Gelling properties of lysine-amidated citrus pectins: The key role of pH in both amidation and gelation.

The amidation of pectin by amino acids has been widely applied due to its safety and excellent gelling properties. This study systematically examined the effects of pH on the gelling properties of lysine-amidated pectin during amidation and gelation. Pectin was amidated over the range of pH 4-10, and the amidated pectin obtained at pH 10 showed the highest degree of amidation (DA, 27.0 %) due to the de-esterification, electrostatic attraction, and the stretching state of pectin. Moreover, it also exhibited the best gelling properties due to its greater numbers of calcium-binding regions (carboxyl groups) and hydrogen bond donors (amide groups). During gelation, the gel strength of CP (Lys 10) at pH 3-10 first increased and then decreased, with the highest gel strength at pH 8, which was due to the deprotonation of carboxyl groups, protonation of amino groups, and ß-elimination. These results show that pH plays a key role in both amidation and gelation, with distinct mechanisms, and would provide a basis for the preparation of amidated pectins with excellent gelling properties. This will facilitate their application in the food industry.

Caseinate-reinforced pectin hydrogels: Efficient encapsulation, desirable release, and chemical stabilization of (-)-epigallocatechin.

(-)-Epigallocatechin (EGC) has good health benefits, but its chemical stability is low. Pectin hydrogels have potential for the encapsulation and delivery of EGC, but they are limited by porous networks and poor mechanical properties. In this study, protein (whey protein isolate and caseinate)-reinforced pectin hydrogel beads (HBPEC-WPI and HBPEC-CAS) were developed to overcome these limitations. The results showed that HBPEC-CAS was a superior delivery system for EGC. HBPEC-CAS had a compact network structure, mainly because of the hydrogen bonds that formed between caseinate and pectin. Moreover, the EGC encapsulation efficiency of HBPEC-CAS (2.4%) reached 92.23 %; HBPEC-CAS (2.4%) could also delay the release of EGC in an aqueous environment, while ensuring its sufficient release in a simulated gastrointestinal environment. Notably, EGC was chemically stabilized in HBPEC-CAS (2.4%) during a 6-day storage period at 37 °C through the inhibition of its epimerization, oxidation, dimerization, and trimerization. The numerous hydroxyl groups in EGC readily interacted with the exposed amino acid residues in caseinate and created more protective sites. This study developed a strategy for protein-reinforced pectin hydrogel development and approaches for the protection of tea polyphenols; the findings offer useful insights for the tea-based food and beverage industry.

Orange Pectin with Compact Conformation Effectively Alleviates Acute Colitis in Mice.

A comprehensive understanding of the relationships between the structure and function is critical for the targeted preparation of functional pectins. In this study, we compared the alleviating effects of five orange pectins (200 mg/kg) extracted using acid (P2), alkali (P10), cellulase (C), acid + cellulase (P2 + C), and alkali + cellulase (P10 + C) on dextran sodium sulfate-induced acute colitis. The physiological and histopathological indicators revealed that the alleviating effects were most significant for P10 + C, followed by P10, P2 + C, P2, and C. P10 + C increased the diversity and relative abundance of Akkermansia, leading to increased generation of colonic short-chain fatty acids as well as mRNA and protein expressions of GPR43, GPR109A, claudin-1, ZO-1, and occludin. Therefore, proinflammatory cytokines were decreased, and anti-inflammatory cytokines were increased. A compact conformation of P10 + C contributed to the alleviation effects on acute colitis. Alkali + cellulase-extracted orange pectin with a compact conformation has potential as adjuvant treatment for intestinal inflammation.

Upper digestion fate of citrus pectin-stabilized emulsion: An interfacial behavior perspective.

Citrus pectin can serve as a naturally digestion-resistant emulsifier, although how it achieves this effect is still unknown. In this study, the upper digestion fate of an emulsion stabilized by different concentrations of citrus pectin, and changes in its interfacial properties during digestion, were investigated. Emulsions stabilized by high-concentration citrus pectin (3 %) were relatively stable during digestion and had a lower free fatty acid (FFA) release rate than emulsions stabilized by low-concentration citrus pectin (1 %). At the low concentration, the citrus pectin interface had a thin absorbing layer and was largely replaced by bile salts, while at high concentration the citrus pectin interface possessed a uniform and thick adsorbing layer that resisted the replacement of bile salts and enabled lipase adsorption. This study has improved our understanding of the digestion of emulsion from the interface and will be useful for designing emulsion-based functional foods that can achieve targeted release.

