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Carrot rhamnogalacturonan-I (cRG-I) is a polydisperse polysaccharide with molecular weights of 7-250 kDa. Using size exclusion chromatography cRG-I was fractionated and pooled in fractions (PF1-6). All fractions contained the same RG-I monosaccharides and similar glycosidic linkages although in varying relative amounts. The main differences were in rhamnose substitution, arabinan- and galactan side chain length and in levels of acetylation and methyl esterification. Atomic force microscopy showed either spheric or elongated structures for cRG-I and its derived fractions. To gain insight in the structure-function relationship of cRG-I, the immunomodulatory effect of the six fractions and their saponified derivatives was assessed in vitro. All fractions, except PF2, dose-dependently stimulated TNFα, IL-6, IL-1β, IL-8 and IL-10 production in peripheral blood mononuclear cells (PBMCs) of three healthy donors. Cytokine levels were largely influenced by the Mw and degree of esterification of the individual fractions. Notably, the highest Mw fraction (100 kDa) displayed the most potent activity, which was strongly reduced after the removal of ester residues by saponification. In contrast, the 75 kDa Mw population (PF2) proved inactive while its saponified counterpart exhibited substantial immunomodulatory activity. This confirmed the role of ester residues on the immune profile of RG-I subpopulations., Competing Interests: Declaration of competing interest The authors declare the following financial interests which may be considered as potential competing interests. NutriLeads holds intellectual property rights for the use cRG-I. Annick Mercenier and Ruud Albers were employed at NutriLeads and remain shareholders affiliated to NutriLeads for scientific matters., (Copyright © 2024 The Authors. Published by Elsevier Ltd.. All rights reserved.)

Background: Mineral oil aromatic hydrocarbon (MOAH) analysis in foods is a major analytical challenge. Quantification is associated with a high uncertainty. The sources of uncertainty are multiple, but the major one is related to data interpretation and integration, which is partially derived from insufficiently efficient sample preparation. Recently, an updated ISO method for the analysis of mineral oil in fats and oils and a standard operating procedure for infant formula analysis have been published. Both methods reported significantly different (up to 1.25) distributions of the internal standards used for quantification (i.e., tri-tert-butyl benzene (TBB) and 2-methyl naphthalene (2-MN)) over the different solvent phases used in the saponification step., Results: In this work, a microwave-assisted saponification and extraction method was optimized for MOAH analysis to solve the problem related to the MOAH internal standards partition. The paper examines the impact of the solvent mixture used, the concentration of KOH on the partition of TBB and 2-MN, and the effect of the matrix and the washing step to extract the unsaponifiable fraction containing the mineral oils., Significance: The optimized procedure achieved a TBB/2-MN ratio of 1.05 ± 0.01 tested in five different fats and oils, namely, sunflower, rapeseed, coconut, palm, and extra virgin olive oils. The method can significantly contribute to reducing the uncertainty of the MOAH quantification when saponification is applied., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

This work investigates the physicochemical characteristics of grease-trap wastewater discharged from a large community market. It proposes potential mechanisms of fat, oil, and grease (FOG) solid formation, separation, and accumulation inside grease traps. Sixty-four samples, i.e., the floated scum, suspended solid-liquid wastewater, and settled sludge, were collected from the grease-trap inlet and outlet chambers. A lower pH of 5-6 at 25-29 °C inside the grease trap than those reported under the sewer conditions (pH 6-7) was revealed. A significant difference in solid and dissolved constituents was also discovered between the inlet and outlet chambers, indicating that the baffle wall could affect the separation mechanism. The sludge samples had 1.5 times higher total solids (TS) than the scum samples, i.e., 0.225 vs. 0.149 g g -1 TS, revealing that the sludge amount impacted more significantly the grease trap capacity and operation and maintenance. In contrast, the scum samples had 1.4 times higher volatile solids (VS) than the sludge samples, i.e., 0.134 vs. 0.096 g g -1 VS, matching with the 64.2 vs. 29.7% of carbon content from CHN analysis. About 2/3 of the free fatty acids (FFAs) with palmitic acids were the primary saturated FFAs, while the remaining 1/3 of unsaturated FFAs were found in the solid and liquid samples. Although up to 0.511 g g -1 FOG can be extracted from the scum samples, none from the sludge samples. More diverse minerals/metals other than Na, Cl, and Ca were found in the sludge samples than in the scum samples. Grease-trap FOG solids and open drain samples exhibited similar physicochemical properties to those reported in the literature. Four potential mechanisms (crystallization, emulsification, saponification, and baffling) were presented. This work offers insights into the physicochemical properties of grease-trap wastewater that can help explore its FOG solid formation, separation, and accumulation mechanisms inside a grease trap., Competing Interests: Declaration of competing interest The authors declare the following financial interests/personal relationships which may be considered as potential competing interests: Ngie Hing Wong reports financial support was provided by Malaysia Ministry of Higher Education. If there are other authors, they declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024. Published by Elsevier Ltd.)

The results revealed the significant effect of NaCl, KCl, CaCl 2 , MgCl 2 , CaSO 4 , MgSO 4 , and Na 2 SO 4 and pH values of 3.5-11 on the interfacial tension (IFT) reduction using three types of neutral, acidic, and basic crude oils, especially for acidic crude oil (crude oil II) as the pH was changed from 3.5 to 11 (due to saponification process). The findings showed the highest impact of pH on the IFT of crude oil II with a reducing trend, especially for the pH 11 when no salts exist. The results revealed that the salts except MgCl 2 and CaCl 2 led to a similar IFT variation trend for the case of distilled water/crude oil II. For the MgCl 2 and CaCl 2 solutions, a shifting point for IFT values was inevitable. Besides, the dissolution of 1-dodecyl-3-methyl imidazolium chloride ([C 12 mim][Cl]) with a concentration of 100-1000 ppm eliminates the effect of pH on IFT which leads to a reducing trend for all the examined crude oils with minimum IFT of 0.08 mN/m. Finally, the [C 12 mim][Cl] adsorption (under pH values) for crude oils using only Na 2 SO 4 was measured and the minimum adsorption of 0.41 mg surfactant/g Rock under the light of saponification process was obtained., (© 2024. The Author(s).)

The effects of sulfate salts under low and high salinity conditions and pH of 3.5-11 on interfacial tension (IFT) reduction and IL adsorption using resinous (RSO) and asphaltenic (8 wt/wt%) synthetic oils are investigated. The measurements showed the increasing effect of pH on the IFT of RSO/DW from 23.5 to 27.3 mN/m (pH = 3.5 → 7) in the first place and a reducing effect (0.4 mN/m) if pH = 7 → 11. Using a high concentration of 50,000 ppm for MgSO 4 , and Na 2 SO 4 revealed an extensive IFT reduction for a pH value of 11 with the value of 0.20 mN/m for Na 2 SO 4 . The measured IFT values showed the significant impact of IL (500 ppm) on the IFT (minimum value of 0.01 mN/m for RSO/50,000 Na 2 SO 4  + 500 ppm 1-decyl-3-methyl imidazolium triflate ([C 10 mim][TfO])) for pH = 11. The IL adsorption measurements showed the role of in-situ surfactant production (saponification process) on the 1-decyl-3-methyl imidazolium chloride ([C 10 mim][Cl]) and [C 10 mim][TfO] adsorption reduction from 3.67 to 2.33 and 4.21 to 3.34 mg IL/g rock, respectively. The performed core flooding experiments using the optimum chemical formulation showed the possibility of tertiary oil recovery with maximum oil recovery of 28.8% based on original oil in place in the presence of 500 ppm., (© 2024. The Author(s).)

