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ABSTRACT Effect of different extraction methods viz., ultra sound assisted aqueous extraction (UAAE), enzyme assisted aqueous extraction (EAAE), mechanical extraction (ME) and solvent extraction (SE) on recovery and quality characteristics of sesame oil was evaluated. The oil so extracted was packed in glass bottles and kept under ambient conditions to study the shelf life. Different quality parameters like refractive index, acid value, saponification value and free fatty acids were evaluated at regular interval of 15 days for 90 days of storage. It was observed that the oil recovery was highest in SE (45%), followed by UAAE (41%) and ME (39%) method. But the quality parameters like acid value (2.25 mg KOH/gm), free fatty acids (1.19 mg KOH/gm), saponification value (199 mg KOH/gm), color and refractive index were better retained in oil extracted by UAAE method than the SE method. It was found that there was a significant increase (p<0.05) in refractive index, acid value, saponification value and free fatty acid content during storage irrespective of extraction methods. The sesame oil extracted by UAAE method packaged in glass bottles can be stored under ambient conditions up to 90 days of storage without deterioration of quality, besides being green method and eco friendly in nature. [ABSTRACT FROM AUTHOR]

In this paper, a comparative study of the physico-chemical properties and composition of walnuts and peanuts oils obtained by cold pressing or Soxhlet extraction in hexane was performed. The physical properties (color, density, refractive index, acidity, saponification, iodine and peroxide values, rheological behavior), the distribution of the major fatty acids in oils (through gas-chromatographic analysis) and the metal content were determined. [ABSTRACT FROM AUTHOR]

An ultrasound‐assisted direct in situ saponification (U‐DS) process was developed to extract unsaponifiable matter (rich in squalene) from the livers of four fish species, sea bass, skipjack tuna, gray bamboo shark, and spot‐tail shark. The conventional solvent extraction method was used for comparison. Box–Behnken experimental design (BBD) was adopted to optimize the independent variables including the biomass/methanol ratio (1:3 to 1:9 w/v), 50% KOH volume (1–12 mL), and sonication time (0–30 min) over the unsaponifiable yield. With the conventional process, the yield of squalene was 0.10 ± 0.02 to 5.52 ± 0.06 g (100 g)−1, whereas the U‐DS process rendered the yield of 0.13 ± 0.03 to 6.86 ± 0.05 g (100 g)−1, depending on the fish species. After extraction, squalene was further concentrated (purity ≥60%) from all fish species via fractional crystallization (yield of squalene concentrate ranged from 48.35% to 74.49%) and purified using a silica gel column with a maximum recovery up to 98%. For all the fractions, components were examined using thin layer chromatography (TLC). Squalene was qualitatively and quantitatively analyzed using reversed‐phase high‐performance liquid chromatography (RP‐HPLC). Entire extraction processes yielded squalene with a purity of ≥94%. Fourier transform infrared (FTIR) analysis confirmed the native structure of squalene with six nonconjugated bonds, suggesting no degradation of squalene taken place during the U‐DS process. Thus, the U‐DS process along with fractionation and purification could be used for recovering the squalene from fish livers. [ABSTRACT FROM AUTHOR]

Cellulose-acetate nanofibers (CA-NF) and regenerated cellulose nanofibers (RC-NF) were separately compounded as reinforcement materials for enhancement of the mechanical property of polylactide (PLA). PLA has a great potential as an alternative to widely-used plastics such as polystyrene and poly(ethylene terephthalate), which are made from petroleum. PLA is well known for its biodegradability and renewability, but the mechanical property of PLA is not sufficient for industrial applications. In this study, CA-NF were successfully fabricated by electrospinning using 20 wt% cellulose-acetate solution with acetone/N,N-dimethylacetamide (6/4, wt/wt) mixture solvent, and RC-NF were synthesized by subsequent saponification, as reinforcement materials for PLA composites. The Young's modulus of CA-NF/PLA composites increased linearly from 1670 to 1840 MPa with the increase in the nanofiber concentration to 15 wt%. In contrast, the Young's modulus of RC-NF/PLA composites rapidly increased to ~ 1840 MPa at the relatively low nanofiber concentration of 5.0 wt%. Above 5.0 wt%, the Young's modulus became stable and almost constant. RC-NF exhibited better reinforcing efficiency due to the excellent mechanical property of RC-NF, although the interfacial compatibility of RC-NF for PLA matrix was relatively poor as compared with that of CA-NF. [ABSTRACT FROM AUTHOR]

