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.

Targeted metabolomics combined with network pharmacology to reveal the protective role of luteolin in pulmonary arterial hypertension.

Pulmonary arterial hypertension (PAH) is a progressive disease that significantly endangers human health, where metabolism may drive pathogenesis: a shift from mitochondrial oxidation to glycolysis occurs in diseased pulmonary vessels and the right ventricle. An increase in pulmonary vascular resistance in patients with heart failure with a preserved ejection fraction portends a poor prognosis. Luteolin exists in numerous foods and is marketed as a dietary supplement assisting in many disease treatments. However, little is known about the protective effect of luteolin on metabolism disorders in diseased pulmonary vessels. In this study, we found that luteolin apparently reversed the pulmonary vascular remodeling of PAH rats by inhibiting the abnormal proliferation of pulmonary artery smooth muscle cells (PASMCs). Moreover, network pharmacology and metabolomics results revealed that the arachidonic acid pathway, amino acid pathway and TCA cycle were dysregulated in PAH. A total of 14 differential metabolites were significantly changed during the PAH, including DHA, PGE2, PGD2, LTB4, 12-HETE, 15-HETE, PGF2α, and 8-iso-PGF2α metabolites in the arachidonic acid pathway, and L-asparagine, oxaloacetate, N-acetyl-L-ornithine, butane diacid, ornithine, glutamic acid metabolites in amino acid and TCA pathways. However, treatment with luteolin recovered the LTB4, PGE2, PGD2, 12-HETE, 15-HETE, PGF2α and 8-iso-PGF2α levels close to normal. Meanwhile, we showed that luteolin also downregulated the gene and protein levels of COX 1, 5-LOX, 12-LOX, and 15-LOX in the arachidonic acid pathway. Collectively, this work highlighted the metabolic mechanism of luteolin-protected PAH and showed that luteolin would hold great potential in PAH prevention.

Zingerone (4-(four-hydroxy-3-methylphenyl) butane-two-1) modulates adjuvant-induced rheumatoid arthritis by regulating inflammatory cytokines and antioxidants.

OBJECTIVE: Ginger (Zingiber officinale Roscoe) is considered to be one of the most commonly consumed dietary condiments of the world. The present study was designed to explicate the protective role of zingerone; an active ingredient of ginger in complete Freund's adjuvant (FCA)-immunized arthritic rats. METHODS: 24 Wistar rats were divided into 4 groups with 6 rats each. Group I as control followed by group II, III and IV were treated with single intradermal injection of FCA (0.1 ml = 100 µg) to induce rheumatoid arthritis. Group III and IV were also administered with zingerone orally at 25 mg/kg b.w for 3 weeks at two different time points. RESULTS: Adjuvant-treated rats exhibited a significant increase in lipid peroxidation and a reduction in the enzymatic antioxidants such as SOD, catalase and GPx, in the liver and joint tissues. Moreover, FCA inoculation resulted in the increase in levels of NF-κB, TGF-ß, TNF-α, IL-1ß, IL-6 and Hs-CRP and a decrease in IL-10 levels. Zingerone significantly reduced the levels of NF-κB, TGF-ß, TNF-α, IL-1ß, IL-6 and Hs-CRP and markedly increased IL-10 levels. Levels of antioxidant enzymes were also restored by zingerone treatment. DISCUSSION: Oral administration of zingerone ameliorated inflammatory outburst and decreased oxidative stress, suggesting its role in the prevention of rheumatoid arthritis. Further mechanistic insights are necessary to study the exact mechanism involved.

Extraction and Characterization of Flaxseed Oil Obtained with Subcritical n-Butane.

In this study, subcritical n-butane was adopted to extract oil from flaxseed. The extraction conditions i.e. extraction temperature, extraction time, and liquid-solid ratio were investigated and optimized by response surface methodology. The flaxseed oil obtained by subcritical n-butane were characterized and compared with those prepared by n-hexane and cold pressing. Results indicated that the optimal combination of parameters was 53.93℃, 56.82 min, and 19.98:1 mL/g. Subcritical n-butane had higher yield (28.75%) than n-hexane and cold pressing. GC analysis indicated that subcritical n-butane extraction had no obvious influence on the fatty acid composition. Nevertheless, the oil obtained by subcritical n-butane with higher contents of phytosterols (2.93 mg/g) and carotenoids (46.56 mg/kg), and presented a higher oxidation stability (9.27 h). Thus, it was suggested that subcritical n-butane extraction is a promising alternative to extract high quality flaxseed oil.