The study demonstrates the significant enhancement in oil production from a Romanian oil field using alkali-polymer (AP) flooding for reactive viscous oil. We conducted comprehensive interfacial tension (IFT) measurements across various alkali and AP concentrations, along with phase behavior assessments. Micromodel flooding experiments were used to examine pore-scale effects and select appropriate chemical concentrations. We tested displacement efficiency at the core level and experimented with different sequences and concentrations of alkali and polymers to minimize costs while maximizing the additional recovery of reactive viscous oil. The IFT analysis revealed that saponification at the oil-alkali interface significantly lowers IFT, but IFT gradually increases as soap diffuses away from the interface. Micromodels indicated that polymer or alkali injection alone achieve only minimal incremental recovery beyond waterflooding. However, AP flooding significantly enhanced incremental oil recovery by efficiently moving the mobilized oil with the viscous fluid and increasing exposure of more oil to the alkali solution. Coreflood experiments corroborated these findings. We also explored how divalent cations influence polymer concentration selection, finding that softening the injection brine significantly increased the viscosity of the AP slug.

Objective: To establish a rapid and accurate method for the determination of cholesterol in a variety of finished dishes., Methods: The samples were saponified with ethanol and potassium hydroxide solution at 80 ℃ for 0.5 h, then vortexed and mixed fully with ultrapure water, and extracted twice with 25 mL n-hexane. The extracting solution were evaporated to dryness under vacuum and redissolved by ethanol, finally determined by gas chromatograph. The sample loading solution was separated by HP-5 capillary column(30 m×0.25 mm, 0.25 μm) and quantified with external standard method., Results: The method had good linearity in the concentration range of 2.5-250 μg/mL for cholesterol and the correlation coefficient was 0.9999. The detection limit was 0.25 mg/100 g edible part, and the limit of quantification was 0.75 mg/100 g edible part. Three representative samples were picked for spiked recovery experiments with three concentration levels according to their content of cholesterol. The average recovery rates ranged from 91.1% to 101%, and the relative standard deviations were not more than 5%. The content range of cholesterol in 15 vegan dishes was from negative to 10.3 mg/100 g edible part, in 14 dishes contained meat and vegetable was from 2.34 to 80.2 mg/100 g edible part and in 9 pure meat dishes was from 25.4 to 288 mg/100 g edible part., Conclusion: Compared with the national standard method, the method is simple to operate and more friendly to the experimenter while ensuring the accuracy and sensitivity requirements. It can meet the needs of efficient batch determination of cholesterol in a variety of finished dishes.

Objective: (1) Determine if a relationship exists between ionized calcium (iCa) and pancreatic lipase (cPLI) concentration in dogs, and (2) assess for correlation between resolving hypercalcemia and cPLI concentrations in dogs after treatment for primary hyperparathyroidism (PHPT)., Samples: Phase I, 44 residual serum samples (collected April 2023) from client-owned dogs with a clinical indication for cPLI quantification. Phase II, 24 residual serum samples (collected August 2022 through February 2023) from client-owned dogs with PHPT pre- and postcorrection of hypercalcemia., Methods: Serum cPLI and iCa concentrations were measured via the Spec cPL assay and a spectrophotometric method respectively. Spearman's rank correlation coefficients were used to investigate if there was a correlation between serum calcium and cPLI concentrations. A paired t-test was used to investigate the effect of the resolution of hypercalcemia on serum cPLI concentrations., Results: Phase I, serum cPLI concentrations were negatively correlated with serum iCa concentrations (r = -.429, 95% CI [-.64, -.14], P = .005) in dogs with a clinical indication for cPLI quantification. Phase II, median serum cPLI concentrations were higher before (median: 228.5 μg/L, IQR: 351.3 μg/L) than after (median: 141.0 μg/L, interquartile ranges (IQR): 279.5 μg/L) management of hypercalcemia (PHPT model). However, the decrease in cPLI concentration was not statistically significant (P = .70)., Clinical Relevance: Calcium depletion may result in an inverse relationship between serum cPLI and iCa concentrations in dogs with a clinical indication for cPLI quantification. Hypercalcemia may be associated with an above reference interval cPLI concentration in some dogs.

A green viewpoint based on the production of soap using waste products such waste cooking oils (WCOs) and Endod ( Phytolacca dodecandra ) is presented. The process of saponification, which involves reacting triglycerides with fats and oils in an alkaline solution, produces soap. With the help of WCO and Endod as manufacturing inputs, this study intends to create high-quality, commercially viable eco-friendly soaps. The optimal blend of WCO and Endod with sodium hydroxide solution was used in the current investigation to create laundry soaps. Evaluations were done on the cleansing effects and physico-chemical makeup of prepared soap. As a reference control, the raw oil soaps made without and with frying were employed. The free caustic alkali content, chloride content, moisture content, ethanol-insoluble-matter, total fatty matter, pH, and foam height values of the prepared soap were found to be in the range of 0%, 0%, 16.56-22.52%, 0.1-3.05%, 63.41-75.46%, 9.22-9.82%, and 3.3-8.1 cm respectively. The results obtained by blending fried WCOs and Endod were comparable to the Physico-chemical properties of the Endod-free uncooked/fresh oil soap. The soap made by blending WCO and Endod has higher cleansing power and better lather formation than the prepared soap with WCO without Endod. Moreover, the observed data are comparable with similar data reported in other literature, recommended acceptable standards (EAS, CES), and from many countries including the British, Malaysia, and the Philippines. Cooking oils fried at different temperatures do not have much effect on the quality of soap making. This suggested that the blending of WCOs and Endod can be used as raw materials to prepare high-quality and economically feasible soaps by replacing imported oils and fats., Competing Interests: The authors whose names are listed immediately below title of the manuscript certify that they have NO any known conflict interest with or involvement in any organization or entity with any financial interest, or non-financial interest (such as personal or professional relationships, affiliations, knowledge or beliefs) in the subject matter or materials discussed in this manuscript., (© 2023 The Authors.)

This study investigates the composition and form of carotenoids in typical fruits and vegetables obtained through saponification or non-saponification and evaluates the correlation between carotenoids and antioxidant capacity. The results showed that the content of the total carotenoids in non-saponified broccoli was the highest, reaching 1505.93 ± 71.99 µg/g d.w. The content of the total carotenoids in pumpkin flesh and broccoli after saponification was reduced by 71.82% and 52.02%, respectively. The content of lutein in spinach decreased by 24.4% after saponification, but the content of β-carotene increased compared to non-saponification. After saponification, the total antioxidant activities of apple peel, radish peel, radish flesh, and maize were significantly increased by 30.26%, 91.74%, 425.30%, and 242.88%, respectively. Saponification also improved the antioxidant activities of carotenoids in maize under six different antioxidant assays. The highest correlation was found between the total amount of carotenoids and oxygen radical absorbance capacity (R = 0.945), whereas the correlation coefficients among reducing power, 2,2-diphenyl-1-picrylhydrazyl, 2,2'-azinobis (3-ethylbenzothiazoline-6-sulfonic acid), hydroxyl and superoxide radical scavenging activity, and total carotenoids' content were 0.935, 0.851, 0.872, 0.885, and 0.777, respectively, all showing significant correlations. The study demonstrates that saponification can increase the total carotenoid content and antioxidation for apple peel, radish peel, radish flesh, and maize. Moreover, carotenoids were significantly positively correlated with most in vitro antioxidant assays. This study provides a theoretical basis for improving the postharvest added value of fruits and vegetables and rationally utilizing their byproducts., (© 2023 Institute of Food Technologists.)

