Evaluation of Quality Properties of Brown Tigernut (Cyperus esculentus L.) Tubers from Six Major Growing Regions of China: A New Source of Vegetable Oil and Starch.

Tigernut has been recognized as a promising resource for edible oil and starch. However, the research on the quality characteristics of tigernut from different regions is lagging behind, which limits the application of tigernut in food industry. Tigernut tubers were obtained from six major growing regions in China, and the physicochemical properties of their main components, oil and starch, were characterized. Tigernut tubers from Baoshan contained the most oil (30.12%), which contained the most ß-carotene (130.4 µg/100 g oil) due to high average annual temperature. Gas chromatography analysis and fingerprint analysis results indicated that tigernut oil (TNO) consists of seven fatty acids, of which oleic acid is the major component. Changchun TNO contained the least total tocopherols (6.04 mg/100 g oil) due to low average annual temperature. Tigernut tubers from Chifeng (CF) contained the most starch (34.85%) due to the large diurnal temperature range. Xingtai starch contained the most amylose (28.4%). Shijiazhuang starch showed the highest crystallinity (19.5%). Anyang starch had the highest pasting temperature (76.0°C). CF starch demonstrated superior freeze-thaw stability (syneresis: 50%) due to low mean annual precipitation. The results could be further applied to support tigernut industries and relevant researchers that looks for geographical origin discrimination and improvements on tigernut quality, with unique physicochemical and technological properties.

Modified Chinese quince oligomeric proanthocyanidin protects deep-frying oil quality by inhibiting oxidation.

Chinese quince (Chaenomeles sinensis) fruit is an underutilized resource, rich in proanthocyanidins with antioxidant ability but poor lipid solubility. In this study, a novel modified oligomeric proanthocyanidin (MOPA) was prepared, which exhibited favorable lipid solubility (354.52 mg/100 g). It showed higher radical scavenging abilities than commercial antioxidant-BHA (butylated hydroxyanisole), both at 0.4-0.5 mg/mL. The addition of MOPA (0.04 %wt.) significantly increased the oxidative stability index of the soybean oil from 5.52 to 8.03 h, which was slightly lower than that of BHA (8.35 h). Analysis of the physicochemical properties and composition of oil during deep-frying showed that MOPA demonstrated significant antioxidant effects and effectively restricted the oil oxidation. This inhibition also delays the formation of heterocyclic amines (HAs) in fried food, thereby reducing the migration of HAs from food to deep-frying oil. Therefore, MOPA is a promising novel liposoluble antioxidant for protecting the quality of deep-frying oil.

Investigations on color and flavor formed by roasting sesame polysaccharide-protein mixtures.

Roasting is an important operation to produce attractive colors and distinctive flavors during the production of sesame oil. To investigate the contributions of macromolecules to the color and flavor during roasting sesame seeds, water-soluble polysaccharides (WSP) and chelator-soluble polysaccharides (CSP) sequentially extracted from sesame hull were mixed with sesame protein isolate (SPI) at different ratios (1:1, 1:2, and 2:1, w/w), then the mixtures were roasted at 180 °C for 35 min. Results showed that WSP, CSP, and SPI degraded approximately at 150 °C and SPI had the highest thermal stability. According to monosaccharide/amino acid analysis, glucose and galacturonic acid showed the highest reduction rates, as well as lysine and arginine. CSP + SPI mixtures showed greater reactivity than WSP + SPI mixtures, resulting in a darker color and many more Maillard reaction products. The predominant volatiles of roasted WSP/CSP + SPI mixtures were aldehydes and heterocyclic compounds identified by headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry (HS-SPME/GC-MS). This work provides some new information about flavor and color development during roasting sesame seeds.

Optimization and Kinetics Modeling of Microwave-Assisted Subcritical n-Butane Extraction of Tigernut Oil.

In this study, tigernut oil was extracted from tigernut meal by subcritical n-butane extraction with the assistance of microwave pretreatment. Effects of microwave pulse duration, particle size of tigernut meal, and subcritical extraction variables (temperature, time, solid-liquid ratio, number of extraction cycles) on extraction efficiency were examined by single-factor experiments and Response Surface Methodology (RSM) modeling. The results indicate that microwaving (560 W, 6 min) significantly increased the subcritical extraction efficiency. The variation of extraction yield could be interpreted as a nonlinear function of extraction time, temperature and liquid-solid ratio. Changing the independent variables could affect the oil extraction efficiency. The subcritical extraction of tigernut oil with a liquid-solid ratio of 3.62 kg/(kg of tigernut meal) at a temperature of 52°C for 32 min after three extraction cycles produced the most oil, and a maximum yield (24.736%) of tigernut oil was achieved. The ratio of unsaturated to saturated fatty acids (4.68 UFA/SFA), low acid value (3.30 mg KOH/g oil), low peroxide value (0.28 meq.kg-1), and preponderance of oleic acid indicate a high-quality oil. To describe the extraction kinetics, a modified Brunner's mathematical model was used. The model fit the experimental data well over the entire operating range, and the explanation coefficient exceeds 96%. Our results can be used to develop an optimized method for subcritical fluid extraction of tigernut oil and can move industry further toward implementing microwave-assisted subcritical extraction in oil processing.