A novel and efficient subcritical butane extraction method and UHPLC analysis of oxyprenylated phenylpropanoids from grapefruits peels.

Biologically active prenyoxyphenylpropanoids are well known to be biosynthesized by Citrus species, for which they have been found most abundantly in fruit peels. Although several extraction methodologies have been described, the development of novel and alternative extraction processes is a field of research of current interest. In this preliminary communication, we studied the performance of the subcritical butane promoted extraction of selected oxyprenylated phenylpropanoids from grapefruit peels under a counter-current mode using a handmade extraction apparatus coupled to UHPLC analysis. The application of such a method yielded 7-isopentenyloxycoumarin, auraptene, and boropinic acid in quantities higher than those recorded for other extraction methodologies like the ultrasound- and microwave-assisted macerations (0.234, 1.035, and 0.211 mg/g of dry extract respectively). The use of subcritical butane as the extraction solvent for oxyprenylated phenylpropanoids is reported herein for the first time and can be easily adopted for several other food matrices.

Cyhalofop-butyl and Glyphosate Multiple-Herbicide Resistance Evolved in an Eleusine indica Population Collected in Chinese Direct-Seeding Rice.

Eleusine indica is a typical xerophytic weed species with a cosmopolitan distribution. It is invasive and highly adaptable to diverse habitats and crops. Due to rice cropping-pattern changes, E indica has become one of the main dominant grass weeds infecting direct-seeding paddy fields. A Chinese E. indica population has evolved multiple-herbicide resistance to cyhalofop-butyl and glyphosate. In this study, the multiple-resistance profile of E. indica to these two different types of herbicides and their resistance mechanisms were investigated. Whole-plant dose-response assays indicated that the multiple-herbicide-resistant (MHR) population exhibited 10.8-fold resistance to cyhalofop-butyl and 3.1-fold resistance to glyphosate compared with the susceptible (S) population. ACCase sequencing revealed that the Asp-2078-Gly mutation was strongly associated with E. indica resistance to cyhalofop-butyl. The MHR plants accumulated less shikimic acid than S plants at 4, 6, and 8 days after glyphosate treatment. In addition, no amino acid substitution in the EPSPS gene was found in MHR plants. Further analysis revealed that the relative expression level of EPSPS in MHR plants was 6-10-fold higher than that in S plants following glyphosate treatment, indicating that EPSPS overexpression may contribute to the glyphosate resistance. Furthermore, the effectiveness of nine post-emergence herbicides against E. indica were evaluated, and one PPO inhibitor pyraclonil was identified as highly effective in controlling the S and MHR E. indica populations.

Molecular basis of resistance to ACCase-inhibiting herbicide cyhalofop-butyl in Chinese sprangletop (Leptochloa chinensis (L.) Nees) from China.

Chinese sprangletop (Leptochloa chinensis (L.) Nees) is one of the most troublesome grass weeds in rice in China. Seven suspected cyhalofop-butyl-resistant L. chinensis populations were collected from different rice fields with a history of cyhalofop-butyl use. The level of resistance and resistance mechanisms in seven populations were studied. Dose-response tests indicated that five populations (JS3, JS4, JS6, JS7 and JS8) had evolved high-level resistance (26.9 to 123.0-fold) to cyhalofop-butyl compared with the susceptible (S) population, and other two populations (JS2 and JS5) were still sensitive to the herbicide. Two acetyl-coenzyme A carboxylase (ACCase) genes were cloned from each population, and three different ACCase mutations (Ile-1781-Leu, Trp-1999-Cys, and Trp-2027-Cys) in ACCase2 gene were determined in different resistant (R) populations. In addition, no resistance-conferring mutations was detected in the R population (JS7), and ACCase gene expression was similar between the S and R populations. Thus, non-target-site resistance mechanisms may be involved in the JS7 population. Moreover, the patterns of cross-resistance of JS6 (Ile-1781-Leu), JS4 (Trp-1999-Cys), JS8 (Trp-2027-Cys), and JS7 (unknown resistance mechanisms) populations to other ACCase-inhibiting herbicides were determined. The JS6 and JS8 populations showed resistance to fenoxaprop-P-ethyl, metamifop, clethodim and pinoxaden, the JS4 population was resistant to fenoxaprop-P-ethyl, metamifop and pinoxaden, and the JS7 population had resistance only to fenoxaprop-P-ethyl and metamifop. These results indicated the diversity of the target-site mutations in ACCase gene of L. chinensis, and provide a better understanding of cross-resistance in L. chinensis, which would be helpful for the management of cyhalofop-butyl-resistant L. chinensis.