An efficient redox initiating system, ceric ammonium nitrate/nitric acid, has been employed for the first time to carry out photo-induced graft copolymerization of acrylonitrile (AN) onto sodium salt of partially carboxymethylated sodium alginate, having an average degree of substitution value to be 1.10. The photo-grafting reaction conditions for maximum grafting have been systematically optimized by varying the reaction variables such as reaction time, temperature, the concentration of acrylonitrile monomer, ceric ammonium nitrate, and nitric acid, as well as the amount of the backbone. The optimum reaction conditions are obtained with a reaction time of 4 h, reaction temperature of 30 °C, acrylonitrile monomer concentration of 0.152 mol/L, initiator concentration of 5 × 10 -3 mol/L, nitric acid concentration of 0.20 mol/L, amount of backbone of 0.20 (dry basis) and the total volume of the reaction system of 150 mL. The highest percentage of grafting (%G) and grafting efficiency (%GE) achieved are 316.53% and 99.31%, respectively. The optimally prepared graft copolymer, sodium salt of partially carboxymethylated sodium alginate-g-polyacrylonitrile (%G = 316.53), has been hydrolyzed in an alkaline medium (0.7N NaOH, 90-95 °C for ~2.5 h) to obtain the superabsorbent hydrogel, H-Na-PCMSA-g-PAN. The chemical structure, thermal characteristics, and morphology of the products have also been studied.

Sterols are the main components of the fungal membrane. Their study can be used to describe the chemical biodiversity among the strains and species or to work on antifungal treatment. Those molecules can be analyzed by gas chromatography coupled with mass spectrometry (GC-MS) as free molecules or after derivation as acetate or trimethylsilyl ether (TMSi). Here we describe how to extract sterols from fungal biomass according to its physiological form and the culture conditions (liquid and solid media). The different methodologies that can be used to obtain free sterols, acetate, and/or TMSi derivatives are presented. Identification keys using the fragmentation at 70 eV are also described., (© 2023. The Author(s), under exclusive license to Springer Science+Business Media, LLC, part of Springer Nature.)

Background: Saponification contributed to an increase in the in vitro antioxidant activity of astaxanthin (Asta) extracts derived from Penaeus sinensis (Solenocera crassicornis) by-products. However, the influence of non-saponification (N-Asta) and saponification Asta (S-Asta) absorption on antioxidant activity in vivo was limited. The antioxidant properties of N-Asta and S-Asta were therefore compared in Sprague Dawley male rats after 6 h and 12 of absorption using biochemistry assays combined with an untargeted metabonomics strategy., Results: Non-saponified Asta and S-Asta showed similar digestive properties in a stimulated gastrointestinal tract. Increased glutathione content and decreased malondialdehyde content were measured in the liver tissues of N-Asta and S-Asta treated rats after 12 h of absorption. Absorption of N-Asta increased liver total superoxide dismutase, glutathione peroxidase, and catalase activity. Treatment with S-Asta up-regulated NAD(P)H: quinine oxidoreductase-1, and heme oxygenase-1 expression was associated with the nuclear erythroid 2-related factor 2/antioxidant responsive element pathway at the end of 12 h absorption. With partial least square-discriminant analysis and metabolite heatmap profiles, the S-Asta group was clearly separated from the N-Asta group. The S-Asta treatment also demonstrated stronger influences on plasma metabolites than the N-Asta treatment. Both N-Asta and S-Asta absorption showed critical roles in the regulation of specific metabolites, and 15 potential biomarkers were identified in eight key pathways to separate these experimental groups after 12 h of absorption. However, an increased serotonin level was only detected in the S-Asta group after 12 h absorption., Conclusion: Absorption of N-Asta and S-Asta induced different antioxidant effects in normal rats, which were associated with metabolite changes. © 2022 Society of Chemical Industry., (© 2022 Society of Chemical Industry.)

Spent coffee ground (SCG) oil is an ideal substrate for the biosynthesis of polyhydroxyalkanoates (PHAs) by Cupriavidus necator. The immiscibility of lipids with water limits their bioavailability, but this can be resolved by saponifying the oil with potassium hydroxide to form water-soluble fatty acid potassium salts and glycerol. Total saponification was achieved with 0.5 mol/L of KOH at 50 °C for 90 min. The relationship between the initial carbon substrate concentration (C 0 ) and the specific growth rate (µ) of C. necator DSM 545 was evaluated in shake flask cultivations; crude and saponified SCG oils were supplied at matching initial carbon concentrations (C 0  = 2.9-23.0 g/L). The Han-Levenspiel model provided the closest fit to the experimental data and accurately described complete growth inhibition at 32.9 g/L (C 0  = 19.1 g/L) saponified SCG oil. Peak µ-values of 0.139 h -1 and 0.145 h -1 were obtained with 11.99 g/L crude and 17.40 g/L saponified SCG oil, respectively. Further improvement to biomass production was achieved by mixing the crude and saponified substrates together in a carbon ratio of 75:25% (w/w), respectively. In bioreactors, C. necator initially grew faster on the mixed substrates (µ = 0.35 h -1 ) than on the crude SCG oil (µ = 0.23 h -1 ). After harvesting, cells grown on crude SCG oil obtained a total biomass concentration of 7.8 g/L and contained 77.8% (w/w) PHA, whereas cells grown on the mixed substrates produced 8.5 g/L of total biomass and accumulated 84.4% (w/w) of PHA. KEY POINTS: • The bioavailability of plant oil substrates can be improved via saponification. • Cell growth and inhibition were accurately described by the Han-Levenpsiel model. • Mixing crude and saponified oils enable variation of free fatty acid content., (© 2022. The Author(s).)

Polychlorinated naphthalenes (PCNs) are emerging organic pollutants that are harmful to the environment and human health. In this study, a headspace solid-phase-microextraction (HS-SPME)-gas chromatography-tandem mass spectrometry method for the separation and enrichment of PCNs in shrimp was developed and validated. A graphene aerogel was prepared by modifying graphene oxide with a deep eutectic solvent to prevent graphene oxide stacking. As a result, the aerogel had a three-dimensional porous structure, which resulted in easy sorption/desorption for PCNs, and was used as the SPME fiber coating. Next, the experimental parameters for the saponification of the sample matrix and the extraction and desorption of the PCNs were systematically optimized. After optimization, the method showed good linearity (R 2 ≥0.9968), low limits of detection (0.00983-0.0661 pg g -1 ), and satisfactory recoveries (80.4-108%). Crucially, compared with previously reported methods, this method does not require the use of large amounts of organic reagents or complex operations, giving it the advantages of simplicity, sensitivity, and environmental friendliness. As an example of the practical application of the developed method, the PCNs in river and sea shrimp were quantified., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2022 Elsevier B.V. All rights reserved.)

Supplementing long-chain omega-3 polyunsaturated fatty acids (n3-PUFA) improves health. We characterized the pattern of total and non-esterified oxylipins and fatty acids in n3 supplements made of fish, krill, or micro-algae oil by LC-MS. All supplements contained the declared amount of eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA); however, their content per capsule and the concentration of other fatty acids varied strongly. Krill oil contained the highest total n3 oxylipin concentration (6000 nmol/g) and the highest degree of oxidation (EPA 0.7%; DHA 1.3%), while micro-algae oil ( Schizochytrium sp.) showed the lowest oxidation (<0.09%). These oils contain specifically high amounts of the terminal hydroxylation product of EPA (20-HEPE, 300 nmol/g) and DHA (22-HDHA, 200 nmol/g), which can serve as an authenticity marker for micro-algae oil. Refined micro-algae and fish oil were characterized by NEFA levels of ≤0.1%. Overall, the oxylipin and fatty acid pattern allows gaining new insights into the origin and quality of n3-PUFA oils in supplements.