In this work, sesame oil and protein hydrolysates were extracted via the enzyme-assisted aqueous extraction (EAAE) process using Neutrase (a commercial protease), Pectinex (a commercial carbohydrate-hydrolyzing enzyme) and a 1:1 mix of Neutrase and Pectinex. All the extractions were performed at 50 °C and the optimum pH of the enzymes for 6 h, and the water to sesame ratio was raged between 1:1 and 6:1. The highest oil recoveries were obtained at 2:1 water to sesame ratio for each treatment and the Neutrase-Pectinex treatment gave the max recovery (89.7%, p < 0.05). The oil extracted using Neutrase-Pectinex treatment, contained the highest amount of unsaponifiables, total phenolic compounds, lignans and showed the highest oxidative stability, color indices and sensory attributes, even higher than the solvent-extracted oil (p < 0.05). However, oils obtained using different treatments were not significantly different in terms of free fatty acids content, iodine value, peroxide value, saponification value and anisidine value (p > 0.05). Protein hydrolysates obtained using Neutrase-Pectinex treatment (NPPH) had lower protein and higher carbohydrate content than that obtained using Neutrase treatment (NPH). The lowest solubility, emulsifying activity and stability indices, foam capacity and foam stability of NPPH and NPH was found to be at pH 4.0. The solubility of NPPH was higher than the NPH, but the emulsification properties of the NPH was better than NPPH at pH 2–10 (p < 0.05). NPPH and NPH were not significantly different in terms of foaming properties (p > 0.05). [ABSTRACT FROM AUTHOR]

The synthesis and investigation of fluorescence and antimicrobial properties of a new series of 1,2,3-triazoles were described. Acetylenes 4a–c were resulted via alkylation of 2-oxonicotinonitriles 3a–c with propargyl bromide in base medium. [2 + 3] cycloaddition of acetylenes 4a–c with ethyl 2-azidoacetate, p-acetylphenylazide, and p-tolylsulfonylazide in the presence of Cu(I) afforded 1,2,3-triazoles 5a–c, 7a–c, and 9, respectively (via click reaction). The triazoles 5a–c were subjected to saponification process to give the acids 6a–c. The fluorescence and antimicrobial properties of triazoles 5a–c, 7a–c, and 9 were investigated and significant results were obtained. [ABSTRACT FROM AUTHOR]

Highlights • Ultrasound-assisted saponification and LLE were used to extract targets from oil. • Conditions of saponification were optimized by using central composite design. • Simultaneous determination of tocopherols, carotenoids and phytosterols were proposed. Abstract A method was developed to simultaneously determine eight bioactive compounds in edible oil based on ultrasound-assisted saponification, liquid-liquid extraction and liquid chromatography coupled with tandem mass spectrometry. Central composite design was employed to optimize ultrasonic temperature and time of saponification. Sample treatment was conducted by ultrasound-assisted saponification at temperature of 75 °C for 40 min. Limits of detection and limits of quantification ranged from 2.0 to 3.2 and from 6.1 to 10.0 ng/mL, respectively. Linear correlations were obtained (R2 > 0.99) and the recoveries at three spiked levels were between 81.7% and 112.0%. This method was employed to determine eight compounds in camellia oils and olive oils. As results, the contents of stigmasterol, δ-tocopherol, γ-tocopherol, β-carotene and lutein in camellia oils were significantly higher than those in olive oils (p < 0.05). The proposed method can be successfully used to determination of these eight active compounds in camellia oil and other edible oils. [ABSTRACT FROM AUTHOR]

