Extraction, Characterization, and Antioxidant Activity of Pectin from Lemon Peels.

Pectin is a natural polymer that is found in the cell walls of higher plants. This study presents a comprehensive analysis of pectin extracted from lemon in two different geographic regions (Peddie and Fort Beaufort) in two consecutive years (2023 and 2024) named PP 2023, PP 2024, FBP 2023, and FBP 2024. The dried lemon peels were ground into a powder, sifted to obtain particles of 500 µm, and then subjected to pectin extraction using a conventional method involving mixing lemon peel powder with distilled water, adjusting the pH level to 2.0 with HCl, heating the mixture at 70 °C for 45 min, filtering the acidic extract, and precipitating pectin with ethanol. The yield of these pectin samples was statistically significant, as FBP 2024 had a maximum yield of 12.2 ± 0.02%, PP 2024 had a maximum yield of 13.0 ± 0.02%, FBP 2023 had a maximum yield of 12.2 ± 0.03%, and PP 2023 had a maximum yield of 13.1 ± 0.03%, The variation in yield could be due to the differences in the growing conditions, such as the climate and soil, which could have affected the pectin content in the lemons. The physicochemical characterization of all samples proved that our pectin samples could be used in the pharmaceutical and food industries, with anhydrouronic acid content which was greater than 65%, as suggested by the FAO. The scanning electron microscope analysis of all extracted pectin was rough and jagged, while the commercial pectin displayed a smooth surface morphology with a consistent size. FTIR confirmed the functional groups which were present in our samples. Thermogravimetric analysis was employed to investigate the thermal behavior of the extracted pectin in comparison with commercial pectin. It was found that the extracted pectin had three-step degradation while the commercial pectin had four-step degradation. Additionally, pectin samples have been shown to have antioxidants, as the IC50 of PP 2024, PP 2023, FBP 2023, FBP 2024, and Commercial P was 1062.5 ± 20.0, 1201.3 ± 22.0, 1304.6 ± 19.0, 1382.6 ± 29.9, and 1019.4 ± 17.1 mg/L, respectively. These findings indicate that lemon pectin has promising characteristics as a biopolymer for use in biomedical applications.

Physicochemical and functional properties of pectin extracted from the edible portions of jackfruit at different stages of maturity.

BACKGROUND: The physicochemical and functional properties of pectin (JFP) extracted from edible portions (including pericarp and seed) of raw jackfruit (an underutilized tropical fruit) at four different maturity stages (referred to as stages I, II, III, and IV) were characterized in terms of extraction yields, chemical composition, molecular weight, and antioxidant properties to evaluate its potential use in foods. RESULT: The JFP yield increased from 9.7% to 21.5% with fruit maturity, accompanied by an increase in the galacturonic acid content (50.1%, 57.1%, 63.6%, and 65.2%) for stages I-IV respectively. The molecular weight increased from 147 kDa in stage I to 169 kDa in stage III, but decreased to 114 kDa in stage IV, probably due to cell-wall degradation during maturation. The JFP was of the high methoxyl type and the degree of esterification increased from 65% to 87% with fruit maturity. The functional properties of JFP were similar to or better than those reported for commercial apple pectin, thus highlighting its potential as a food additive. Although the phenolics and flavonoids content of JFP decreased with fruit maturity, their antioxidant capacity increased, which may be correlated with the increased content of galacturonic acid upon fruit development. Gels prepared from JFP showed viscoelastic behavior. Depending on the maturity stage in which they were obtained, different gelation behavior was seen. CONCLUSION: The study confirmed the potential of pectin extracted from edible parts of jackfruit as a promising source of high-quality gelling pectin with antioxidant properties, for food applications. © 2022 Society of Chemical Industry.

Modeling the influence of extraction parameters on the yield and chemical characteristics of microwave extracted mango (Mangifera indica L.) peel pectin by response surface methodology.