Comparison of key aroma-active compounds between roasted and cold-pressed sesame oils.

This was the first study to compare the key aroma-active compounds that contributed to the different aroma profiles between roasted and cold-pressed sesame oils. Aroma compounds were extracted by headspace solid-phase micro-extraction (HS-SPME) and simultaneous distillation extraction (SDE) and were analysed using gas chromatography-olfactometry-mass spectrometry (GC-O-MS) and aroma extract dilution analysis (AEDA). The numbers of aroma-active compounds with the flavour dilution (FD) factors between 1 and 2048 were 57 and 16 in the roasted and cold-pressed sesame oils, respectively. A total of 28 volatile compounds were identified as aroma-active compounds in sesame oils for the first time. Important aroma compounds (FD ≥ 8) were quantified by the external standard method, and their odour activity values (OAV) were calculated as the ratio of their concentrations to odour thresholds in oil. The numbers of key aroma-active compounds defined by OAVs ≥ 1 were 23 (OAVs = 1-385) and 8 (OAVs = 1-42), respectively, in the roasted and cold-pressed sesame oils. 2-Methoxy-4-vinylphenol (smoked, 1924 µg/kg, OAV = 385), 2-methoxyphenol (smoked, 1488 µg/kg, OAV = 114) and pyrazines (roasted and nutty, 578-22750 µg/kg, OAV = 1-67) were the most important aroma-active compounds in the roasted sesame oil, whereas hexanal (green and fruity, 3094 µg/kg, OAV = 42) was the most important aroma-active compound in the cold-pressed sesame oil, followed by (E,E)-2,4-decadienal (earthy, 4170 µg/kg, OAV = 31), dimethyl sulfone (sulphur-like, 406 µg/kg, OAV = 20) and octanal (green and fruity, 901 µg/kg, OAV = 16). This study provides valuable information for manufacturers to achieve precise flavour control of sesame oil products.

Pectic polysaccharides extracted from sesame seed hull: Physicochemical and functional properties.

The objective of the present investigation was to extract pectic polysaccharides from sesame seed hull and to determine their physicochemical and functional characteristics. The pectic polysaccharides in the seed hull were extracted with HCl and then collected at three ethanol concentrations of 30% (SSP30), 50% (SSP50), and 90% (SSP90). We found that SSP30 represented 75.6% of the total polysaccharides, and that it contained 76.39% galacturonic acid, with many HG domains and few short side chains in the RG-I domains. SSP30 exhibited the strongest hydroxyl radical scavenging activity among the three fractions, and was better able to stabilize the emulsions. Higher Mw pectic polysaccharides were firstly precipitated at lower ethanol concentrations, and the Mw of the precipitated pectic polysaccharides decreased with increasing ethanol concentration. These results provide important information on the structure and functional characteristics of sesame hull polysaccharides. This information can contribute to the future development of sesame hull polysaccharides for industrial purposes.

Structural changes of lignin-carbohydrate complexes (LCCs) from Chinese quince fruits during the sequential fractionation of pectic and hemicellulosic polysaccharides.

Chinese quince (Chaenomeles sinensis) fruits offer a potential source of pectin and hemicellulose. However, the existence of lignin-carbohydrate complexes (LCCs) can negatively impact the extraction of pectin and hemicellulose. In this work, LCCs were sequentially fractionated from Chinese quince during the removal of pectin and hemicellulose. The structures of LCCs were characterized by HPAEC, FT-IR, GPC, Py-GC/MS, TGA and 2D HSQC NMR. The results showed that the carbohydrate content and molecular weight of LCCs was found to be changed significantly after the removal of hemicellulose (KSH). The lignin in Björkman LCCs was found to be linked mainly to galactan and fructan, whereas the lignin LCC-AcOHs was found to be linked mainly to arabinan after the removal of KSH. The isolation of carbonate-soluble pectin (NSP) increased thermal stability of Björkman LCC fraction, however, the isolation of chelator-soluble pectin (CSP) increased the thermal stability of LCC-AcOHs. The S/G ratios of LCC-AcOHs increased and large amounts of S-type lignin released during sequential fractionation of pectin and hemicellulose. These results will be beneficial for understanding the mechanisms of pectin and hemicellulose isolation, thereby facilitating the potential application of Chinese quince as a valuable natural resource for food and other industries.