Effect of mesoscopic structure of citrus pectin on its emulsifying properties: Compactness is more important than size.

We previously explored citrus oil emulsion stabilized by citrus pectin. In this report, we characterized key parameters of the citrus pectin mesoscopic structure and their effect on emulsifying capacity, and explored the underlying mechanism by determining the interfacial properties, emulsifying ability, and micromorphology. To generate different mesoscopic structure, citrus pectins were hydrolyzed or regulated by pH and NaCl. Hydrolysis decreased the size of citrus pectin mesoscopic structure with constant compactness, leading to superior interfacial properties but inferior emulsifying ability. In contrast, pH and NaCl regulation decreased the mesoscopic structure size and increased the compactness, and pH- and NaCl-regulated citrus pectin formed a compact absorbed layer at the interface to resist droplet coalescence/flocculation during homogenization. Our results support the importance of compactness of the citrus pectin mesoscopic structure on emulsifying capacity. This study increased our understanding on the relationship between the mesoscopic structures of polysaccharide emulsifier and emulsifying ability.

Biosynthesis of citrus flavonoids and their health effects.

Citrus-derived flavonoids play important roles in the regulation of physiological conditions of citrus plants, including color changes of flower and fruit, flavor development, and anti-stress physiology. Moreover, citrus flavonoids possess multiple health-promoting effects in humans, and they are important ingredients for nutraceuticals and functional foods. The biosynthesis of flavonoids in citrus plants is of special significance because it determines the chemical structures and bioaccumulation of these bioactive compounds in the plants, which consequently influences their physiological functions in both citrus plants and human body. This review systematically summarizes: 1) the biosynthesis pathway of citrus-derived flavonoids, 2) the biosynthesis location and distribution of flavonoids in citrus plants, 3) the factors affecting flavonoid biosynthesis, 4) the biological significance of flavonoid biosynthesis in citrus plants, and 5) the health-promoting properties of citrus-derived flavonoids. The collation of this information provides scientific guidance for the development of healthy citrus foods and other health-promoting products containing citrus flavonoids.

The structure-property relationships of acid- and alkali-extracted grapefruit peel pectins.

Structure and properties of pectin can be affected by extraction methods. In this study, grapefruit peel pectins extracted by HCl (at pH 1 [P1], 2 [P2], and 3 [P3]) and NaOH (at pH 9 [P9], 10 [P10], and 11 [P11]) were prepared and characterized. Atomic force microscopy (AFM) provided direct evidence of complex nano-structural patterns of pectins and revealed cross-linked networks of P10 and P11. Small-angle X-ray scattering (SAXS) demonstrated that P1, P2, and P3 possessed a relatively extended conformation, whereas P9, P10, and P11 displayed a three-dimensional structure and folded conformation. The compact and extended conformations of P3 contributed to its high viscosity in solution and the stability of the formed emulsion (75%). Porous surface and larger three-dimensional nanostructure (Dmax: 23 nm) of P10 facilitated its ion-binding capacity. Our results provide valuable insight into relationship between extraction methods and structure-properties of pectin, facilitating design of functional pectins.

Characterization of polymethoxyflavone demethylation during drying processes of citrus peels.

Polymethoxyflavones (PMFs) are found almost exclusively in citrus peel and have attracted much attention due to their potential health benefits. Dried citrus peel is an important ingredient for applications in food and traditional Chinese medicine. However, the structural changes of PMFs during drying processes of citrus peel remain unknown. In this study, for the first time we discovered that four major permethoxylated PMFs, i.e. sinensetin, nobiletin, heptamethoxyflavone and tangeretin, underwent demethylation at the 5-position on the A ring of their flavonoid structures to yield corresponding 5-demethylated PMFs during the drying process of citrus peel. Our results further demonstrated that the aforementioned PMF demethylation was through two mechanisms: acid hydrolysis and enzyme-mediated catalysis. PMF demethylation in citrus peels was systematically characterized during hot-air drying (HAD), vacuum-freeze drying (VFD) and sun drying (SD). The highest PMF demethylation was obtained in SD followed by HAD and VFD. This study provided a solid scientific basis for rational control of PMF demethylation in citrus peels, which could facilitate the production of high-quality citrus peel and related products.

