Investigation of ionic liquid adsorption and interfacial tension reduction using different crude oils; effects of salts, ionic liquid, and pH.

The results revealed the significant effect of NaCl, KCl, CaCl2, MgCl2, CaSO4, MgSO4, and Na2SO4 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 MgCl2 and CaCl2 led to a similar IFT variation trend for the case of distilled water/crude oil II. For the MgCl2 and CaCl2 solutions, a shifting point for IFT values was inevitable. Besides, the dissolution of 1-dodecyl-3-methyl imidazolium chloride ([C12mim][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 [C12mim][Cl] adsorption (under pH values) for crude oils using only Na2SO4 was measured and the minimum adsorption of 0.41 mg surfactant/g Rock under the light of saponification process was obtained.

Ionic liquids adsorption and interfacial tension reduction for synthetic resinous and asphaltenic oils: salinity and pH effects.

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 MgSO4, and Na2SO4 revealed an extensive IFT reduction for a pH value of 11 with the value of 0.20 mN/m for Na2SO4. 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 Na2SO4 + 500 ppm 1-decyl-3-methyl imidazolium triflate ([C10mim][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 ([C10mim][Cl]) and [C10mim][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.

Physicochemical characteristics of grease-trap wastewater with different potential mechanisms of FOG solid formation, separation, and accumulation inside grease traps.

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.

Alkali Polymer Flooding of a Romanian Field Containing Viscous Reactive Oil.

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.

A Novel Fabrication of Heterogeneous Saponified Poly(Vinyl Alcohol)/Pullulan Blend Film for Improved Wound Healing Application.

In this study, a novel film of poly(vinyl alcohol) (PVA)/pullulan (PULL) with improved surface characteristics was prepared from poly(vinyl acetate) (PVAc)/PULL blend films with various mass ratios after the saponification treatment in a heterogeneous medium. According to proton nuclear magnetic resonance (1H-NMR), Fourier transform infrared, and X-ray diffraction results, it was established that the successful fabrication of saponified PVA/PULL (100/0, 90/10, and 80/20) films could be obtained from PVAc/PULL (100/0, 90/10, and 80/20) films, respectively, after 72 h saponification at 50 °C. The degree of saponification calculated from 1H-NMR analysis results showed that fully saponified PVA was obtained from all studied films. Improved hydrophilic characteristics of the saponified films were revealed by a water contact angle test. Moreover, the saponified films showed improved mechanical behavior, and the micrographs of saponified films showed higher surface roughness than the unsaponified films. This kind of saponified film can be widely used for biomedical applications. Moreover, the reported saponified film dressing extended the lifespan of dressing as determined by its self-healing capacity and considerably advanced in vivo wound-healing development, which was attributed to its multifunctional characteristics, meaning that saponified film dressings are promising candidates for full-thickness skin wound healing.

[Optimization and application of determination method of cholesterol in various dishes].

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.

Serum calcium concentrations are inversely correlated with pancreatic lipase concentrations in dogs.

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.

Fungal Sterol Analyses by Gas Chromatography-Mass Spectrometry Using Different Derivatives.

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.

The synergistic effect of waste cooking oil and endod (Phytolacca dodecandra) on the production of high-grade laundry soap.

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.

Sodium Salt of Partially Carboxymethylated Sodium Alginate-g-Poly(acrylonitrile): I. Photo-Induced Synthesis, Characterization, and Alkaline Hydrolysis.

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.

Identification of carotenoids from fruits and vegetables with or without saponification and evaluation of their antioxidant activities.

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 ß-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.

Effective biosorption of As(V) from polluted water using Fe(III)-modified Pomelo (Citrus maxima) peel: A batch, column, and thermodynamic study.

Pomelo, Citrus maxima, peel was chemically modified with lime water and then loaded with Fe(III) to develop anion exchange sites for effective sequestration of As(V) from water. Biosorbent characterizations were done by using FTIR, SEM, XRD, EDX, and Boehm's titration. The batch biosorption studies were carried out at various pHs using modified and non-modified biosorbents and optimum biosorption of As(V) occurred at acidic pH (3.0-5.0) for both the biosorbents. A kinetic study showed a fast biosorption rate and obtained results fitted well with the pseudo-second-order (PSO) model. When isotherm data were modeled using the Langmuir and Freundlich isotherm models, the Langmuir isotherm model fit the data better and produced maximal As(V) biosorption capacities of 0.72 ± 03, 0.86 ± 06, and 0.95 ± 05 mmol/g at temperatures 293± 1K, 298± 1K and 303± 1K, respectively. Desorptionof As(V) was effective using 0.1 M NaOH in batch mode. Negative values of ΔG° for all temperatures with positive ΔH° confirmed the spontaneous and endothermic nature of As(V) biosorption. The existence of co-existing chloride (Cl-), nitrate (NO3 -), sodium (Na+), and calcium (Ca2+) showed insignificant interference whereas a high concentration of sulphate (SO4 2-) and phosphate (PO4 3-) significantly lowered As(V) biosorption percentage. Arsenic concentrations in actual arsenic polluted groundwater could be reduced to the WHO drinking water standard (10 µg/L) by using only 1 g/L of investigated Fe(III)-SPP. The dynamic biosorption of As(V) in a fixed bed system showed that Fe(III)-SPP was effective also in continuous mode and different design parameters for fixed bed system were determined using Thomas, Adams-Bohart, BDST, and Yoon-Nelson models. Therefore, from all of these results it is suggested that Fe(III)-SPP investigated in this study can be a potential, low cost and environmentally benign biosorbent material for an effective removal of trace amounts of arsenic from polluted water.