Structural Changes in Milled Wood Lignin (MWL) of Chinese Quince (Chaenomeles sinensis) Fruit Subjected to Subcritical Water Treatment.

Subcritical water treatment has received considerable attention due to its cost effectiveness and environmentally friendly properties. In this investigation, Chinese quince fruits were submitted to subcritical water treatment (130, 150, and 170 °C), and the influence of treatments on the structure of milled wood lignin (MWL) was evaluated. Structural properties of these lignin samples (UL, L130, L150, and L170) were investigated by high-performance anion exchange chromatography (HPAEC), FT-IR, gel permeation chromatography (GPC), TGA, pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS), 2D-Heteronculear Single Quantum Coherence (HSQC) -NMR, and 31P-NMR. The carbohydrate analysis showed that xylose in the samples increased significantly with higher temperature, and according to molecular weight and thermal analysis, the MWLs of the pretreated residues have higher thermal stability with increased molecular weight. The spectra of 2D-NMR and 31P-NMR demonstrated that the chemical linkages in the MWLs were mainly ß-O-4' ether bonds, ß-5' and ß-ß', and the units were principally G- S- H- type with small amounts of ferulic acids; these results are consistent with the results of Py-GC/MS analysis. It is believed that understanding the structural changes in MWL caused by subcritical water treatment will contribute to understanding the mechanism of subcritical water extraction, which in turn will provide a theoretical basis for developing the technology of subcritical water extraction.

Effects of various oil extraction methods on the gelatinization and retrogradation properties of starches isolated from tigernut (Cyperus esculentus) tuber meals.

Gelatinization and retrogradation characteristics of starches from tigernut (Cyperus esculentus) tuber before and after various oil extraction processes were studied in this investigation. The results indicated that starches isolated from tigernut tuber after the various oil extraction processes varied significantly in gelatinization and retrogradation properties. The starches isolated from the cakes of tigernut tuber after hot press extraction exhibited higher retrogradation tendency and relatively less shear-thinning than other starch samples. The results of FT-IR, XRD, and NMR analysis indicated that oil extraction had an unfavorable influence on starch retrogradation, which may be due to structural changes caused by oil extraction processes. In particular, oil extraction led to more efficient packing of double helices in the crystalline lamella of the starches during storage. Retrogradation of the starch gels also reduced the water holding capacities of the starches. The starch sample isolated from the cake after cold press extraction exhibited the highest water absorption capacity among the five samples for all storage times. This investigation provides valuable novel information for the industrial utilization of tigernut tuber starches isolated from meals and cakes after oil extraction.

Ultrasound-assisted desolventizing of fragrant oil from red pepper seed by subcritical propane extraction.

In the present study, ultrasound was used to remove the residual solvent from the fragrant oil of red pepper seed obtained by subcritical propane extraction. The physical and chemical characteristics, particularly the volatile flavor compounds present of the oil before and after ultrasound-assisted desolventizing were comprehensively analyzed to determine the effect of the desolventizing process on product quality. The results showed that the maximum loss of residual solvent was achieved at a temperature of 90 °C maintained for 70 min with ultrasound applied during the entire process. After this treatment only a small amount of solvent (2.3% based on the total residual solvent originally present) remained in the oil. Although it was hypothesized that ultrasound treatment could result in the loss of volatile components, the analytical results showed no obvious reduction in the components associated with the typical aroma of the oil. After ultrasonic treatment, the oil also had good oxidation stability and quality. Additionally, after ultrasonic desolventizing, the oil samples were more suitable for cooking because they could more effectively minimize oxidation. Thus, these results demonstrate that this new ultrasonic technique is an effective and efficient method for removing the solvent remaining in fragrant oil after subcritical propane extraction.

Improvement of the oxidative stability of cold-pressed sesame oil using products from the Maillard reaction of sesame enzymatically hydrolyzed protein and reducing sugars.