Marigold flower petals are considered the richest source of lutein which possesses immense applications in the food and health sector. The study was undertaken to improve the stability of sunflower oil by enriching it with lutein extracted from marigold flower petals using safe and green technology. The extraction of lutein was optimized using Box-Behnken design by ultrasound-assisted extraction (UAE) employing sunflower oil as a solvent. The impact of three independent variables i.e., ultrasonic intensity, solid to solvent ratio, and extraction time were evaluated on the amount of lutein extracted and its antioxidant activity. Highest amount of lutein (21.23 mg/g) was extracted by employing ultrasonic intensity of 70 W/m2, extraction time of 12.5 min, and solid to solvent ratio of 15.75%. FT-IR spectra of lutein extracted by ultrasound and conventional extraction show similar peaks depicting that ultrasound does not have any impact on the functionality of lutein. Sunflower oil incorporated with lutein at 1000 PPM and the synthetic antioxidant (TBHQ) showed good oxidative stability than oil with 500 PPM lutein and no lutein during accelerated storage for a month. The oxidative stability was shown by different oil samples in the following order: TBHQ = 1000PPM lutein˃500PPM lutein ˃control oil. It was concluded that the ultrasound technique extracts lutein efficiently from marigold flowers and this lutein was effective in improving the oxidative stability of sunflower oil under accelerated storage conditions., (Copyright © 2022 The Author(s). Published by Elsevier B.V. All rights reserved.)

Hypothesis: Surfactants in emulsions sometimes do not provide adequate stability against coalescence, whereas Pickering emulsions often offer greater stability. In a search for stabilizers offering biocompatibility, we hypothesized that carboxylated nanodiamonds (ND) would impart stability to Pickering emulsions., Experiments: We successfully prepared Pickering emulsions of sunflower oil in water via two different methods: membrane emulsification and probe sonication. The first method was only possible when the pH of the aqueous ND suspension was ≤ 4., Findings: Pendant-drop tensiometry confirmed that carboxylated ND is adsorbed at the oil/water interface, with a greater decrease in interfacial tension found with increasing ND concentrations in the aqueous phase. The carboxylated ND become more hydrophilic with increasing pH, according to three-phase contact angle analysis, because of deprotonation of the carboxylic acid groups. Membrane emulsification yielded larger (about 30 µm) oil droplets, probe sonication produced smaller (sub-μm) oil droplets. The Pickering emulsions show high stability against mechanical vibration and long-term storage for one year. They remain stable against coalescence across a wide range of pH values. Sonicated emulsions show stability against creaming. In this first-ever systematic study of carboxylated ND-stabilized Pickering emulsions, we demonstrate a promising application in the delivery of β-carotene, as a model active ingredient., Competing Interests: Declaration of Competing Interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2021 Elsevier Inc. All rights reserved.)

Squalene is a precursor of steroids with diverse bioactivities. Tea was previously found to contain squalene, but its variation between tea cultivars remains unknown. In this study, tea leaf squalene sample preparation was optimized and the squalene variation among 30 tea cultivars was investigated. It shows that squalene in the unsaponified tea leaf extracts was well separated on gas chromatography profile. Saponification led to a partial loss of squalene in tea leaf extract and so it is not an essential step for preparing squalene samples from tea leaves. The tea leaf squalene content increased with the maturity of tea leaf and the old leaves grown in the previous year had the highest level of squalene among the tested samples. The squalene levels in the old leaves of the 30 tested cultivars differentiated greatly, ranging from 0.289 to 3.682 mg/g, in which cultivar "Pingyun" had the highest level of squalene. The old tea leaves and pruned littering, which are not used in tea production, are an alternative source for natural squalene extraction., Competing Interests: The authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest. The reviewer LR declared a shared affiliation, though no other collaboration, with the authors to the handling editor., (Copyright © 2022 Sheng, Xiang, Wang, Li, Li, Lu, Ye, Liang and Zheng.)

Little is known about the influence of the saturation degree of long chain fatty acids (LCFAs) on the bio-methane potential of calcium-LCFAs salts. In this study, palmitic acid and oleic acid were chosen as the model compounds to investigate the impact of saponification between calcium and saturated/unsaturated LCFAs on the methane recovery from LCFAs in anaerobic digestion. A 2.2-fold enhancement of methane yield was obtained due to the formation of calcium palmitate, which was primarily attributed to the enhanced bio-aggregation and significant change of microbial community. However, saponification between calcium and oleic acid decreased the methane recovery from oleic acid digestion. Only partial saponification with excess oleic acid led to 4% increment of methane production. The low bio-accessibility of calcium oleate and the little change of microbial community may be responsible for the small difference of methane recovery due to the formation of calcium oleate., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

Carotenoid pigments serve many endogenous functions in organisms, but some of the more fascinating are the external displays of carotenoids in the colorful red, orange and yellow plumages of birds. Since Darwin, biologists have been curious about the selective advantages (e.g., mate attraction) of having such ornate features, and, more recently, advances in biochemical methods have permitted researchers to explore the composition and characteristics of carotenoid pigments in feathers. Here we review contemporary methods for extracting and analyzing carotenoids in bird feathers, with special attention to the difficulties of removal from the feather keratin matrix, the possibility of feather carotenoid esterification and the strengths and challenges of different analytical methods like high-performance liquid chromatography and Raman spectroscopy. We also add an experimental test of current common extraction methods (e.g., mechanical, thermochemical) and find significant differences in the recovery of specific classes of carotenoids, suggesting that no single approach is best for all pigment or feather types., (Copyright © 2022 Elsevier Inc. All rights reserved.)

This study compared different extraction methods [sonication, alkaline hydrolysis, supramolecular solvent microextraction (SUPRAS) and Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS)] along with their greenness. An analytical method was validated for determination of USEPA's listed 16 polycyclic aromatic hydrocarbons' (PAHs) in cooked chicken and roasted coffee using high pressure liquid chromatography-fluorescence detector (HPLC-FLD) with a C18 column. The recoveries with QuEChERS ranged between 62.26 and 103.85% (except Naphthalene and Fluorene) and 52.63-78.69% (except Naphthalene) for chicken and coffee respectively while poor recoveries were observed with conventional methods. With SUPRAS, heavy PAHs' recovery in chicken was 71.33-112.23%. Limits of detection (LOD) were 0.03-0.06 ng/mL, regression coefficient values were 0.97-0.99 for 6.25-37.50 ng/mL quantification range. Relative standard deviation was found to be below 22%. The time and energy consumption per sample was 42.50 and 69.06 fold and 77.52 and 139.50 fold less with SUPRAS and QuEChERS method respectively as compared to alkaline hydrolysis., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

Analysis of fatty acids (FA) in food and biological samples such as blood is indispensable in modern life sciences. We developed a rapid, sensitive and comprehensive method for the quantification of 41 saturated and unsaturated fatty acids by means of LC-MS. Optimized chromatographic separation of isobaric analytes was carried out on a C8 reversed phase analytical column (100 × 2.1 mm, 2.6 μm core-shell particle) with a total run time of 15 min with back pressure lower than 300 bar. On an old triple quadrupole instrument (3200, AB Sciex), pseudo selected reaction monitoring mode was used for quantification of the poorly fragmenting FA, yielding limits of detection of 5-100 nM. Sample preparation was carried out by removal of phospholipids and triglycerides by solid-phase extraction (non-esterified fatty acids in oils) or saponification in iso-propanol (fatty acyls). This is not only a rapid strategy for quantification of fatty acyls, but allows the direct combination with the LC-MS-based analysis of fatty acid oxidation products (eicosanoids and other oxylipins) from the same sample. The concentrations of fatty acyls determined by means of LC-MS were consistent with those from GC-FID analysis demonstrating the accuracy of the developed method. Moreover, the method shows high precisions with a low intra-day (≤ 10% for almost all fatty acids in plasma and ≤ 15% in oils) and inter-day as well as inter-operator variability (< 20%). The method was successfully applied on human plasma and edible oils. The possibility to quantify non-esterified fatty acids in samples containing an excess of triacylglycerols and phospholipids is a major strength of the described approach allowing to gain new insights in the composition of biological samples., (© 2021. The Author(s).)