• PCC cylinders were repeatedly exposed to hydrocarbon fluids and high thermal cycles. • Cylinders experienced saponification and developed scaling on the surface. • The depth of penetration of hydrocarbon fluids into cylinders influenced the depth of scaling. • The w/c ratio of concrete significantly affected saponification process and surface scaling. • Exhaust heat of military aircrafts caused micro to hairline cracks in ordinary concrete. The conventional Portland cement concrete (PCC) aprons that house Air Force and Navy aircrafts are reported to experience significant scaling on the surface, which is a serious concern for the safe operation of military aircrafts. The purpose of this study is to investigate the underlying scientific facts for the scaling of PCC aprons at military airbases. An experimental program was developed to replicate the physical and environmental circumstances that prevail in aprons at military airbases. Standard sized PCC cylinders were repeatedly exposed to aviation oils and high temperature, both simultaneously and separately, until surface scaling became obvious. Chemical analyses were conducted on the aviation oils, scaled concrete as well as on the original PCC; analysis results revealed that aviation oils contain ample hydrocarbon compounds to trigger surface scaling at high temperature. When PCC cylinders were repeatedly exposed to aviation oils and high temperature simultaneously, they underwent a saponification process after a couple of cycles of exposure, and rapidly developed scaling on the surface after subsequent exposures. Saponification increased with the increase in numbers of cyclic exposures and consequently resulted in the development of a significant volume of loose fines on the surface of the PCC cylinders. The repeated saponification and deposition of calcium phosphate (salts) at the top layer caused rapid scaling, by acting together. On the other hand, PCC cylinders that were exposed to aviation oils at ambient temperature neither experienced a saponification process nor developed scaling. The influence of w/c ratio on the saponification, scaling and thermal cracking was examined as a part of the current study. The present study reveals a relationship between the depth of scaling and aviation oils' penetration depth, and the effect of high temperature, microcracks and voids, and their influences on the scaling process of PCC are also reported herein. [ABSTRACT FROM AUTHOR]

In order to reduce the environmental threat of kitchen waste, the gutter oil was transformed into renewable collector by saponification and used for flotation of fluorite. The adsorption characteristics of the collector on fluorite surface were analyzed by X-ray photoelectron spectroscopy (XPS). The influence of the collector dosage and inhibitor dosage on the separation efficiency was analyzed by the flotation test. XPS results show that collector can change the charge characteristics of calcium ions, indicating that the collector has significant adsorption on the fluorite surface. Separation results show that the renewable collector has achieved an excellent effect on fluorite flotation. [ABSTRACT FROM AUTHOR]

• Unusual saponification of lead-tin yellow in an egg tempera Gothic painting was found. • Pigment-binder interactions were studied to explain saponification in temperas. • Lead-tin yellow reacted with egg yolk binders more easily than with oils. • Corresponding reference lead carboxylates were synthesised in pure-phase form. • The formed lead soaps are mixed lead palmitate-stearates of various stoichiometry. Saponification occurring in paint layers of artworks represents a serious degradation process affecting the appearance and stability of paintings. Formation of metal soaps is mostly reported as a consequence of the interaction of lead white or zinc white with oil binder. We found the distinct symptoms of saponification in paint layers consisting of lead-tin yellow type I and egg yolk binder in a panel painting from the 15th century. This scarce finding induced the study of interactions between lead-tin yellow type I with three different binders: (i) egg yolk tempera, (ii) emulsion of egg yolk and oil, and (iii) oil. The interactions were studied in long-term model experiments using infrared spectroscopy (FTIR) and powder X-ray diffraction (XRD). Based on the results, a set of mixed lead carboxylates of the series Pb(C16) 2-x (C18) x , where x = 0; 0.25; 0.5; 0,75; 1; 1.5 and 2, was synthesised as reference materials suitable as a basis for proper identification of neo-formed lead soaps by FTIR and XRD. The formation of lead soaps was detected already within 1 month of reaction in egg yolk containing binders, whereas no soap was formed during 6 months of the experiment in the oil mixture. The neo-formed soaps are various mixed lead carboxylates containing both palmitate (C16) and stearate (C18) in one crystal structure and the proportion of carboxylate anions is affected by the type of the binder. We found the C16:C18 ratio in mixed lead carboxylates is higher in egg yolk tempera samples in accordance with the more abundant palmitic acid in egg yolk fat. On the other hand, the lower C16:C18 ratio in emulsion binder correlates with increased content of stearic acid, suggesting contribution of both binders, i.e. egg yolk and oil, to the soap formation. [ABSTRACT FROM AUTHOR]

This article reports on direct electrospinning of water-soluble cellulose acetate (WSCA) and cellulose diacetate (CDA) onto a non-conductive synthetic polymer sheet such as polyurethane (PU) sheet to modify its surface morphology. The direct electrospinning was successfully performed after spraying an anti-static agent on the PU sheet. Furthermore, tight fixation of the fibers was achieved by spraying a dimethylformamide/ethanol (1/1) solution during the spinning. Finally, the cellulose acetate fibers on the PU sheet were converted to regenerated cellulose fibers by saponification. Changes in surface morphology were evaluated via tribology tests. The friction coefficient of the PU sheet significantly decreased with increases in the amount of deposited fiber, thereby suggesting that the PU sheet surface became smoother. After saponification, the friction coefficients of the sheets slightly increased, with the exception of the PU sheet with the increased amount of saponified WSCA fibers, and this was potentially attributed to changes in the elasticity upon saponification. [ABSTRACT FROM AUTHOR]