Extraction is considered to be a critical unit operation to recover bioactive compounds from the in-situ state of many plant-based food processing wastes. The characteristics of pectin were predicted to vary with the source of raw material, extraction and post-extraction conditions. The study was focused to investigate the optimal conditions for extracting mango peel pectin (MPP) with increased yield and quality by microwave-assisted extraction (MAE). Box Behnken experimental design was used to model the influence of extraction parameters (microwave power, pH, and time) on the responses (yield, esterification degree, equivalent weight, anhydrouronic acid, and methoxyl content of pectin). The predicted models were adequately fitted to the experimental data (p ≤ 0.001) for all the response variables. A higher yield of pectin with better quality was obtained with optimal conditions of microwave power 606 watts (W), extraction time 5.15 min, and pH 1.83. The MPP obtained is categorized as low-methoxyl pectin as the range for the degree of esterification (DE) at all possible treatment variations remained below 50%. The study revealed that mango peel was an effective alternative source of pectin which could be extracted by microwave method on large scale.

Optimization of calcium pectinate gel production from high methoxyl pectin.

BACKGROUND: Calcium pectinate (CaP) gel is traditionally prepared by de-esterifying high methoxyl pectin (HMP) to low methoxyl pectin (LMP), followed by gelation with calcium. To save both time and cost in the production of CaP gel, an alternative method was developed by the addition of CaCl2 to HMP at alkaline pH. To optimize the production, response surface methodology (RSM) was used to investigate the effects of temperature (30-50 °C), time (20-40 min) and pH (8-10) on yield, calcium content of the CaP gel and the degree of esterification (DE) of pectin following decalcification of CaP (DC-pectin). RESULTS: The linear term for pH had a significant effect (P < 0.01) on all three responses, whereas interaction effects were not significant (P > 0.01), except on the calcium content (P < 0.01). The optimized process conditions (temperature, time and pH) to obtain maximum CaP-HMP gel yield (88.83%) were 50 °C, 40 min and pH 9.6, and for the highest calcium content (97.23 mg g-1 ) they were 40 °C, 30 min and pH 9.7. DC-pectin was a typical LMP with DE varying from 26.92% to 50.33%. The DE of DC-pectin could be predicted by a model that proved significant (R2  = 0.9888). CONCLUSION: The optimum conditions were established to produce CaP gels from HMP with high yield and calcium content. Also, LMP with predictable DE can be produced following a significant model. This study provides new insights into the production and application of CaP gel. © 2021 Society of Chemical Industry.

Interactions between cell wall polysaccharides and polyphenols: Effect of molecular internal structure.

Cell wall polysaccharides (CPSs) and polyphenols are major constituents of the dietary fiber complex in plant-based foods. Their digestion (by gut microbiota) and bioefficacy depend not only on their structure and quantity, but also on their intermolecular interactions. The composition and structure of these compounds vary with their dietary source (i.e., fruit or vegetable of origin) and can be further modified by food processing. Various components and structures of CPSs and polyphenols have been observed to demonstrate common and characteristic behaviors during interactions. However, at a fundamental level, the mechanisms that ultimately drive these interactions are still not fully understood. This review summarizes the current state of knowledge on the internal factors that influence CPS-polyphenol interactions, describes the different ways in which these interactions can be mediated by molecular composition or structure, and introduces the main methods for the analysis of these interactions, as well as the mechanisms involved. Furthermore, a comprehensive overview is provided of recent key findings in the area of CPS-polyphenol interactions. It is becoming clear that these interactions are shaped by a multitude of factors, the most important of which are the physicochemical properties of the partners: their morphology (surface area and porosity/pore shape), chemical composition (sugar ratio, solubility, and non-sugar components), and molecular architecture (molecular weight, degree of esterification, functional groups, and conformation). An improved understanding of the molecular mechanisms that drive interactions between CPSs and polyphenols may allow us to better establish a bridge between food processing and the bioavailability of colonic fermentation products from CPSs and antioxidant polyphenols, which could ultimately lead to the development of new guidelines for the design of healthier and more nutritious foods.

Physicochemical properties of modified citrus pectins extracted from orange pomace.