Rhodopseudomonas palustris wastewater treatment: Cyhalofop-butyl removal, biochemicals production and mathematical model establishment.

Simultaneous (SPW and cyhalofop-butyl) wastewater treatment and the production of biochemicals by Rhodopseudomonas palustris (R. palustris) was investigated with supplementation of soybean processing wastewater (SPW). Compared to control group, cyhalofop-butyl was removed and single cell protein, carotenoid, bacteriochlorophyll productions were enhanced with the supplementation of SPW. Cyhalofop-butyl removal reached 100% after 5 days under 4000 mg/L COD group. Cyhalofop-butyl induced chbH gene expression to synthesize cyhalofop-butyl-hydrolyzing carboxylesterase through activating MAPKKKs, MAPKKs, MAPKs genes in MAPK signal transduction pathway. The induction process took one day for R. palustris. However, lack of organics in original wastewater did not maintain R. palustris growth for over one day. The supplementation of SPW provided sufficient carbon source. This new method resulted in the mixed wastewater treatment and improvement of biochemicals simultaneously, as well as the realization of reutilization of R. palustris. High-order non-linear mathematical model of the relationship between Rchb, Xc, and Xt was established.

A preliminary investigation of lung availability of cannabinoids by smoking marijuana or dabbing BHO and decarboxylation rate of THC- and CBD-acids.

Highly potent cannabis concentrates obtained by butane or by supercritical carbon dioxide-extraction are gaining popularity. These extracts called butane hash oil (BHO) with Δ9-tetrahydrocannabinolic acid A (THCA) contents above 60% are consumed by flash vaporization on a glowing titanium nail, followed by inhalation of the resulting vapor through a water pipe in a single puff - a technique referred to as "dabbing". We herein investigated the decarboxylation rate of THCA during artificial smoking of cannabis plant material and simulated dabbing, and the lung availability of Δ9-tetrahydrocannabinol (THC) which we define as the recovery of THC in the smoke and vapor condensates. Preliminary smoking and dabbing experiments were performed using an apparatus built in-house. Due to availability of cannabidiol (CBD)-rich hemp in Switzerland, we included a sample of CBD flowers in our experiments and investigated the decarboxylation and recovery of cannabidiolic acid (CBDA) and CBD, respectively. Decarboxylation of THCA and CBDA during combustion of the plant material and vaporization of the BHO, respectively, was complete. The high recovery of total THC (75.5%) by dabbing cannot be achieved by smoking marijuana. Lung availability ranged from 12% for mixed cannabis material with a rather low THC content, to approximately 19-27% for marijuana flowers, similar for THC in marijuana as for CBD in CBD-rich marijuana. In reality, when smoking a joint, further losses in recovery must be assumed by additional sidestream smoke. The rather high lung availability of THC via dabbing can explain the increased psychoactive and adverse effects associated with this new trend of cannabis consumption.

Process Optimization, Characterization and Antioxidant Capacity of Oat (Avena Sativa L.) Bran Oil Extracted by Subcritical Butane Extraction.

Oat bran is a traditional agricultural byproduct and rarely used in edible oil processing. In this paper, oat bran oil (OBO) was firstly extracted by subcritical butane extraction (SBE) and the extraction process was optimized using response surface methodology. Three variables involving liquid-to-solid ratio, extraction time and extraction temperature were studied. The optimum conditions for extraction of OBO were obtained as follows: liquid-to-solid ratio 4.30, extraction time 48.15 min, and extraction temperature 46.52 °C. Based on this, an alternative method (SBE-e) for cosolvent (ethanol) was proposed to improve SBE method. Compared to conventional hexane extraction (CHE), the SBE-e had significant effect on yield, bioactive compounds (phytosterols and phenols) and antioxidant capacity (AC) in the extracted OBO. The results indicated that the proposed methods were appropriate for OBO extraction. Additionally, OBO had the potential to be an acceptable substitute for edible oil, owing to its desirable physicochemical characteristics, a balanced fatty acids composition and high antioxidant capacity.