The objective of this study was to develop a safe and ecologically sustainable protocol, to extract and separate lutein and chlorophyll from spinach discards. A saponification in an aqueous medium was carried out to release the phytyl aliphatic chain from the porphyrin ring of chlorophyll. Polar chlorophyll derivatives were formed, remaining in the aqueous medium, whereas apolar lutein remaining in the plant residues and was extracted thereafter by maceration in 95% ethanol. However, the saponification step may cause a significant degradation of lutein, resulting in low extraction yields. The saponification parameters were studied using response surface methodology to determine the conditions providing the highest recovery of lutein in an ethanolic extract, combined with the lowest loss of chlorophyll derivatives. Through this procedure, using the Derringer's desirability function, we uncovered that the optimal conditions for saponification were 16 h of aqueous maceration with 3.9% (W/V) sodium hydroxide at 60 °C. This procedure can be easily scaled for high volume commercial extraction of these compounds. [ABSTRACT FROM AUTHOR]

Camellia oleifera, C. japonica and C. sinensis are three representative crops of the genus Camellia. In this work, we systematically investigated the lipid characteristics of these seed oils collected from different regions. The results indicated significant differences in acid value (AV), peroxide value (PV), iodine value (IV), saponification value (SV) and relative density of the above-mentioned camellia seed oils (p < 0.05). The C. japonica seed oils showed the highest AV (1.7 mg/g), and the C. sinensis seed oils showed the highest PV (17.4 meq/kg). The C. japonica seed oils showed the lowest IV (79.9 g/100 g), SV (192.7 mg/g) and refractive index (1.4633) of all the oils, while the C. sinensis seed oils showed the lowest relative density (0.911 g/cm3). The major fatty acids in the camellia seed oils were palmitic acid (16:0), oleic acid (18:1) and linoleic acid (18:2); the oleic acid in C. oleifera and C. japonica seed oils accounted for more than 80% of the total fatty acids. The oleic acid levels in the C. oleifera and C. japonica oils were higher than those in the C. sinensis seed oils, while the linoleic acid levels in the former were lower than those in the latter one. Differences also exist in the triacylglycerol (TAG) composition, although the most abundant TAG molecular species in the camellia seed oils was trioleoylglycerol (OOO). Seven sterol species, squalene and a-tocopherol were detected in the camellia seed oils, however, the contents of tocopherol and unsaponifiable molecules in the C. oleifera and C. japonica seed oils were significantly lower than those in the C. sinensis seed oil. These results demonstrated that the varieties of Camellia affected the seed oil lipid characteristics. [ABSTRACT FROM AUTHOR]

Introduction. A deodorizer distillate is a byproduct of oil deodoration, a natural source of tocopherols. The methods of obtaining a native antioxidants from a sunflower deodorizer distillate was investigated in this study. Materials and methods. The sunflower deodorizer distillates from a local enterprise were used in this work. The unsaponificated fraction of deodorizer distillate was separated by saponification. The kinetics of sunflower oil oxidation with/without antioxidants is investigated by the volumetric method. Results and Discussion. Deodorizer distillate increased sunflower oil induction period of oxidation by 1.5 times. Antioxidant activity of obtained concentrates was proved by increase of the induction period of oil oxidation almost three times as result of them addition in the amount of 50 mg per 100 g. Thus, saponification of deodorizer distillate gives possibility to obtain sufficiently effective inhibitor of oxidation. It was shown that more effective way of antioxidants concentrating from a deodorizer distillates was to dissolve it in n-hexane with further adsorption of tocopherols on the activated carbon. Tocopherols were proposed to be eluted from activated carbon by m-xylene, after evaporation of which a concentrate of tocopherols was obtained. Obtained concentrate increased in the period of sunflower oil oxidation induction by 4.2 times when 50 mg per 100 g of the antioxidant were added to the oil. The value of the rate constant of interaction of the peroxide radical with the inhibitor (K7) for the obtained antioxidant was determined to be 106 mol/l∙sec. Conclusions. A method of obtaining tocopherol concentrates from sunflower oil deodorant was proposed. The efficacy of the obtained tocopherol concentrate as an antioxidant was proved. [ABSTRACT FROM AUTHOR]

