ S.R. Brncic, Ultrasound assisted extraction and characterization work. of pectin from tomato waste. Food Chem. 198, 93–100 (2016) 7. S.B. Hawthorne, C.B. Grabanski, E. Martin, D.J. 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Biol. Macromol. 147, 1107–1115 (2020) Publisher’s Note Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.
Journal of The Institution of Engineers (India): Series A – Springer Journals
Published: Apr 5, 2021
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