Isobutylhydroxyamides from Sichuan Pepper and Their Protective Activity on PC12 Cells Damaged by Corticosterone.

The pericarp of Zanthoxylum bungeanum Maxim., commonly known as Sichuan pepper, is a widely used spice to remove fishy odor and add palatable taste. A phytochemical investigation of the 95% ethanol extract of Sichuan pepper resulted in the isolation of 21 isobutylhydroxyamides, including 8 new ones named ZP-amides G-N, among which the chiral resolution of racemic ZP-amide A and ZP-amide B was successfully accomplished. The protective activity on corticosterone-treated PC12 cells of the isolated isobutylhydroxyamides was also evaluated. The new compounds 3-5 and the known compounds 1, 1a, 2, 2a, 11, and 15 improved the survival rate of PC12 cells. The bioactivity studies disclosed the potential of Sichuan pepper to be developed as new neuroprotective functional food.

Zeolites as Catalysts for Fuels Refining after Indirect Liquefaction Processes.

The use of zeolite catalysts for the refining of products from methanol synthesis and Fisher-Tropsch synthesis was reviewed. The focus was on fuels refining processes and differences in the application to indirect liquefaction products was compared to petroleum, which is often a case of managing different molecules. Processes covered were skeletal isomerisation of n-butenes, hydroisomerisation of n-butane, aliphatic alkylation, alkene oligomerisation, methanol to hydrocarbons, ethanol and heavier alcohols to hydrocarbons, carbonyls to hydrocarbons, etherification of alkenes with alcohols, light naphtha hydroisomerisation, catalytic naphtha reforming, hydroisomerisation of distillate, hydrocracking and fluid catalytic cracking. The zeolite types that are already industrially used were pointed out, as well as zeolite types that have future promise for specific conversion processes.

Cardamom extract induces cell proliferation by increasing potassium currents in NIH3T3 cell line.

Amommum subulatum (Roxb.) or Cardamom extract is known to have anti-inflammatory and neuroprotective effects towards many gastrointestinal related problems. However, uptill now different fractions of cardamom extract on fibroblasts with respect to potassium channel activity have not been investigated. Therefore, present study investigated the effects of different fractions of cardamom extract on potassium channels in non-tumor NIH3T3 cell line. Phytochemical analysis of hydroalcoholic, n-hexane, butane and ethyl acetate fractions of cardamom extracts were purified and isolated by thin layer chromatography (TLC). 3T3 cells were cultured and incubated with hydroalcohol (1-2 µ/ml), n-hexane (1 µ/ml), butane (2 µ/ml) and ethyl acetate (1-2 µ/ml) for 5 hrs at 37°C. Modulation in potassium currents were recorded by whole-cell patch clamp method. The data showed two constituents Cineol (C10H18O) and Terpinyl acetate (C10H17OOCCH3) by TLC method. The present study shows that the constituents in n-hexane, hydro alcohol (1 µ/ml) and ethyl acetate (2 µ/ml) significantly increased (p<0.01) the potassium outward rectifying currents from NIH3T3 cells when compared to untreated controls cells. Whereas, butanol fraction (2 µ/ml) significantly decreased (p<0.01) the inward rectifying currents when compared to controls. Moreover hydroalcoholic and n-hexane fractions have increased the proliferation in 3T3 cell line. On the other hand butanol and ethyl acetate did not induce proliferation in 3T3 cells. Taken together, our data suggested that cardamom extract contains constituents that increased K+ currents, cell migration and proliferation and are involved in wound healing.

Highly Selective and Considerable Subcritical Butane Extraction to Separate Abamectin in Green Tea.

We specially carried out the subcritical butane extraction to separate abamectin from tea leaves. Four parameters, such as extraction temperature, extraction time, number of extraction cycles, and solid-liquid ratio were studied and optimized through the response surface methodology with design matrix developed by Box-Behnken. Seventeen experiments with three various factors and three variable levels were employed to investigate the effect of these parameters on the extraction of abamectin. Besides, catechins, theanine, caffeine, and aroma components were determined by both high-performance liquid chromatography and gas chromatography-mass spectrometry to evaluate the tea quality before and after the extraction. The results showed that the extraction temperature was the uppermost parameter compared with others. The optimal extraction conditions selected as follows: extraction temperature, 42°C; number of extraction cycles and extraction time, 1 and 30 min, respectively; and solid-liquid ratio, 1:10. Based on the above study, the separation efficiency of abamectin was up to 93.95%. It is notable that there has a quite low loss rate, including the negligible damage of aroma components, the bits reduce of catechins within the range of 0.7%-13.1%, and a handful lessen of caffeine and theanine of 1.81% and 2.6%, respectively. The proposed method suggested subcritical butane possesses solubility for lipid-soluble pesticides, and since most of the pesticides are attached to the surfaces of tea, thus the as-applied method was successfully effective to separate abamectin because of the so practical and promising method.