Efficiency of four different dietary preparation methods in extracting functional compounds from dried tangerine peel.

Dried tangerine peel (DTP) is an excellent plant resource that has been used as ingredients for both food and traditional Chinese medicine. In this study, the efficiency of four different dietary preparation methods (i.e. soaking, boiling, steaming, and ethanol extraction) in extraction of functional compounds (i.e. flavonoids and essential oil constituents) from DTP was evaluated systematically for the first time. To conduct a comprehensive evaluation of the extraction of the functional compounds, a synthetic evaluation model based on a weighting method was established. The optimum conditions of each dietary preparation method (e.g., time, temperature, solid-liquid ratio, etc.) were determined by response surface methodology. Ethanol extraction showed the best extraction efficiency, followed by soaking, boiling, and steaming. Additionally, different DTP extracts were shown to be clearly distinguished by electronic eye and electronic tongue. This research provides essential findings for the effective dietary instruction of DTP consumption.

Citrus Oil Emulsions Stabilized by Citrus Pectin: The Influence Mechanism of Citrus Variety and Acid Treatment.

Citrus pectin and citrus oil are the main functional components of citrus residuals in the processing industry. In this study, citrus oil emulsions were fabricated for the first time using four different citrus pectins (orange, mandarin, grapefruit, and commercial citrus pectins) as the emulsifier. The influence mechanism of citrus variety and acid treatment (pH 1, 2, 3, 4, 5, 6, and 7) on the emulsifying capacity of citrus pectins was systematically investigated by understanding the relationship between molecular structure, solution property, interfacial property, and emulsion property. The results suggest that citrus variety and acid treatment can significantly influence the emulsifying capacity in relation to the molecular structure and molecular state of citrus pectins. A smaller molecular size of citrus pectin and lower pH between 2 and 7 produced a reduction in aggregate size, which improved the interfacial capacity and emulsifying ability by promoting their distribution at the interface. Although hydrolyzed citrus pectins at pH 1 with a lower molecular size exhibited better interfacial capacity, citrus oil emulsions were unstable due to electrostatic attraction caused by partially positive charged citrus pectins. Fine stable citrus oil emulsion was prepared using mandarin pectin with a relative high methyl ester content and small molecular size at pH 2. Our results provide a scientific basis for the fabrication of citrus oil emulsion based on citrus pectin and facilitate the application of citrus residuals in the food industry.

Characterization of physical properties and electronic sensory analyses of citrus oil-based nanoemulsions.

Citrus oils and their emulsions have been widely used in food and beverage products due to their flavor, various beneficial health functions and relative high solubility for lipophilic bioactive components. However, the non-digestibility and instability has limited the application of emulsions made from a single type of citrus oil. In this study, common triacylglycerol oils (i.e. corn oil and MCT oil) and citrus oils (i.e. bergamot oil and sweet orange oil) were used in combination with different mixing ratios (triacylglycerol oil:citrus oil = 1:0, 9:1, 5:1, 3:1, 1:1 and 0:1) to produce various nanoemulsions (10% oil phase), and their physical and electronic sensory properties were systematically characterized. The results demonstrated that the mixed oil nanoemulsions were much more stable than pure citrus oil emulsions. Electronic nose, electronic eye and electronic tongue were shown to be able to provide informative evaluation of the electronic sensory of the emulsions. Data-fitting of these electronic sensory devices significantly improved the effective discrimination and accuracy of sensory evaluation of the emulsions. These results provided basis for using triacylglycerol oils and citrus oils in combination to produce nanoemulsions with superior physical and electronic sensory properties. Moreover, the electronic sensory evaluation method utilized in this study provided a useful approach for evaluation of emulsion-based food and beverage products.

Chemical Mapping of Essential Oils, Flavonoids and Carotenoids in Citrus Peels by Raman Microscopy.