BACKGROUND: In recent years, cold-pressed oils have become more and more popular with consumers. However, their oxidative stability is low. Improving the oxidative stability of cold-pressed oils will increase their shelf life. Maillard reaction products (MRPs) have been shown to promote the oxidative stability of lipids. In this study, products from the Maillard reaction of reducing sugars and sesame enzymatically hydrolyzed protein (SEHP) were added to cold-pressed sesame oils to improve their oxidative stability. RESULTS: Three types of MRPs from reducing sugars (xylose, fructose, and glucose) and SEHP were prepared. Xylose-SEHP MRPs prepared under optimum conditions had the highest antioxidant activities among the three. The optimum conditions for xylose-SEHP were as follows: reaction temperature, 130 °C; reaction time, 180 min; pH, 6.5; and sugar/protein ratio, 10:1. The addition of xylose-SEHP MRPs at a level of 20 g kg-1 could significantly improve the oxidative stability of cold-pressed sesame oil. Besides, the addition of MRPs reduced the loss of tocopherol. The interaction of MRPs with endogenous antioxidants in the sesame oil (sesamol and tocopherol) was proved by comparison with lard. There was a synergistic increase in antioxidant activity for the combination of MRPs and sesamol and the combination of MRPs and tocopherol. CONCLUSIONS: The results provide evidence that adding certain MRPs can improve the oxidative stability of cold-pressed sesame oil. © 2019 Society of Chemical Industry.

Structure, rheological, thermal and antioxidant properties of cell wall polysaccharides from Chinese quince fruits.

To investigate the composition and structural characteristics of cell wall polysaccharides, three pectic fractions and two hemicellulose fractions, namely water-soluble pectin (WSP), chelator-soluble pectin (CSP), sodium carbonate-soluble pectin (NSP), 1 mol/L KOH soluble hemicellulose (KSH-1) and 4 mol/L KOH soluble hemicellulose (KSH-2), were isolated from Chinese quince fruits. The five fractions exhibited structural and compositional variation. The results showed NSP was the predominant cell wall polysaccharide fraction in the fruit. All pectic fractions had a low degree of esterification (31.7-42.4%). WSP fraction had the highest thermal stability among the five fractions. The polysaccharide chain lengths ranged from 19.4 nm to 121.4 nm. CSP had the highest molecular weight, giving it also the highest solution viscosity. NMR spectra revealed that NSP was composed of RG-I and galacturonic acid main chains, KSH-1 was composed of 1,4-ß-D-Xylp backbone attached to 1,5-α-L-Araf units. Among the five fractions, CSP has the highest DPPH radical scavenging activity while KSH-1 has the highest reducing power. This study can contribute to the applications of Chinese quince fruit polysaccharides in food and pharmaceutical industries.

Effect of drying pretreatment methods on structure and properties of pectins extracted from Chinese quince fruit.

Pectin was extracted from the sun-dried, lyophilized, and subcritical dimethyl ether (DME) dewatered fruits as well as fresh fruits, giving rise to fractions SP, LP, DP, and FP, respectively. The structure and properties of the pectin samples were investigated. Among all the pectin samples, LP had the highest yield (10.49%), the highest molar mass (Mw 65,120 g/mol), and the highest water holding capacity, and was the most thermally stable. In addition, LP exhibited the highest DPPH scavenging activity and reducing power. DP had the highest degree of esterification (72.95%), the lowest molar mass (Mw 45,860 g/mol), and the highest oil holding capacity. The four pectin samples had different surface morphology. At the concentration of 2.5% (w/w) in water, all four pectins presented pseudo-plastic behavior. The study provides theoretical support for the potential application of Chinese quince pectin in food field.

Subcritical Fluid Extraction of Chinese Quince Seed: Optimization and Product Characterization.

Chinese quince seed (CQS) is an underutilized oil source and a potential source of unsaturated fatty acids and α-tocopherol-rich oil. Subcritical fluid (SCF) extraction is executed at lower pressures and temperatures than the pressures and temperatures used in supercritical fluid extraction. However, no studies on the SCF extraction of CQS oil are reported. Therefore, the objective of this study was to evaluate the use of SCF for the extraction of CQS oil and to compare the use of SCF with the classical Soxhlet (CS) and supercritical CO2 (SC-CO2) extraction methods. Response surface methodology (RSM) was used to investigate the extraction conditions: temperature (45-65 °C), time (30-50 min), and solvent/solid ratio (5-15 mL/g). The optimization results showed that the highest yield (27.78%) was obtained at 56.18 °C, 40.20 min, and 12.57 mL/g. The oil extracted by SCF had a higher unsaturated fatty acid content (86.37%-86.75%), higher α-tocopherol content (576.0-847.6 mg/kg), lower acid value (3.97 mg/g), and lower peroxide value (0.02 meq O2/kg) than extractions using CS and SC-CO2 methods. The SCF-defatted meal of oilseed exhibited the highest nitrogen solubility index (49.64%) and protein dispersibility index (50.80%), demonstrating that SCF extraction was a promising and efficient technique as an alternative to CS and SC-CO2 methods, as very mild operating conditions and an eco-friendly solvent can be used in the process with maximum preservation of the quality of the meal.