An unusual etiology in cold injury: Liquefied petroleum gas.

Cold injury is a condition that causes reversible and irreversible damage when tissues are exposed to cold. This injury occurs due to various etiologies, and the most commonly observed ones include contact with liquefied petroleum gas (LPG) used in households, vehicles, and industry. LPG is a type of gas stored in liquid state under high pressure within cylinders. LPG contains a mixture of propane and butane gases. Direct contact of these gases with the tissues has the potential to cause metabolic, toxic, and respiratory damage. In this study, we present the cases of four patients with cold injury in the face and upper extremity caused by a pressurized jet stream of liquid gas that escaped out of the valves of the LPG cylinders. The patients had bullous lesions in the upper extremities and the face and second- and third-degree cold injuries with fibrotic and necrotic areas. The superficial defects secondarily healed with minimal scarring, while the necrotic finger had to be amputated. Cold injury on the skin caused by high-pressure jet streams of liquid gas as in our study is a rare occurrence. Our patients are important cases due to the rare etiology of cold injury.

Effective Subcritical Butane Extraction of Bifenthrin Residue in Black Tea.

As a natural and healthy beverage, tea is widely enjoyed; however, the pesticide residues in tea leaves affect the quality and food safety. To develop a highly selective and efficient method for the facile removal of pesticide residues, the subcritical butane extraction (SBE) technique was employed, and three variables involving temperature, time and extraction cycles were studied. The optimum SBE conditions were found to be as follows: extraction temperature 45 °C, extraction time 30 min, number of extraction cycles 1, and in such a condition that the extraction efficiency reached as high as 92%. Further, the catechins, theanine, caffeine and aroma components, which determine the quality of the tea, fluctuated after SBE treatment. Compared with the uncrushed leaves, pesticide residues can more easily be removed from crushed leaves, and the practical extraction efficiency was 97%. These results indicate that SBE is a useful method to efficiently remove the bifenthrin, and as appearance is not relevant in the production process, tea leaves should first be crushed and then extracted in order that residual pesticides are thoroughly removed.

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.

Effects of a dietary ketone ester on hippocampal glycolytic and tricarboxylic acid cycle intermediates and amino acids in a 3xTgAD mouse model of Alzheimer's disease.

In patients with Alzheimer's disease (AD) and in a triple transgenic (3xTgAD) mouse model of AD low glucose metabolism in the brain precedes loss of memory and cognitive decline. The metabolism of ketones in the brain by-passes glycolysis and therefore may correct several deficiencies that are associated with glucose hypometabolism. A dietary supplement composed of an ester of D-ß-hydroxybutyrate and R-1,3 butane diol referred to as ketone ester (KE) was incorporated into a rodent diet and fed to 3xTgAD mice for 8 months. At 16.5 months of age animals were killed and brains dissected. Analyses were carried out on the hippocampus and frontal cortex for glycolytic and TCA (Tricarboxylic Acid) cycle intermediates, amino acids, oxidized lipids and proteins, and enzymes. There were higher concentrations of d-ß-hydroxybutyrate in the hippocampus of KE-fed mice where there were also higher concentrations of TCA cycle and glycolytic intermediates and the energy-linked biomarker, N-acetyl aspartate compared to controls. In the hippocampi of control-fed animals the free mitochondrial [NAD+ ]/[NADH] ratio were highly oxidized, whereas, in KE-fed animals the mitochondria were reduced. Also, the levels of oxidized protein and lipids were lower and the energy of ATP hydrolysis was greater compared to controls. 3xTgAD mice maintained on a KE-supplemented diet had higher concentrations of glycolytic and TCA cycle metabolites, a more reduced mitochondrial redox potential, and lower amounts of oxidized lipids and proteins in their hippocampi compared to controls. The KE offers a potential therapy to counter fundamental metabolic deficits common to patients and transgenic models. Read the Editorial Highlight for this article on page 162.

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.