Modified pectin is a polysaccharide rich in galacturonic acid altered by pH adjustment and thermal treatment used especially as an anti-cancer agent. The aim of this work was to study the physical and chemical properties of modified pectins extracted from orange pomace with citric and nitric acids. The galacturonic acid content, degree of esterification, Fourier Transform Infrared Spectroscopy profile, molecular weight, intrinsic viscosity, rheological properties and antioxidant activity of the pectins were evaluated. The modification process caused the de-esterification of pectins and a decrease of molecular weight due to removal of neutral sugars, maintaining the linear chain of galacturonic acid. Such changes also caused a significant increase in the in vitro antioxidant activity (p ≤ 0.05) and influenced the rheological properties of pectin, reducing its viscosity. This work showed that the modification of pectin from orange pomace with citric and nitric acids altered its structural and physical characteristics as well as its biological activity toward a free-radical.

Optimization of subcritical water extraction for pectin extraction from cocoa pod husks using the response surface methodology.

This study optimized subcritical water extraction (SWE) conditions to maximize pectin yield from cocoa pod husk (CPH) and compared the characteristics of CPH pectin extracted through SWE with those of CPH pectin obtained through conventional extraction (CE) with citric acid. The Box-Behnken experimental design was employed to optimize SWE and examine the influence of process parameters, including temperature (100 °C-120 °C), extraction time (10-30 min), and solid:liquid ratio (SLR) (1:30-2:30 g/mL), on pectin yield. The maximum pectin yield of 6.58% was obtained under the optimal extraction conditions of 120 °C for 10 min with 1:15 g/mL SLR and closely corresponded with the predicted value of 7.29%. Compared with CE, SWE generated a higher yield and resulted in a higher degree of esterification, methoxyl content, and anhydrouronic acid value but a lower equivalent weight. The extracted pectin was pure, had low-methoxyl content, and similar melting and degradation temperatures.

Acid-catalyzed transformation of orange waste into furfural: the effect of pectin degree of esterification.

The transformation of biomasses from agro-industrial waste can significantly impact the production of green chemicals from sustainable resources. Pectin is a biopolymer present in lignocellulosic biomass as Orange Peel Waste (OPW) and has possibilities for making platform compounds such as furfural for sustainable chemistry. In this work, we studied the transformation to furfural of OPW, pectins, and D-galacturonic acid (D-GalA), which is the main component (65 wt%) of pectin. We analyzed pectins with different degrees of esterification (45, 60 and 95 DE) in a one-pot hydrolysis reaction system and studied the differences in depolymerization and dehydration of the carbohydrates. The results show that the production of furfural decreases as the DE value increases. Specifically, low DE values favor the formation of furfural since the decarboxylation reaction is favored over deesterification. Interestingly, the furfural concentration is dependent upon the polysaccharide composition of pentoses and uronic acid. The obtained concentrations of furfural (13 and 14 mmol/L), D-xylose (6.2 and 10 mmol/L), and L-arabinose (2.5 and 2.7 mmol/L) remained the same when the galacturonic acid was fed either as a polymer or a monomer under the same reaction conditions (0.01 M SA, 90 min and 433 K). OPW is proposed as a feedstock in a biorefinery, in which on a per kg OPW dry basis, 90 g of pectin and 15 g of furfural were produced in the most favorable case. We conclude that the co-production of pectin and furfural from OPW is economically feasible.

NMR fingerprinting of depolymerised durian rind pectin and its antibacterial activity.

This study investigated the effect of commercial sterilisation treatment (121 °C for 15 min) on durian rind pectin. The change of structure was observed by NMR (nuclear magnetic resonance) and the antibacterial activity was assessed by microdilution method to obtain the minimum inhibitory concentration (MIC) value. NMR spectra revealed the rhamnogalacturonan-I and homogalacturonan structure, with lower methyl-ester in sterilised pectin. Native pectin was unable to inhibit Escherichia coli and Staphylococcus aureus at the highest tested concentration (MIC > 25 mg/mL), but sterilised pectin showed inhibitory effect against E.coli (MIC 12.5 mg/mL) and S. aureus (MIC 6.25 mg/mL). Membrane filtration to obtain fraction < 20 kDa enhanced the inhibition against S. aureus further, but not for E.coli. The antibacterial effect was possibly correlated to the decrease of molecular weight (MW) and degree of esterification (DE) of durian rind pectin. E. coli was more resistant to pectin than S. aureus.