Citrus peels, by-products in large quantity, are rich in various functional and beneficial components which have wide applications. Chemical analysis of these components in citrus peels is an important step to determine the usefulness of the by-products for further applications. In this study, we explored Raman microscopy for rapid, nondestructive, and in situ chemical mapping of multiple main functional components from citrus peels. The relative amount and distribution in different locations (flavedo, albedo, and longitudinal section) of 3 main functional components (essential oils, carotenoids, and flavonoids) in citrus peels were systematically investigated. The distribution profiles of these components were heterogeneous on the peels and varied between different species of citrus peels. Essential oil was found mainly existed in the oil glands, while carotenoids were in the complementary location. Some flavonoids were observed in the oil glands. This study showed the capability of Raman microscopy for rapid and nondestructive analysis of multiple bio-components without extraction from plants. The information obtained from this study would assist the better production and application of the functional and beneficial components from citrus by products in an effective and sustainable manner. PRACTICAL APPLICATION: This study indicated the capability of Raman microscopy for rapid and nondestructive analysis of multiple bioactive components in plant tissues. The information obtained from the study would be valuable for developing effective and sustainable strategy of utilization of citrus peels for further applications.

Effects of Preheating and Storage Temperatures on Aroma Profile and Physical Properties of Citrus-Oil Emulsions.

Citrus oils are used as good carrier oil for emulsion fabrication due to their special flavor and various health-promoting functions. In this study, the effects of preheating temperature (30, 40, 50, 60, and 70 °C) and storage temperature (4, 25, and 37 °C) on aroma profiles and physical properties of three citrus-oil (i.e., mandarin, sweet orange, and bergamot oils) emulsions were systematically investigated for the first time. The results demonstrated the significant impact of temperature on aroma profile and physical properties. The abundance of d-limonene was found to be the main factor determining the aroma of the three citrus-oil emulsions at different preheating and storage temperatures, while ß-linalool and linalyl acetate were important for the aroma of bergamot oil emulsion. Preheating temperature showed a profound impact on the aroma of citrus-oil emulsions, and the aroma of different citrus oil emulsions showed different sensitivity to preheating temperature. Storage temperature was also able to alter the properties of citrus oil emulsions. The higher was the storage temperature, the more alteration of aroma and more instability of the emulsions there was, which could be attributed to the alteration of the oil components and the properties of emulsions. Among all three emulsions, bergamot-oil emulsion was the most stable and exhibited the most potent ability to preserve the aroma against high temperature. Our results would facilitate the application of citrus-oil emulsions in functional foods and beverages.

Encapsulation of Polymethoxyflavones in Citrus Oil Emulsion-Based Delivery Systems.

The purpose of this work was to elucidate the effects of citrus oil type on polymethoxyflavone (PMF) solubility and on the physicochemical properties of PMF-loaded emulsion-based delivery systems. Citrus oils were extracted from mandarin, orange, sweet orange, and bergamot. The major constituents were determined by GC/MS: sweet orange oil (97.4% d-limonene); mandarin oil (72.4% d-limonene); orange oil (67.2% d-limonene); and bergamot oil (34.6% linalyl acetate and 25.3% d-limonene). PMF-loaded emulsions were fabricated using 10% oil phase (containing 0.1% w/v nobiletin or tangeretin) and 90% aqueous phase (containing 1% w/v Tween 80) using high-pressure homogenization. Delivery systems prepared using mandarin oil had the largest mean droplet diameters (386 or 400 nm), followed by orange oil (338 or 390 nm), bergamot oil (129 or 133 nm), and sweet orange oil (122 or 126 nm) for nobiletin- or tangeretin-loaded emulsions, respectively. The optical clarity of the emulsions increased with decreasing droplet size due to reduced light scattering. The viscosities of the emulsions (with or without PMFs) were similar (1.3 to 1.4 mPa·s), despite appreciable differences in oil phase viscosity. The loading capacity and encapsulation efficiency of the emulsions depended on carrier oil type, with bergamot oil giving the highest loading capacity. In summary, differences in the composition and physical characteristics of citrus oils led to PMF-loaded emulsions with different encapsulation and physicochemical characteristics. These results will facilitate the rational design of emulsion-based delivery systems for encapsulation of PMFs and other nutraceuticals in functional foods and beverages.