Extraction of Fenugreek (Trigonella foenum-graceum L.) Seed Oil Using Subcritical Butane: Characterization and Process Optimization.

In this study, the subcritical butane extraction process of fenugreek seed oil was optimized using response surface methodology with a Box-Behnken design. The optimum conditions for extracted oil from fenugreek seed was as follows: extraction temperature of 43.24 °C , extraction time of 32.80 min, and particle size of 0.26 mm. No significant differences were found between the experimental and predicted values. The physical and chemical properties of the oil showed that the oil could be used as edible oil. Fatty acid composition of oils obtained by subcritical butane under the optimum conditions and by accelerated solvent extraction showed negligible difference. The oils were rich in linoleic acid (42.71%-42.80%), linolenic acid (26.03%-26.15%), and oleic acid (14.24%-14.40%). The results revealed that the proposed method was feasible, and this essay shows the way to exploit fenugreek seeds by subcritical butane extraction under the scope of edible oils.

Process optimization and characterization of fragrant oil from red pepper (Capsicum annuum L.) seed extracted by subcritical butane extraction.

BACKGROUND: Red pepper seeds account for 450-500 g kg-1 of the total pepper weight and are often discarded as waste. In this study, process optimization and characterization of fragrant oil from roasted red pepper seed extracted by subcritical butane extraction were carried out. RESULTS: The optimal conditions of extraction were a temperature of 74.61 °C, a time of 68.65 min and a liquid/solid ratio of 30.24:1. The oil had a refractive index (25 °C) of 1.471, a relative density of 0.900, an acid value of 1.421 mg g-1 oil, an iodine value of 127.035 g per 100 g, a saponification value of 184.060 mg KOH g-1 , an unsaponifiable matter content of 12.400 g kg-1 , a peroxide value of 2.465 meq. O2 kg-1 and a viscosity of 52.094 cP. The main fatty acids in the oil were linoleic acid (72.95%) followed by palmitic acid (11.43%) and oleic acid (10.00%). The oil showed desirable thermal and oxidative stability. A total of 19 volatile compounds, mostly aldehydes and alkenes, were identified from the oil. CONCLUSION: The results indicated that the method is appropriate for the preparation of fragrant red pepper seed oil, and the oil is suitable for used as edible oil. © 2016 Society of Chemical Industry.

One-step solvent extraction followed by liquid chromatography-atmospheric pressure photoionization tandem mass spectrometry for the determination of polycyclic aromatic hydrocarbons in edible oils.

A method for rapid analysis of 16 polycyclic aromatic hydrocarbons (PAHs) in edible oils has been developed on the basis of a simplified solvent extraction and liquid chromatography-atmospheric pressure photoionization tandem mass spectrometry performed in multiple reaction monitoring mode. The briefness of the experimental procedure, the use of milliliters of acetonitrile for extraction without any further cleanup process, the short analysis time, and the excellent sensitivity and selectivity demonstrated the advantages of this practical and environmentally friendly method. All the analytes exhibited satisfactory recoveries at three spiking levels (the recoveries ranged from 77.8 to 106.4%), and the relative standard deviations were lower than 10%. The limits of quantitation of this method for the 16 PAHs were in the range of 0.02-0.43 µg/kg. The validated method was successfully applied for the determination of PAHs in coconut oil reference material (BCR-458) and real edible oil samples. The results suggested that a large-scale investigation of the concentration of PAHs in vegetable oils in China is required.

Hydrothermal liquefaction of cornstalk: 7-lump distribution and characterization of products.

Hydrothermal liquefaction of cornstalk at 180-300 °C at ratios of water to cornstalk of 6-14 was conducted, and the reaction products were lumped into gas, water-soluble organics (ethanol-insoluble and ethanol-soluble organics), heavy oil, volatile organic compounds, and acid-soluble and acid-insoluble solid residues. Low temperature, high ratio of water to cornstalk, and short reaction time favored the formation of bio-oil (ethanol-insoluble organics, ethanol-soluble organics, and heavy oil) but inhibited the formation of acid-insoluble solid residue. Increasing temperature and reaction time increased the yields of gas and volatile organic compounds, whereas decreased the yield of acid-soluble solid residue. Bio-oil yields increased first and then decreased at a ratio of water to cornstalk higher than 10. Overall, the studied reaction parameters influenced the conversion among the lumps and product properties. This study suggests that lump analysis provides a promising approach to describe the product distributions in biomass liquefaction.