Characterize the physicochemical properties and microstructure of pectin from high-pressure and thermal processed cloudy hawthorn (Crataegus pinnatifida) juice based on acid heating extraction.

Physicochemical properties and morphological features of pectin in high-pressure-processing (JHPP) and thermal-processing (JTP) treated cloudy hawthorn juice were investigated based on acid heating extraction. Pectin from hawthorn juice was identified as low methoxy pectin (41.77%), which was significantly reduced to 34.56%-39.51% from JHPP, while pectin esterification degree (DE) from JTP increased to 45.58%, which can also be confirmed by Fourier transform infrared spectroscopy. In comparison to control, pectin linearity of JHPP and JTP significantly decreased with more highly branched-chains. However, no significate difference was observed in thermostability, crystallinity and main functional groups. Interestingly, a large number of aggregations was observed in JHPP pectin, and the intermodular distance of JTP pectin was enhanced, which was consistent with the results of viscosity, molecular weight and DE. These findings provided insights into utilization of hawthorn pectin and application of high-pressure processing (HPP) for improving quality property of fruit products by pectin modification.

Insights into pectin O-acetylation in the plant cell wall: structure, synthesis, and modification.

O-Acetyl esterification is an important structural and functional feature of pectins present in the cell walls of all land plants. The amount and positions of pectin acetyl substituents varies across plant tissues and stages of development. Plant growth and response to biotic and abiotic stress are known to be significantly influenced by pectin O-acetylation. Gel formation is a key characteristic of pectins, and many studies have shown that gel formation is dependent upon the degree of acetylation. Previous studies have indicated that members of the TRICHOME BIREFRINGENCE-LIKE (TBL) family may play a role in the O-acetylation of pectin, however, biochemical evidence for acceptor specific pectin acetyltransferase activity remains to be confirmed and the exact mechanism(s) for catalysis must be determined. Pectin acetylesterases (PAEs) affect pectin acetylation as they hydrolyze acetylester bonds and have a role in the amount and distribution of O-acetylation. Several mutant studies suggest the critical role of pectin O-acetylation; however, additional research is required to fully understand this. This review aims to discuss the importance, role, and putative mechanism of pectin O-acetylation.

Cerium binding activity of pectins isolated from the seagrasses Zostera marina and Phyllospadix iwatensis.

Cerium binding activity of three different water soluble pectin compounds of different origin was studied in a batch sorption system. The Langmuir, Freundlich and BET sorption models were adopted to describe the binding reactions between metal ions and pectin molecules. The Langmuir model provided the best fit. Within the pH range from 4.0 to 6.0, the largest amount of the cerium ions was bound by pectin isolated from the seagrass Phylospadix iwatensis in comparison to pectin extracted from the seagrass Zostera marina and pectin obtained from citrus peel (commercial grade). The Langmuir constants were also highest for the pectin samples isolated from the seagrass P. iwatensis. The results obtained from this study suggest that pectin is a prospective source for the development of radioisotope-removing pharmaceuticals.

Effects of various degrees of esterification on antioxidant and immunostimulatory activities of okra pectic-polysaccharides.

Pectic-polysaccharides are considered as one of the most abundant bioactive components in okra, which possess various promising health-promoting effects. However, the knowledge regarding the structure-bioactivity relationship of okra pectic-polysaccharides (OPP) is still limited. In this study, effects of various degrees of esterification (DEs) on in vitro antioxidant and immunostimulatory activities of OPP were analyzed. Results displayed that OPP with high (42.13%), middle (25.88%), and low (4.77%) DE values were successfully prepared by mild alkaline de-esterification, and their primary chemical structures (compositional monosaccharide and glycosidic linkage) and molecular characteristics (molecular weight distribution, particle size, and rheological property) were overall stable. Additionally, results showed that the notable decrease of DE value did not significantly affect antioxidant activities [2,2'-azino-bis (3-ethylbenzthiazoline-6-sulphonic acid) (ABTS) and nitric oxide (NO) radical scavenging abilities as well as ferric reducing antioxidant power (FRAP)] of OPP, suggesting that the DE was not closely related to its antioxidant activity. In fact, the slight decrease of antioxidant activity of OPP after the alkaline de-esterification might be attributed to the slight decrease of uronic acid content. Nevertheless, the immunostimulatory effect of OPP was closely related to its DE, and a suitable degree of acetylation was beneficial to its in vitro immunostimulatory effect. Besides, the complete de-acetylation resulted in a remarkable reduction of immune response. The findings are beneficial to better understanding the effect of DE value on antioxidant and immunomodulatory activities of OPP, which also provide theoretical foundations for developing OPP as functional foods or health products.