A short enantioselective total synthesis of englerin A, a guaiane sesquiterpene with significant in vitro antitumor activity, is reported. Key features of this total synthesis are an organocatalytic asymmetric decarboxylative aldol reaction, a neighboring‐group‐participating [4+3] cycloaddition, a novel one‐pot Heck coupling/regioselective 1,4‐hydrosilylation/Tamao–Fleming oxidation cascade, and a kinetic CBS reduction, generating the optically pure natural product in 6.7 % overall yield over twelve steps starting from methylglyoxal. Selective saponification of the more reactive glycolic ester moiety of englerin A also gave (−)‐englerin B. [ABSTRACT FROM AUTHOR]

Polyurethane foam (PU foam) is a new material which is being used in producing both macro-anatomical and micro-anatomical specimens. PU foam is simple to use, without need for special equipment. The present study was carried out to evaluate morphology of coronary sinus and its tributaries. During the study, we encountered few problems in carrying out injections. Coronary sinus and its tributaries were difficult to cannulate since the coronary sinus lacks a vascular stem, around which ligature can be tied before injection so that the cannula can be held in place. In contrast, in majority of the organs it is easy to inject since they possess tubular vascular stem to hold the cannula in place. A new device was developed which could be used to cannulate coronary sinus orifice to inject the casting media. The second problem we faced was saponification of adipose tissue. This made corrosion of the soft tissue difficult. Hence in this study, we describe the device we have developed to place in the coronary sinus orifice, and how saponified adipose tissue was taken care during the actual maceration step. [ABSTRACT FROM AUTHOR]

Abstract A quick and cheap method for cholesterol quantification in egg yolk by UV-VIS-NIR spectroscopy was developed. Cholesterol was saponified and extracted from shell egg yolks or pasteurised egg yolks. Spectral data (144 spectra) were obtained from 38 samples. Different transformations of the spectra (smoothing Savitzky-Golay, standard normal variate, multiplicative scatter correction, detrending, baseline correction and first and second derivative) and modelling strategies such as Partial Least Squares (PLS) regression or Principal Component Regression (PCR) were evaluated. An enzymatic method was selected as reference procedure. Cholesterol content quantified was significantly lower in pasteurised egg yolks than in shell egg yolks. Best results were obtained using PLS and first derivative Savitzky-Golay combined with baseline correction, achieving a model with a determination coefficient of 0.93. Total cholesterol quantification was increased with saponification conditions improvements. Results obtained demonstrate that UV-VIS-NIR spectroscopy can be used to determine cholesterol from shell egg yolks or pasteurised egg yolks. Highligths • Available techniques for cholesterol quantification in egg are expensive. • Standard methods underestimate the amount of cholesterol in egg. • Yolks from shell eggs and pasteurised egg yolks were analysed. • UV-VIS-NIR spectroscopy followed by chemometrics regression models were applied. • Partial Least Square regression achieved a coefficient of determination of 0.93 [ABSTRACT FROM AUTHOR]

A functionalized hydrogel composed of 2-(hydroxyethyl) methacrylate (HEMA) and acrylamide (AAm) was synthesized by amination and saponification reactions, respectively, and its functionality was examined for the elimination of copper(II) ions. The maximum adsorption capacity for copper(II) ions was 0.617 mmol g-1before saponification, whereas it was 1.2225 mmol g-1 after saponification. The adsorption data was analyzed with pseudo-first-order (r2=0.8867), intra-particle diffusion (r2=0.9453), Elovich (r2=0.9489) and pseudo-secondorder( r2=0.9999) kinetic models. Based on the adsorption equilibrium experimental data Freundlich(r2=0.9964), Langmuir(r2=0.998) and Dubinin-Radushkevich (D-R) (r2=0.9960) adsorption isotherms provided good fits for all of experimental results. Finally, the datas of kinetic experiments obtained in this study showed the applicability of the functionalized gel for Copper(II) ion removal. [ABSTRACT FROM AUTHOR]