The effect of fat saponification and the inclusion or exclusion of blood in slaughterhouse mixtures were assessed in terms of anaerobic digestion performance. Mixtures of animal by-products (ABP) were collected for 1 year, whereby following the daily activity and waste generation at a slaughterhouse facility, seasonal fluctuations were found. The blood content of ABP mixtures was variable, affecting both the methane yield and the production rate (287.8-320.5 NL CH4 kg COD -1 and 80.3-94.7 and NL CH4 kg COD , respectively). The saponification of fatty ABP materials was studied to assess the methane production rate, singularly or combined, with and without the addition of blood. Data showed that saponification significantly reduced the lag phase, from 2.2 to 1.5 days in winter mixtures and from 1.5 to 0.9 days in summer mixtures (all with blood), and from 0.3 to 0.1 days in summer mixtures without blood. Finally, the percentage of energy demand at the slaughterhouse potentially covered by net biogas energy was estimated, finding that the facility could be 100% energy self-sufficient in winter, whereas this would be reduced to 85% in the summer due to different methane yields of ABP mixtures based on season.-1 d -1 , respectively). The saponification of fatty ABP materials was studied to assess the methane production rate, singularly or combined, with and without the addition of blood. Data showed that saponification significantly reduced the lag phase, from 2.2 to 1.5 days in winter mixtures and from 1.5 to 0.9 days in summer mixtures (all with blood), and from 0.3 to 0.1 days in summer mixtures without blood. Finally, the percentage of energy demand at the slaughterhouse potentially covered by net biogas energy was estimated, finding that the facility could be 100% energy self-sufficient in winter, whereas this would be reduced to 85% in the summer due to different methane yields of ABP mixtures based on season., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

The use of mono-substituted malonic acid half oxyesters (SMAHOs) has been hampered by the sporadic references describing their preparation. An evaluation of different approaches has been achieved, allowing to define the best strategies to introduce diversity on both the malonic position and the ester function. A classical alkylation step of a malonate by an alkyl halide followed by a monosaponification gave access to reagents bearing different substituents at the malonic position, including functionalized derivatives. On the other hand, the development of a monoesterification step of a substituted malonic acid derivative proved to be the best entry for diversity at the ester function, rather than the use of an intermediate Meldrum acid. Both these transformations are characterized by their simplicity and efficiency, allowing a straightforward access to SMAHOs from cheap starting materials., (Copyright © 2021, Xavier et al.)

Two liquid chromatographic systems, one coupled to atmospheric pressure chemical ionization and tandem mass spectrometric methods (UHPLC-APCI-MS/MS) and the other a high-performance liquid chromatographic coupled to diode array detector (HPLC-DAD) were used to develop and validate methods for the simultaneous determination of fat-soluble vitamins A, D3 and E in rice cereal baby foods. The chromatographic separation was performed on C18 columns with a mixture of methanol-acetonitrile as mobile phase for all methods. The extraction of fat-soluble vitamins included enzymatic hydrolysis with α-amylase, saponification, extraction with petroleum ether or n-hexane and purification with silica cartridge (only for vitamin D3). Quantification of vitamin D3 and E through UHPLC-APCI-MS/MS was performed by the use of internal standards (IS) D3-d3 and E-d6, respectively, while IS was not used for vitamin A. The methods were optimized and validated in terms of linearity, precision, trueness, limits of detection and quantification. The recoveries were in the range of 85.0-107% for retinol, 92.0-105% for α-tocopherol and 95.2-106% for cholecalciferol and the %RSD (Relative Standard Deviation) values ranged from 6.4% to 15%. The evaluation of the methods was also conducted through the estimation of uncertainties, the application in commercial samples and the participation in a proficiency test.

Sterol analysis of complex matrices can be very laborious. To minimize the existing drawbacks, a new micro-method of sterols and squalene determination in cyanobacteria was developed and applied to monitor their production of Phormidium autumnale cultured heterotrophically. Sample extraction/saponification and GC analysis of the target compounds were optimized separately using Plackett-Burman design (PB) followed by a central composite rotational design (CCRD). The most influential variables were identified to maximize compound recovery. Chloroform presented the highest capability to extract all target compounds with a horizontal shaker table (HST) for homogenization in the saponification step. For the pretreatment, a small amount of chloroform was used for 90 min at 50 °C and 6 min for the saponification time. The sample introduction in the GC injector was studied by evaluating pressure and injector temperature. High response for sterols and squalene were obtained between 19 and 23 psi and at 310 °C of injection temperature. The new method was able to determine different sterol concentrations: 0.2-0.6 mg kg -1 of squalene, 5-18 mg kg -1 of stigmasterol, 6 mg kg -1 of cholesterol, and 3 mg kg -1 of β-sitosterol, showing high analytical performance and fulfilling all steps, thus proving to be a promising technique., (Copyright © 2020 Elsevier B.V. All rights reserved.)

Total sterol content and composition in plant tissues can be easily determined by gas chromatography (GC) after saponification of the total lipid extract. However, in oleogenic tissues a significant proportion of the sterol is esterified to fatty acids, with GC methodologies unable to provide information about the proportion and the molecular species composition of intact steryl esters (SEs). Here we describe an electrospray ionization-tandem mass spectrometry (ESI-MS/MS) and Multiple Reaction Monitoring (MRM) method which, in parallel with GC analysis, allows for the accurate determination of both free and esterified sterol content and composition in seeds. After extraction of seed oil with hexane, free sterols are derivatized with undecanoyl chloride, total steryl esters are then purified from triacylglycerol (TAG) by liquid chromatography, infused and ionized as ammonium adducts, with molecular species identified and quantified by fragmentation in the presence of internal standards.

Poly(dimethylsiloxane) (PDMS) has been extensively used as an electroactive polymer material because it exhibits not only excellent moldability but also mechanical properties sufficient enough for electroactive performance despite low dielectric permittivity. Its low dielectric property is due to its molecular non-polarity. Here, we introduce a polar group into a PDMS elastomer by using vinyl acetate (VAc) as a crosslinker to improve the dielectric permittivity. We synthesized a high-molecular weight PDMS copolymer containing vinyl groups, namely poly(dimethylsiloxane- co -methylvinylsiloxane) (VPDMS), and prepared several of the VPDMS solutions in VAc. We obtained transparent PDMS films by UV curing of the solution layers. Electromechanical actuation-related physical properties of one of the UV-cured films were almost equivalent to or superior to those of platinum-catalyzed hydrosilylation-cured PDMS films. In addition, saponification of the UV-cured film significantly improved the electrical and mechanical properties (ɛ' ~ 44.1 pF/m at 10 kHz, E ~ 350 kPa, ɛ ~ 320%). The chemical introduction of VAc into PDMS main chains followed by saponification would offer an efficacious method of enhancing the electroactive properties of PDMS elastomers.