Modulation of the Gut Microbiota Structure and Function by Two Structurally Different Lemon Pectins.

Pectins are plant polysaccharides consumed as part of a diet containing fruits and vegetables. Inside the gastrointestinal tract, pectin cannot be metabolized by the mammalian cells but is fermented by the gut microbiota in the colon with the subsequent release of end products including short-chain fatty acids (SCFA). The prebiotic effects of pectin have been previously evaluated but reports are inconsistent, most likely due to differences in the pectin chemical structure which can vary by molecular weight (MW) and degree of esterification (DE). Here, the effects of two different MW lemon pectins with varying DEs on the gut microbiota of two donors were evaluated in vitro. The results demonstrated that low MW, high DE lemon pectin (LMW-HDE) altered community structure in a donor-dependent manner, whereas high MW, low DE lemon pectin (HMW-LDE) increased taxa within Lachnospiraceae in both donors. LMW-HDE and HMW-LDE lemon pectins both increased total SCFAs (1.49- and 1.46-fold, respectively) and increased acetic acid by 1.64-fold. Additionally, LMW-HDE lemon pectin led to an average 1.41-fold increase in butanoic acid. Together, these data provide valuable information linking chemical structure of pectin to its effect on the gut microbiota structure and function, which is important to understanding its prebiotic potential.

Physicochemical characteristics and functional properties of high methoxyl pectin with different degree of esterification.

Moderate alkali de-esterification can change the physicochemical characteristics and thus the functional properties of high methoxyl pectin (HMP). The results revealed that de-esterification could increase negative charges (Zeta potential from -21 to -31 mV), decrease molecular weight (from 448 to 136 kDa) and apparent viscosity of HMP. Homogalacturonan (HG) content decreased (from 62% to 49%) while rhamnogalacturonan Ⅰ (RG-Ⅰ) content increased (from 32% to 46%) after de-esterification. The group characteristics of HMP with different degree of esterification (DE) were similar and no obvious impact was made on degree of crystallinity by alkali de-esterification. A conformation transition of HMP molecule implied by Congo red test were occurred as the DE decreased. With the decrease of DE, the molecular structure of HMP became shorter and smaller, and the entanglement was weaker. The de-esterification caused slight decrease of thermal stability. Alkali de-esterification would weaken the gel property and the emulsifying ability of HMP.

Extraction optimization and characterization of persimmon peel pectin extracted by subcritical water.

Persimmon peel pectin (PPP) was extracted by subcritical water via the response surface methodology. The optimal crude PPP extraction yield of 7.62 ± 0.7 % was found at 138 °C, 2.84 min, and liquid-solid ratio of 1:10.02. After treatment of deproteinization and decolorization with papain and hydrogen peroxide, 83.19 % of protein and 78.56 % of the colour in crude PPP were removed, respectively. PPP owned the Mw of 21.79 kDa and its uronic acids content was 64.03 %. PPP was further affirmed by fourier transform infrared, X-ray diffractometer and 1H NMR analysis. Moreover, the degradation temperature (228.05 â„ƒ) of PPP was verified via differential scanning calorimetry. Then, the IC50 of PPP to ABTS•+ was 9.8 times that of commercial citrus pectin. Moreover, PPP could change microbial communities and selectively enrich Bacteroides, Cetobacterium, Erysipelatoclostridium, Parabacteroides and Phocaeicola sartorii. This study demonstrated that subcritical water was practicable for extraction of persimmon peel pectin.

Effects of Molecular Weight and Degree of Esterification of Soluble Soybean Polysaccharide on the Stability of Casein under Acidic Conditions.