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On the basis of the determination of the rate constant of ethyl acetate saponification reaction, theoretical calculation is added. The models of the reactants and intermediate are constructed by using GaussView 5.0, then the energies of reactants and intermediate are calculated by Gaussian 09W, finally the activation energy is calculated. The experimental measurement is mainly to monitor the change of the system conductivity with time and temperature in the process of saponification by the conductivity meter. The reaction rate constant and activation energy are obtained by experimental data. At the end, the activation energies obtained by the two methods are compared. The design explores the feasibility and implementation of combining experiment with theory, and helps to form a new comprehensive chemical experiment mode combining experimental measurement with theoretical calculation. Through this experiment, students not only exercise their ability to operate, but also mastered the use of computing software, understand the mechanism of chemical reaction at the molecular level, their enthusiasm is stimulated to participate in experiments, and their comprehensive experimental skills are improved. [ABSTRACT FROM AUTHOR]

Background: Currently, there is a lack of validation studies available in the literature for the determination of ergocalciferol, especially for those using a direct extraction technique. The current official methodologies for the quantification of ergocalciferol require saponification, liquid−liquid extraction, or both, thus requiring experienced technicians and specialized reflux equipment. This work provides a method that is more easily accessible to laboratories without these resources while still achieving the robustness needed for a successful validation of low levels of ergocalciferol in complex matrixes. Objective: A single-laboratory validation study was conducted for a rapid quantification method of ergocalciferol in protein drink powders and tablets. Methods: The method uses an LC-MS/MS with multimode source utilizing atmospheric pressure chemical ionization positive ionization mode. For both protein drink powders and tablets, the procedure consisted of a liquid extraction step using dimethyl sulfoxide and methanol. Isotopically labeled ergocalciferol was used as an internal standard to correct for signal depression caused by matrix interference. Results: This LC-MS/MS method was found to be accurate, precise, linear (from 0.01 to 0.3 μg/mL), rugged, and suitable for protein drink powders and tablets. Conclusions: The method was validated and is suitable for accurate quantification of ergocalciferol in tablet and protein powder products. Highlights: This work provides a validated method for accurate quantification of ergocalciferol in complex matrixes using a direct extraction technique. This may benefit quality control laboratories in the food and nutraceutical industries, where simple and efficient methodology is key to optimal functioning. [ABSTRACT FROM AUTHOR]

Abstract The saponification process of di(2-ethylhexyl)phosphoric acid extractant (D2EHPA) was investigated by the isothermal titration calorimetry (ITC), attenuated total reflection infrared (ATR-IR), and small-angle X-ray scattering (SAXS) spectroscopies. The effects of the temperature, types of saponifier, and diluent on the saponification process of D2EHPA were disclosed by ITC method. The saponification reaction is an exothermic process, but the contribution of temperature on the maximum saponification degree of D2EHPA is slight. The theoretical maximum saponification degree of D2EHPA is about 40%. Moreover, the maximum effective saponification degree of D2EHPA is the same at the condition of different saponifiers because the two systems release the same amount of heat. The effective saponification degree of D2EHPA in octane is larger than that in toluene at the same content of saponifier. The IR spectra indicate that the structure of organic phases varies significantly with the increase of saponification degree. The most water-in-oil microemulsion in the organic phase is formed at the 40% theoretical saponification degree. The water content and SAXS data of organic phase further verify this phenomenon. Solvent extraction results show that the saponified extractant can obviously improve extraction efficiency of cobalt. These results will be helpful for optimizing the saponification process of D2EHPA during metal extraction. Highlights • The saponification process of D2EHPA was studied by ITC, ATR-IR and SAXS methods. • The effects of the temperature, types of saponifier, and diluent were evaluated. • The theoretical maximum saponification degree of D2EHPA is about 40%. • The most water-in-oil reverse micelles are formed at the 40% saponification degree. [ABSTRACT FROM AUTHOR]

