We extracted and hydrolyzed bioactive flavonoids from C. unshiu peel using subcritical water (SW) in a semi-continuous mode. The individual flavonoid yields, antioxidant and enzyme inhibitory activities of the SW extracts were analyzed. The extraction yields of hesperidin and narirutin increased with increasing temperature from 145 °C to 165 °C. Hydrothermal hydrolysis products (HHP), such as monoglucosides (hesperetin-7-O-glucoside and prunin) and aglycones (hesperetin and naringenin) were obtained in the SW extracts at temperatures above 160 °C. The sum of hesperidin and its HHP in the SW extracts was strongly correlated with antioxidant activities, whereas the contents of hesperetin and naringenin were strongly correlated with enzyme inhibitory activities. Hesperetin exhibited the highest antioxidant activities (2,2-diphenyl-1-picrylhydrazyl radical scavenging activity, ferric-reducing antioxidant power, and oxygen radical absorbance capacity), whereas hesperetin-7-O-glucoside exhibited the highest enzyme inhibitory activities (angiotensin-I converting enzyme (ACE) and pancreatic lipase (PL)). Naringenin exhibited the highest enzyme inhibitory activities (xanthine oxidase and α-glucosidase). PMFs (sinensetin, nobiletin, and tangeretin) also exhibited relatively high inhibitory activities against ACE and PL. This study confirms the potential of SW for extracting and hydrolyzing bioactive flavonoids from C. unshiu peel using an environmentally friendly solvent (water) and a shorter extraction time.

Many citrus varieties are hybridized to improve their quality and to overcome the effects of climate change. However, there is limited information on the effect of the chemical profiles of hybrid varieties on their quality. In this study, we analyzed 10 citrus varieties and evaluated the correlation with their general characteristics and antioxidant activities. Chemical profiles, including the contents of sugars, organic acid compounds, flavonoids, limonoids, and carotenoids, which are related to taste, color, and health benefits, were significantly different depending on the citrus varieties, leading to different antioxidant capacities and general quality parameters. Based on these data, the correlations were investigated, and 10 citrus varieties were clustered into four groups—Changshou kumquat and Jeramon (cluster I); Setoka (cluster II-1); Natsumi, Satsuma mandarin, and Navel orange (cluster II-2); Kanpei, Tamnaneunbong, Saybyeolbong, and Shiranui (cluster II-3). Moreover, a metabolomic pathway was proposed. Although citrus peels were not analyzed and the sensory and functional qualities of the citrus varieties were not investigated in this study, our results are useful to better understand the relationship between citrus quality and metabolite profiles, which can provide basic information for the development and improvement of new citrus varieties.

Citrus fruits undergo significant metabolic profile changes during their development process. However, limited information is available on the changes in the metabolites of Citrus unshiu during fruit development. Here, we analyzed the total phenolic content (TPC), total carotenoid content (TCC), antioxidant activity, and metabolite profiles in C. unshiu fruit flesh during different stages of fruit development and evaluated their correlations. The TPC and antioxidant activity significantly decreased during fruit development, whereas the TCC increased. The metabolite profiles, including sugars, acidic compounds, amino acids, flavonoids, limonoids, carotenoids, and volatile compounds (mono- and sesquiterpenes), in C. unshiu fruit flesh also changed significantly, and a citrus metabolomic pathway related to fruit development was proposed. Based on the data, C. unshiu fruit development was classified into three groups: Group 1 (Aug. 1), Group 2 (Aug. 31 and Sep. 14), and Group 3 (Oct. 15 and Nov. 16). Although citrus peel was not analyzed and the sensory and functional qualities during fruit development were not investigated, the results of this study will help in our understanding of the changes in chemical profile during citrus fruit development. This can provide vital information for various applications in the C. unshiu industry.

Noni fruits (Morinda citrifolia) are a source of phenolic bioactive compounds (scopoletin, alizarin, and rutin), which have antioxidant, antimicrobial, anticancer, and anti-inflammatory activities. In this study, subcritical water was applied to determine the extraction yields and kinetics of phenolic compounds from noni fruits. The scopoletin and alizarin yields increased with the increase in temperature from 100 to 140 °C, while that of rutin increased up to 120 °C and then decreased at 140 °C. The yields of all the compounds rapidly increased from 1 to 2 mL/min and then slightly up to 3 mL/min of water flow rate. The extraction kinetics were assessed using two mathematical models. The two-site kinetic desorption model had a better fit for all experimental conditions throughout the extraction cycle and best described the extraction kinetics of phenolic compounds from noni fruits. The diffusion coefficients of scopoletin and alizarin at 140 °C and 3 mL/min were 3.7- and 16.2-fold higher than those at 100 °C and 1 mL/min, respectively. The activation energies of alizarin were 2.9- to 8.5-fold higher than those of scopoletin at various flow rates. Thus, subcritical water could be an excellent solvent with higher extraction yields and shorter extraction times using an environmentally friendly solvent.

Salt is one of the most important factors for fermented foods, but the effect of salt treatment time on the quality of fermented foods has rarely been studied. In this study, the effect of different salt treatment times (0, 48, and 96 h) after the start of fermentation on the quality of the soy sauce moromi extract (SSME) was investigated. As the salt treatment time was delayed, the population of Aspergillus oryzae, Lactobacillaceae, and Enterococcaecea in SSME increased, whereas the population of Staphylococcaceae and Bacillaceae decreased, leading to changes in the enzymatic activity and metabolite profiles. In particular, the contents of amino acids, peptides, volatile compounds, acidic compounds, sugars, and secondary metabolites were significantly affected by the salt treatment time, resulting in changes in the sensory quality and appearance of SSME. The correlation data showed that metabolites, bacterial population, and sensory parameters had strong positive or negative correlations with each other. Moreover, based on metabolomics analysis, the salt treatment-time-related SSME metabolomic pathway was proposed. Although further studies are needed to elucidate the salt treatment mechanism in fermented foods, our data can be useful to better understand the effect of salt treatment time on the quality of fermented foods.

Aspergillus oryzae (A. oryzae) is an important starter in the fermentation of koji and moromi. However, the effect of different A. oryzae strains on the quality of moromi has rarely been studied. For this reason, this study analyzed the physicochemical properties, enzyme activity, sensory quality, and metabolite profiles of moromi samples fermented using two strains (A. oryzae KCCM12012P (moromi-1) and KCCM12804P (moromi-2)), which were newly isolated from fermented soy foods, and compared them to those of a commercialized A. oryzae strain (control). Amino-type nitrogen contents of moromi-1 and moromi-2 samples were higher than that of control moromi, and their amylase and protease activities were also higher. Moreover, metabolite profiles of moromi were significantly altered according to strains. In particular, the levels of many amino acids, peptides, nucleotides, and acidic compounds were altered, which resulted in changes in the sensory quality of moromi. Although volatile compounds were not investigated, the results suggested that the quality of moromi was significantly different for newly isolated strains, especially A. oryzae KCCM12804P, and they were superior to the commercial strain in terms of taste-related substances. Therefore, these strains could be used as good starters to produce moromi and soy sauce with good sensory quality.