Objective: This study aimed at determining the existence of oils and fats in ghee manufactured in Bangladesh and to validate the nature of the impurity., Materials and Methods: In this study, a ghee sample was prepared in the laboratory by following standard methods and was used as a control sample. On the other hand, 19 ghee samples, including five branded samples (B1-B5), and 14 local samples (L1-L14) were collected from different manufacturers. The ghee samples were assessed for fat composition, Reichert Meissl (RM), saponification, Polenske, acid, Kirschner, and butyro refractometer (BR) values. To validate the ghee samples, vegetable oils and body fats were mixed in different ratios and then analyzed., Results: All the branded samples contained more than 99.5% fat, but only three local samples showed more than 97% fat. Admixing of soybean oil and coconut oil in different ratios showed the RM value from 1.57 ± 0.09 to 4.14 ± 0.21, whereas incorporation of hydrogenated vegetable oils and tallow showed 6.36 ± 0.03 to 14.10 ± 0.14. Nine local samples revealed RM values similar to external fat admixed samples. B2, B4, B5, L2-L8, and L10-L14 samples' saponification values differed from the standard limits. Polenske, acid, Kirschner values and BR reading for L4, L6, L7, L8, L10, L12, L13, and L14 showed the worst results. All values varied significantly ( p < 0.01)., Conclusion: Local samples, L4, L6, L7, L8, L10, L12, L13, and L14, were assumed to be adulterated with external oils and fats. The quality of local ghee is questionable, as the samples contained more than 8% moisture, whereas pure ghee had less than 0.5% moisture., Competing Interests: The authors declare there is no conflict of interests related to any matter of this research article., (Copyright: © Journal of Advanced Veterinary and Animal Research.)

This work deals with up-to-date optimization of cholesterol content determination when saponification and extraction procedures as well as HPLC conditions were studied. As found, optimal conditions for saponification process were identified by 15 min heating in the presence of 0.015 L of methanolic KOH solution with a concentration 1 mol/L with subsequent 0.015 L n-hexane-chloroform binary mixture (1:1, v / v ) double extraction. HPLC separation consisted of isocratic elution with flow rate of 0.5 mL/min mobile phase composed of acetonitrile/methanol 60:40 ( v / v ) and stationary phase Zorbax Eclipse Plus C18 column 2.1 × 100 mm, 3.5 μm particle size diameters with detector wavelength 205 nm. The method passed through in-house validation criteria and its suitability was verified by analysis of butter reference materials. In final, the average content of cholesterol content in butter was determined at 2271.0 mg/kg. Thus, the method is suitable for the determination of cholesterol content in butter and probably also in other dairy products.

Dunaliella salina is well-known for its high content in carotenoids and glycerol. Nevertheless, Dunaliella salina has also a high content in lipids, including polar lipids, which are suitable for nutraceutical/cosmeceutical applications. This work proposes a sustainable process to maximise the potential of Dunaliella salina for the production of distinct fractions of carotenoids, glycerol, polar lipids and proteins, which may contribute to improve the revenues of the microalgae industry. In this work, extraction with non-hazardous solvents and organic solvent nanofiltration are integrated, in order to obtain added-value products and glycerol. Also, aiming to separate carotenoids from glycerides, a saponification process is proposed. High overall recoveries were obtained for carotenoids (85%), glycerol (86%), polar lipids (94%) and proteins (95%). In order to evaluate the profitability of the proposed biorefinery, an economic assessment was accomplished. Both CAPEX and OPEX (Capital and Operating expenditure) were calculated, likewise the Return of Investment (ROI)., (Copyright © 2019 Elsevier Ltd. All rights reserved.)

Haematococcus pluvialis is the richest biological source of astaxanthin under unfavorable growing conditions. Many reports have discussed the optimal astaxanthin extraction methods. Free-astaxanthin could be still hindered by microalgae extracts composition or by prolonged extraction times. In this study we evaluated the effect of enzymolysis and saponification deesterification processes of astaxanthin and its carotenoid precursors under high irradiance and nitrogen deprivation stress time conditions. Results showed that cholesterol esterase facilitated astaxanthin deesterification (975.65 μg mg -1 DW) while saponification positively affected zeaxanthin (1038.68 μg mg -1 DW).

A method for the direct preparation of fatty-acid methyl esters (FAME) was simplified for fatty-acid analysis of a single fish larva using gas chromatography (GC). The method included the isolation of a larval trunk and drying in a glass vial, followed by saponification of all the contents without prior lipid extraction. Thereafter, the fatty acids released were methylated by trimethylsilyldiazomethane. This method has advantages over another method, direct acid-catalyzed transesterification, because both the saponification and methylation at room temperature can reduce loss of unsaturated fatty acids and formation of artifacts unavoidable in acidic reaction at high temperature. GC of the products showed that the simplified method can yield methyl esters without artifacts interfering analysis. More than 50 fatty acids were determined, which are twice as many as those previously analyzed using high-performance liquid chromatography. Observation of consistent small impurities in GC of blank tests allowed the accurate determination of fatty acids by correcting the peak areas. Dry matter weights (<3 mg) and the total fatty-acid contents displayed a linear relationship. Fatty-acid analysis of wild larvae of bluefin tuna, yellowfin tuna, and skipjack tuna collected from the waters around Japan (n = 100) revealed that the eicosapentaenoic acid (EPA) level in bluefin tuna collected from the Japan Sea was significantly higher than that in the three species collected from Nansei Islands. The simplified direct saponification/methylation method will be a powerful tool for investigating growth and survival of individual larval tuna and other fish species., (© 2018 AOCS.)

Microalgae are an interesting source of natural pigments that have valuable applications. However, further research is necessary to develop processes that allow us to achieve high levels of carotenoid recovery while avoiding degradation. This work presents a comprehensive study on the recovery of carotenoids from several microalgae genera, optimizing carotenoid extraction using alkaline saponification at various temperatures and KOH concentrations. Results show that I. galbana requires a temperature of 60 °C and <10% KOH, N. gaditana and K. veneficum require 60 °C and no saponification, P. reticulatum requires 40 °C and 10% KOH, T. suecica and H. pluvialis require 25 °C and 40% KOH while C. sp. and S. almeriensis require 80 °C and 40% KOH. The influence of the solvent on carotenoid recovery was also studied. In general terms, an ethanol:hexane:water (77:17:6 v/v/v) mixture results in good yields., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

Here, a new bioprinting process by combining drop-on-demand inkjet printing with a spray-coating technique, which enables the high-resolution, high-speed, and freeform fabrication of large-scale cell-laden hydrogel structures is reported. Hydrogel structures with various shapes and composed of different materials, including alginate, cellulose nanofiber, and fibrinogen, are fabricated using the inkjet-spray printing. To manufacture cell-friendly hydrogel structures with controllable stiffness, gelatine methacryloyl is saponified to stabilize jet formation and is subsequently mixed with sodium alginate to prepare blend inks. The hydrogels crosslinked from the blend inks are characterized by assessing physical properties including the microstructure and mechanical stiffness and cellular responses including the cell viability, metabolic activity, and functionality of human dermal fibroblasts within the hydrogel. Cell-laden hydrogel structures are generated on a large scale and collagen type I secretion and spreading of cells within the hydrogels are assessed. The results demonstrate that the inkjet-spray printing system will ensure the formation of a cell-laden hydrogel structure with high shape fidelity in a rapid and reliable manner. Ultimately, the proposed printing technique and the blend bioink to be used to fabricate 3D laminated large-scale tissue equivalents that potentially mimic the function of native tissues is expected., (© 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