• Used cooking oils (UCOs) generation was estimated for Colombia and its capital city. • Household users were identified as the major UCOs generators. • Hamburger and chicken restaurants were identified as main UCOs generators. • Available UCOs were subjected to physicochemical characterization. • Available UCOs can be used as oleochemical feedstock. This work is focused on assessing the potential for the exploitation of used cooking oils (UCOs) as oleochemical feedstock for urban biorefineries. The study case was developed for the city of Bogotá, Colombia. Initially, and according to data from major fats and oils distributors, market information, and public databases, it was estimated that total annual generation of UCOs in Colombia is about 225,000 t, with a per capita of ca. 5 kg/person/yr. Correspondingly, UCOs generation in Bogotá was estimated in at least 45,000 t/yr., with a major generation occurring at Household and HORECA (Hotels, Restaurants and Catering) segments. Specifically in HORECA, fast food restaurants (in particular those of hamburger and chicken) were identified as the main UCOs generators with a suitable supply for industrial exploitation. Then, UCOs samples from this segment of restaurants were subjected to physicochemical characterization by determination of density, volatile matter content, acid value, color, peroxide value, saponification value, iodine value, and content of total polar compounds. The properties associated with the degree of degradation of the oil showed a large variation, even among samples from the same origin. This heterogeneity indicates the need for a pre-treatment process before its reuse. Despite the heterogeneity of the samples, density, iodine value, and saponification value showed slight changes among the different restaurants, largely depending on the nature of the processed cooking oil rather than on the cooking conditions. The collected UCOs showed iodine values and saponification indexes ranging between 80 and 119 g I2/100 g, and 178–201 mg KOH/g, respectively. This indicates that after a suitable purification, UCOs could be used as raw material for a variety of high value oleochemicals. Finally, based upon market data, and to boost further studies, some promissory value-added derivatives are identified. [ABSTRACT FROM AUTHOR]

The synthesis of biodiesel using rubber seed oil by a transesterification reaction using cement clinker catalysts was studied. The mineral composition and morphology of both the catalysts were analysed using X-ray diffraction and scanning electron microscopy. The gas chromatography-mass spectrometry, Fourier transform infrared spectroscopy and nuclear magnetic resonance studies were used to find the Fatty acid methyl ester content and various compounds of esters in the synthesised biodiesel, which showed an efficient conversion of rubber seed oil to biodiesel. The highest yield of 80% was obtained from calcium oxide catalyst (1.5 g) activated at 50°C with a methanol-to-oil ratio of 6:1. The highest yield of 70% biodiesel was obtained using a cement clinker catalyst (0.5 g) activated at 50°C with a methanol-to-oil ratio of 6:1. The significant physical properties of biodiesel flash point, acid value and saponification value were found, and the results are within the American standard test method (ASTM D6751) limits. [ABSTRACT FROM AUTHOR]

Sample preparation techniques for the analysis of vitamin D3 in food matrices typically utilise a saponification step, either at room temperature or at elevated temperatures. A calciferol (vitamin D2 or isotope labelled vitamin D3) is generally chosen as the internal standard to compensate for changes of previtamin D3–vitamin D3 isomerisation during analysis, as well as to correct for analyte loss through complex sample preparation steps. Manufacturing practices and processing parameters contribute to previtamin D formation in food products. A significant proportion (5.6–8.3%) of the total vitamin D3 in premixes was found as previtamin D3, indicating that it is likely, depending upon storage temperature and the time since manufacture, that a vitamin D3-fortified food product will contain a similar proportion of previtamin D3 prior to analysis. Conversely, freshly prepared internal standard solutions have low previtamin D levels (< 1%). In lieu of direct measurement, this discrepancy in previtamin D content between the internal standard and analyte forms of vitamin D will lead to analytical bias. To mitigate this as a source of potential error, it is recommended that sample pretreatment steps are appropriately set and controlled. Based on this work, saponification times greater than 300, 120, or 60 min for temperatures of 60, 70, or 80 °C respectively should be employed and that saponification at room temperature be avoided. [ABSTRACT FROM AUTHOR]

This article was aimed to compare soap character with the difference concentration of bidara leaf extraction. Bidara leaf soap was prepared by soft saponification using NaOH which is involved with bidara leaf. Soap analysis has been investigated by colour, cleaning power, foam power dan pH. Based on the result, the soap with 2% concentration of bidara leaf had the highest cleaning power with soft texture, high soap power and appropriate pH for skin care. From FTIR observation and manual soap test was predicted that bidara leaf not only act as catalyst that increase saponification rate but also act as soap hidrophilicity enhancer. [ABSTRACT FROM AUTHOR]