The effects of molecular weight (MW) and degree of esterification (DE) of soluble soybean polysaccharide (SSPS) on the stability of casein under acidic conditions were investigated. The ability of SSPS to stabilize casein was characterized by the content of SSPS-casein complex, the LUMiSizer instability index, average particle size, zeta potential, and storage experiments. The long-term storage stability of the mixtures was related to their ability to combine casein and the stability of the complexes. At the same DE, SSPSs with medium MW formed more complexes with casein than SSPSs with high or low MW; and at the same MW, SSPSs with medium or low DE formed more complexes than SPSSs with high DE. In addition, SSPSs with higher MW had a better stabilizing behavior due to the large steric repulsion between complexes. SSPSs with high MW and low DE showed the best ability to stabilize casein under acid conditions.

Optimization of Pectin Extraction from Sweet Potato Peels Using Citric Acid and its Emulsifying Properties.

BACKGROUND: Pectin is a natural polysaccharide that has been used widely as a stabilizer in food emulsion system. OBJECTIVE: This study aimed to optimize the yield of pectin extracted from sweet potato residue and investigate its emulsifying properties. METHODS: Response surface methodology (RSM) has been utilized to investigate the pectin extracted from sweet potato peels using citric acid as the extracting solvent. Investigation of the effect of different extraction conditions namely temperature (°C), time (min) and solution pH on pectin yield (%) were conducted. A Box-Benhken design with three levels of variation was used to optimize the extraction conditions. RESULTS: The optimal conditions determined were temperature 76°C, time 64 min and pH 1.2 with 65.2% yield of pectin. The degree of esterification (DE) of the sweet potato pectin was determined using Fourier Transform Infrared (FTIR) Spectroscopy. The pectin is high-methoxyl pectin with DE of 58.5%. Emulsifying properties of sweet potato pectin were investigated by measuring the zeta-potential, particle size and creaming index with addition of 0.4 and 1.0 wt % pectin to the emulsion. CONCLUSION: Extraction using citric acid could improve the pectin yield. Improved emulsion stability was observed with the addition of the sweet potato pectin.

Characterization of water status and water soluble pectin from peaches under the combined drying processing.

Characterization of water status and water soluble pectin (WSP) from peach were evaluated after different stage of combined drying in which osmotic dehydration (OD) was considered as the pre-treatment prior to instant controlled pressure drop (DIC) - assisted infrared radiation drying (IRD) (IR-DIC). Results showed that the contents of free water and immobilized water decreased to 0 g after the combined drying. The content of bound water increased after IRD treatment. The residual PME activity in peach slices was 153.3-179.6% after OD treatment, while, the PG were totally inactivated after IRD. The degree of esterification (DE), WSP content and average molar mass (Mw) decreased significantly (from 75.00 to 43.74, from 156.00 to 74.91 mg/g AIR and from 2.28 to 0.49 × 105 Da, respectively) after the combined drying. The neutral sugar of WSP was mainly composed by galactose, arabinose and rhamnose, whose contents decreased after the combined drying. However, OD treatment would slow down the degradation. There was a low peak at 1740 cm-1 in FT-IR spectrum observed for WSP after IRD and DIC treatment, which might illustrate the degradation of WSP during the combined drying.

Microwave heating extraction of pectin from lime peel: Characterization and properties compared with the conventional heating method.

Microwave and conventional heating methods were used to extract pectin from lime peel waste using different acid extractants (hydrochloric or citric acid) and peel-to-extractant ratios (1:20 or 1:40). Hydrochloric acid as the extractant resulted in a higher yield of pectin with both methods. The methoxyl content and galacturonic acid content of lime peel pectin were in the range 8.74-10.51% and 79.29-95.93%, respectively. The intense band around 1730 cm-1 corresponded to methyl esterified uronic carboxyl groups and confirmed the higher equivalent weight and degree of esterification for the microwave-extracted pectin than that from conventional extraction. Lime peel pectin could be classified as high methoxyl pectin having a rapid-set gel formation. The viscosity and viscoelastic properties of the pectin solution from both heating methods enhanced with increasing solid concentration. Hence, microwave heating can be a short processing time for pectin extraction from lime peel waste with suitable pectin properties.