We propose a method for the simultaneous determination of 15 kinds of polycyclic aromatic hydrocarbons in marine samples (muscle) employing gas chromatography with mass spectrometry after saponification with ultrasound-assisted extraction and solid-phase extraction. The experimental conditions were optimized by the response surface method. In addition, the effects of different lyes and extractants on polycyclic aromatic hydrocarbons extraction were discussed, and saturated sodium carbonate was first used as the primary saponification reaction and extracted with 10 mL of ethyl acetate and secondly 1 mol/L of sodium hydroxide and 10 mL of n-hexane were used to achieve better results. The average recovery was 67-112%. Satisfactory data showed that the method has good reproducibility with a relative standard deviation of <13%. The detection limits of polycyclic aromatic hydrocarbons were 0.02-0.13 ng/g. Compared with other methods, this method has the advantages of simple pretreatment, low solvent consumption, maximum polycyclic aromatic hydrocarbons extraction, the fast separation speed, and the high extraction efficiency. It is concluded that this method meets the batch processing requirements of the sample and can also be used to determine polycyclic aromatic hydrocarbons in other high-fat (fish, shrimp, crab, shellfish) biological samples., (© 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

Phytoprostanes (PhytoPs) and phytofurans (PhytoFs) are prostaglandin-like compounds, contributing to defense signaling and prevention of cellular damage. These plant oxylipins result from autoxidation of α-linolenic acid (ALA) and have been proposed as new bioactive compounds due to their structural analogies with isoprostanes (IsoPs) and prostanoids derived from arachidonic acid in mammals, which have demonstrated diverse biological activities. The present work assesses a wide range of vegetable oils - including extra virgin olive oils (n = 7) and flax, sesame, argan, safflower seed, grapeseed, and palm oils - for their content of PhytoPs and PhytoFs. Flax oil displayed the highest concentrations, being notable the presence of 9-epi-9-D 1t -PhytoP, 9-D 1t -PhytoP, 16-B 1 -PhytoP, and 9-L 1 -PhytoP (7.54, 28.09, 28.67, and 19.22 μg mL -1 , respectively), which contributed to a total PhytoPs concentration of 119.15 μg mL -1 , and of ent-16-(RS)-9-epi-ST-Δ 14 -10-PhytoF (21.46 μg mL -1 ). Palm and grapeseed oils appeared as the most appropriate negative controls, given the near absence of PhytoPs and PhytoFs (lower than 0.15 μg mL -1 ). These data inform on the chance to develop nutritional trials using flax and grapeseed oils as food matrices that would provide practical information to design further assays intended to determine the actual bioavailability/bioactivity in vivo., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

In this work, the molybdenum disulfide/reduced graphene oxide (MoS 2 /RGO) composite material was synthesized as a fiber coating to extract seven indicator polychlorinated biphenyls (PCBs; PCB28, PCB52, PCB101, PCB118, PCB138, PCB153, and PCB180) present in food via a saponification-headspace solid-phase microextraction assay (saponification-HS-SPME). The MoS 2 /RGO coating was prepared and deposited on a stainless steel wire with the help of a silicone sealant and used as an SPME fiber. The alkali solution dissolved the fat and helped in releasing the PCBs present in milk to the headspace for extraction under 100°C. Following desorption in the inlet, the targets were quantified by gas chromatography-mass spectrometry. The effects of sorbent dosage, extraction time, added salts, and stirring rate on the extraction efficiency were investigated. The new coating was able to adsorb a higher amount of analytes, which was about 1.1-2.9 times in comparison with the commercially available SPME fiber (coated with divinylbenzene/carboxen/polydimethylsiloxane). It also showed the highest adsorption capability toward PCBs, which was 1.5-2.7 times that of the prepared RGO modified fiber. Moreover, MoS 2 also showed a strong affinity toward PCBs in a manner similar to its affinity for graphene. The developed method is simple and environmentally friendly as it does not require any organic solvents. Furthermore, it exhibits good sensitivity with detection limits less than 0.1ngmL -1 , linearity (0.25-100ngmL -1 ), and reproducibility (relative standard deviation below 10% for n=3). The novel SPME fibers are inexpensive, reusable, and can be easily prepared and manipulated. In addition, the saponification-HS-SPME assay was also found to be suitable for screening persistent organic pollutants in dairy products., (Copyright © 2017 Elsevier B.V. All rights reserved.)

Lutein is a commercial carotenoid with potential health benefits. Microalgae are alternative sources for the lutein production in comparison to conventional approaches using marigold flowers. In this study, a process analysis of a single-step simultaneous extraction, saponification, and primary purification process for free lutein production from wet microalgae biomass was carried out. The feasibility of binary solvent mixtures for wet biomass extraction was successfully demonstrated, and the extraction kinetics of lutein from chloroplast in microalgae were first evaluated. The effects of types of organic solvent, solvent polarity, cell disruption method, and alkali and solvent usage on lutein yields were examined. A mathematical model based on Fick's second law of diffusion was applied to model the experimental data. The mass transfer coefficients were used to estimate the extraction rates. The extraction rate was found more significantly related with alkali ratio to solvent than to biomass. The best conditions for extraction efficiency were found to be pre-treatment with ultrasonication at 0.5 s working cycle per second, react 0.5 h in 0.27 L/g solvent to biomass ratio, and 1:3 ether/ethanol (v/v) with 1.25 g KOH/L. The entire process can be controlled within 1 h and yield over 8 mg/g lutein, which is more economical for scale-up.

Objective: The aim of this study was to develop a test method to evaluate the preservation efficacy for a specific product, a very high-alkaline liquid soap (pH around 10) made by a saponification process. Several manufacturers have experienced contamination issues with these high-pH soaps despite passing a classic preservative efficacy challenge test or even a multi-inoculation challenge test., Methods: Bacteria were isolated from contaminated soaps and were identified using 16S rRNA gene sequencing. High-alkaline-pH unpreserved soaps were tested using the Thor Personal Care internal multichallenge test method (TM206) with classical microorganisms and then with the bacterial strains isolated from various contaminated soaps (TM768). Preservatives were added to these soaps and assessed for their efficacy using the newly developed test., Results: Four different species of bacteria (Nesterenkonia lacusekhoensis, Dermacoccus sp., Halomonas sp. and Roseomonas sp.) were identified by sequencing among the contaminants of the various soaps tested. Among these, only one bacterial species, Nesterenkonia lacusekhoensis, appeared to be responsible for the specific contamination of these high-alkaline soaps. Thus, one specific wild-type strain of Nesterenkonia lacusekhoensis, named as strain 768, was used in a new multi-inoculation test (TM768). Unlike the single inoculation challenge test, the multi-inoculation test using the Nesterenkonia strain 768 was able to predict the sensitivity of a product towards this bacterium. Among the 27 different preservatives tested, 10 were able to protect the formula against contamination with this bacterium., Conclusion: This study enabled the development of a test method to evaluate the efficacy of preservation using a specific bacterium, Nesterenkonia lacusekhoensis, responsible for the contamination of very alkaline soaps made by saponification and identify an appropriate preservative system., (© 2017 Society of Cosmetic Scientists and the Société Française de Cosmétologie.)