Alkaline Treatment Variables to Characterize Poly(Vinyl Alcohol)/Poly(Vinyl Butyral/Vinyl Alcohol) Blend Films.

Novel poly(vinyl alcohol) (PVA)/poly(vinyl butyral-vinyl alcohol) (P(VB-VA)) films with improved hydrophobicity were prepared from poly(vinyl acetate) (PVAc)/poly(vinyl butyral) (PVB) blend films with various mass ratios by saponification in a heterogeneous medium. The successful conversion of PVAc to PVA and PVAc/PVB to PVA/P(VB-VA) films was confirmed by Fourier transform infrared spectrometry, X-ray diffraction, and proton nuclear magnetic resonance analysis. This study also shows that the degree of saponification (DS) depends on the saponification time. The maximum DS of 99.99% was obtained at 96 h of saponification for all films, and the presence of PVB did not affect the DS at saponification times of 48-96 h. The effects of the PVAc/PVB blend ratio before and after saponification were determined by contact angle measurement, and the hydrophobicity was found to increase in both cases with increasing PVB content. Additionally, all the films exhibited improved mechanical properties after saponification, and the treated films possessed an unusual porous and uneven surface, in contrast with the untreated films. The prepared films with improved hydrophobicity can be used for various applications, such as biomaterials, filters, and medical devices.

High sensitivity determination of mineral oils and olefin oligomers in cocoa powder and related packaging: Method validation and market survey.

Mineral oil saturated (MOSH) and aromatic hydrocarbons (MOAH) and related hydrocarbons of synthetic origin are both packaging and processing contaminants of health concerns. The purpose of this work was to validate a method for their rapid and high-sensitivity determination in cocoa powder, using it to monitor the presence of these contaminants in products purchased in Italy and North Macedonia. Relevant primary and secondary packaging was also analyzed. Method performance was good (average recovery 74-106 %, with RSD ≤13 %). In addition to pre-existing contamination, oligomeric polyolefin hydrocarbons (POH) from primary plastic packaging and MOSH/MOAH from recycled cardboard secondary packaging were found in many samples. Total MOSH/POH ranged from 1.2 to 69.2 mg/kg (on average 20.9 mg/kg), exceeding the German benchmark levels of 9 mg/kg in half of the samples from Italy and in all those from Northern Macedonia. Most of the samples had MOAH >0.5 mg/kg.

Optimized cell growth and poly(3-hydroxybutyrate) synthesis from saponified spent coffee grounds oil.

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 (C0) 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 (C0 = 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 (C0 = 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.

Methods for extracting and analyzing carotenoids from bird feathers.

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.

Astaxanthin absorption modulated antioxidant enzyme activity and targeted specific metabolic pathways in rats.

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.

Saponification Value of Fats and Oils as Determined from 1H-NMR Data: The Case of Dairy Fats.

The saponification value of fats and oils is one of the most common quality indices, reflecting the mean molecular weight of the constituting triacylglycerols. Proton nuclear magnetic resonance (1H-NMR) spectra of fats and oils display specific resonances for the protons from the structural patterns of the triacylglycerols (i.e., the glycerol backbone), methylene (-CH2-) groups, double bonds (-CH=CH-) and the terminal methyl (-CH3) group from the three fatty acyl chains. Consequently, chemometric equations based on the integral values of the 1H-NMR resonances allow for the calculation of the mean molecular weight of triacylglycerol species, leading to the determination of the number of moles of triacylglycerol species per 1 g of fat and eventually to the calculation of the saponification value (SV), expressed as mg KOH/g of fat. The algorithm was verified on a series of binary mixtures of tributyrin (TB) and vegetable oils (i.e., soybean and rapeseed oils) in various ratios, ensuring a wide range of SV. Compared to the conventional technique for SV determination (ISO 3657:2013) based on titration, the obtained 1H-NMR-based saponification values differed by a mean percent deviation of 3%, suggesting the new method is a convenient and rapid alternate approach. Moreover, compared to other reported methods of determining the SV from spectroscopic data, this method is not based on regression equations and, consequently, does not require calibration from a database, as the SV is computed directly and independently from the 1H-NMR spectrum of a given oil/fat sample.

Green extraction of lutein from marigold flower petals, process optimization and its potential to improve the oxidative stability of sunflower oil.

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.

Headspace solid-phase-microextraction using a graphene aerogel for gas chromatography-tandem mass spectrometry quantification of polychlorinated naphthalenes in shrimp.

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 (R2≥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.