Microalgae have the potential to synthesize and accumulate lipids which contain high value fatty acids intended for nutrition and biodiesel applications. Nevertheless, lipid extraction methods for microalgae cells are not well established and there is not a standard analytical methodology to extract fatty acids from lipid-producing microalgae. In this paper, current lipid extraction procedures employing organic solvents (chloroform/methanol, 2:1 and 1:2, v/v), sodium hypochlorite solution (NaClO), acid-catalysed hot-water extraction and the saponification process [2.5 M KOH/methanol (1:4, v/v)] have been evaluated with two species of microalgae with different types of cell walls. One is a marine diatom, Phaeodactylum tricornutum, and the other a freshwater green microalga, Haematococcus pluvialis. Lipids from all types of extracts were estimated gravimetrically and their fatty acids were quantified by a HPLC equipped with Q-TOF mass spectrometer. Results indicated significant differences both in lipids yield and fatty acids composition. The chloroform and methanol mixture was the most effective extraction solvent for the unsaturated fatty acids such as DPA (C22:05), DHA, (C22:06), EPA (C20:05) and ARA (C20:04). While acid treatments improved the saturated fatty acids (SFAs) yield, especially the short chain SFA, lauric acid (C12:0), whose amount was 64% higher in P. tricornutum and 156% higher in H. pluvialis compared to organic solvent extractions. Graphical abstract ᅟ.

For the analysis of edible oils, saponification is well known as a useful method for eliminating oil matrices. The conventional approach is conducted with alcoholic alkali; it consumes a large volume of organic solvents and impedes the retrieval of analytes by microextraction. In this study, a low-organic-solvent-consuming method has been developed for the analysis of benzo[a]pyrene in edible oils by high-performance liquid chromatography with fluorescence detection. Sample treatment involves aqueous alkaline saponification, assisted by a phase-transfer catalyst, and selective in situ extraction of the analyte with a supramolecular solvent. Comparison of the chromatograms of the oil extracts obtained by different microextraction methods showed that the supramolecular solvent has a better clean-up effect for the unsaponifiable matter from oil matrices. The method offered excellent linearity over a range of 0.03- 5.0 ng mL -1 (r > 0.999). Recovery rates varied from 94 to 102% (RSDs <5.0%). The detection limit and quantification limit were 0.06 and 0.19 μg kg -1 , respectively. The proposed method was applied for the analysis of 52 edible oils collected online in China; the analyte contents of 23 tested oil samples exceeded the maximum limit of 2 μg kg -1 for benzo[a]pyrene set by the Commission Regulation of the European Union., (© 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

During the excavation of the Spanish Civil War mass grave at La Pedraja (Burgos, Spain), 104 individuals were found interred within it, 45 of which displayed brains that were preserved but dehydrated and reduced in size. This exceptional finding has resulted in the formation of a multidisciplinary team, with the aim of obtaining as much information as possible and to primarily understand the taphonomic phenomena that has led to the preservation of these brains. The following types of analyses were undertaken on three of these brains: macroscopy, histology, radiology, chemical-toxicology, genetics, chemical analysis of the soil and 3D modelling for stereolithography. The historical context was considered, plus all archaeological and other forensic data provided by the investigation of the mass grave. The results of the analyses on these morphologically identifiable human brains confirmed the presence of nerve structures, fatty acids, and in one case ante-mortem evidence for an intracranial haemorrhage. The fatty acid profile corresponds to the process of saponification. Therefore, the interpretation is that the preservation of these brains at the mass grave of La Pedraja was due to the saponification process, which was influenced by the manner and cause of death, the chemical composition of the brain, the physicochemical properties of the soil and the meteorological conditions at the time., (Copyright © 2016 The Chartered Society of Forensic Sciences. Published by Elsevier Ireland Ltd. All rights reserved.)

Rose hip fruit, which contains high concentration of carotenoids is commonly used for different food products in Europe and it is considered to have medical properties. In this study, a simple, rapid and efficient HPLC-DAD-APCI(+)-MS method was developed and applied to identify and quantify the carotenoids in rose hip fruit of four rose species, including both unsaponified and saponified extract. In the unsaponified extract 23 carotenoid esters were detected, in which either rubixanthin ester or violaxanthin ester was the dominant component of the ester composition. In the saponified extract 21 carotenoids, including 11 xanthophylls and 10 carotenes were detected. This is the first time the total carotenoid composition, including the carotenoid esters in rose hip fruit were identified and quantified. This work reveals the potential of rose hip fruit to be utilized as a healthy dietary material and give chemical information for the possible future development in the pharmacology field., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

In vitro effects of acetylated pectin (OP) isolated from cacao pod husks (Theobroma cacao L.), its partially deacetylated and de-esterified form (MOP), and a commercial homogalacturonan (PG) were investigated on murine peritoneal macrophages. MOP stood out among the studied pectins. After 48h of incubation, compared with the control group, it was able to promote significant macrophage morphological differentiation from resident to activated stage and also stimulated nitric oxide production, which reached a level of 85% of that of LPS stimulus. In the presence of the highest tested concentration of MOP (200μg·mL -1 ), the levels of the cytokines TNF-α (6h) and IL-12 and IL-10 (48h) increased substantially in relation to untreated cells. Our results show that the partial deacetylation and de-esterification of pectin extracted from cacao pod husks (T. cacao L.) produced a polymer with greater ability than its native form to activate macrophages to a cytotoxic phenotype. Like this, they provide the possibility of a therapeutic application to MOP, which could lead to a decreased susceptibility to microbial infection besides antitumor activity. Additionally, the present results also corroborate with the proposition of that the chemical modifications of the biopolymers can result in an improved molecule with new possibilities of application., (Copyright © 2016 Elsevier B.V. All rights reserved.)

Microalgae oil is an optimal feedstock for nutraceutical, pharmaceutical and biodiesel production, but its high levels of chlorophyll limit its large-scale application. To date, few effective approaches have been developed to remove chlorophyll from microalgae oil. The main purpose of this study was to present a preprocessing method of algae oil feedstock (Scenedesmus) to remove chlorophyll by saponification. The results showed that 96% of chlorophyll in biomass was removed. High quality orange transparent oil could be extracted from the chlorophyll reduced biomass. Specifically, the proportion of neutral lipids and saturation levels of fatty acids increased, and the pigments composition became carotenoids-based. The critical parameters of chlorophyll reduced biodiesel conformed to the standards of the USA, China and EU. Sodium copper chlorophyllin could be prepared from the bleaching effluent. The results presented herein offer a useful pathway to improve the quality of microalgae oil and reduce the cost of microalgae biodiesel., Competing Interests: The authors declare that they have no competing interests.

Oil pulling is a traditional folk remedy practiced in ancient India. It is believed to cure more than thirty systemic diseases when practiced regularly and as directed. Due to occurrence of side effects to modern medicines and oral hygiene products, people are increasingly attracted towards complementary and traditional practices. Oil pulling in addition to offering several oral health benefits has also beneficial effects on overall health. The present article attempts to review and discuss this ancient practice.

Ergosterol, a molecule with high commercial value, is the most abundant mycosterol in Agaricus bisporus L. To replace common conventional extraction techniques (e.g. Soxhlet), the present study reports the optimal ultrasound-assisted extraction conditions for ergosterol. After preliminary tests, the results showed that solvents, time and ultrasound power altered the extraction efficiency. Using response surface methodology, models were developed to investigate the favourable experimental conditions that maximize the extraction efficiency. All statistical criteria demonstrated the validity of the proposed models. Overall, ultrasound-assisted extraction with ethanol at 375 W during 15 min proved to be as efficient as the Soxhlet extraction, yielding 671.5 ± 0.5mg ergosterol/100 g dw. However, with n-hexane extracts with higher purity (mg ergosterol/g extract) were obtained. Finally, it was proposed for the removal of the saponification step, which simplifies the extraction process and makes it more feasible for its industrial transference., (Copyright © 2015 Elsevier Ltd. All rights reserved.)