Highlights • Determination of eight PAHs in fruits, vegetables, meats products, and their products. • Method validation proceeded on non-fatty solid (fruit, vegetable) & fatty solid (meat) • Good linearity gained for the PAHs at all concentrations (R2 > 0.99) • Recovery experiments for the PAHs ranged from 88.75 to ∼100.00% • LOD was 0.08–0.25 µg/kg and LOQ was 0.24–0.75 µg/kg. Abstract The current investigation was performed to evaluate the chemical analytical techniques for PAHs (organic, carcinogenic and mutagenic compounds) in food. It also determines the content of eight polycyclic aromatic hydrocarbons (PAHs) in frequently consumed fruit, vegetables, meats and their products. The methodology included saponification or ultrasonication, liquid-liquid extraction with solvents like n -hexane, clean-up using a silica solid phase extraction cartridge and a gas chromatography-mass spectrometry technique. A good linearity (R2 > 0.99) was achieved for the PAHs at different concentrations. Recovery results for PAHs extended from 88.75 to ∼100.00%. The limit of detection was 0.08–0.25 µg/kg and the limit of quantification was 0.24–0.75 µg/kg. The mean concentration (n = 3) of benzo[a]pyrene was not identified in fruits, was 0.05 µg/kg in vegetables, and 0.64 µg/kg in meat products. Overall concentration of the eight PAHs was 0.67 µg/kg in fruits, 0.82 µg/kg in vegetables, and 3.37 µg/kg in meat products. [ABSTRACT FROM AUTHOR]

This study deals with the covalorization of spent bleaching clay (SBC) and palm fatty acid distillate (PFAD), the by‐products of palm oil‐refining plants (3 Mt. year−1), through soap manufacture. Obtained SBC and PFAD samples show differing acidity and saponification values depending on their content of free fatty acids and of acylglycerols. The SBC sample had an acidity of 60.5% and a saponification value of 182 mg KOH g−1 of oil, and the PFAD sample has an acidity of 88.4% and a saponification value of 204 mg KOH g−1 of oil. Soaps are prepared using the stoichiometric amount of NaOH, under varying proportion of water introduced through the basic solution. The overall reaction (neutralization and saponification) is complete (99.9%) with PFAD, whereas the yield reaches only 56.1% with SBC. When mixing SBC and PFAD, for example under a 1:1 weight ratio, the overall reaction completion (87.7%) is surprisingly higher than expected based on the computed individual reaction yields (78%), showing a synergistic effect of about 10% on the course of the saponification reaction of acylglycerols in SBC. The water content was found to be a critical parameter, 30% w/w of added water providing the highest yield. These results show an innovative way for covalorizing two important by‐products of palm oil industrial processing as a single final product. By‐products of the physical refining of other oils could also be valorized following the same method. [ABSTRACT FROM AUTHOR]

The aim of present study is to develop an accessible accurate estimation of CN based on fatty acid methyl esters and to provide a proper solution for presenting a user‐friendly method. In fact, this study calculates the density, viscosity, and HHV based on FAMEs and predicts the CN by employing fuzzy method within a set. This is an interesting approach that has not been used in similar articles. Gaussian membership functions with 81 roles were employed to develop the fuzzy model. The model was developed based on Carbon number, Double bond, Saponification number, and Iodine value to predict the CN. Performance factors of r, RMSE, MAE, and R2 were calculated as 0.9912, 1.0723, 0.63427, and 0.9828, respectively to predict the CN. The results of FAMEs effect on properties of biodiesel showed, increasing Carbon number of FAMEs increases the CN, viscosity, and HHV, but increasing the number of Double bonds decreases CN, viscosity, and HHV. While the effect of increasing Carbon number of FAMEs on density was vice versa. Based on results, C16:00, C18:00, C18:1, and C18:02 FAMEs are approximately in components of all conventional oils; therefore, they can be effective on physical properties of biodiesels. © 2019 American Institute of Chemical Engineers Environ Prog, 38: 584–599, 2019 [ABSTRACT FROM AUTHOR]

Graphical abstract Abstract We investigated the effects of polymer addition on crack formation in particulate films of colloidal silica. Two types of polyvinyl alcohol (PVA) with different degrees of saponification were compared. Partially saponified PVA (PVA-1) suppressed crack formation. In contrast, weaker suppression was observed when we used fully saponified PVA (PVA-2). Centrifugation experiments of colloid–polymer suspensions revealed that PVA-1 adsorbed on particles well whereas PVA-2 was not adsorbed effectively, suggesting that the polymer–particle interactions strongly depended on the content of polymer functional groups. In addition, we observed segregation of PVA-2 between packed particles, which contributed to a sparse packing structure. We did not observe such segregation of PVA-1 and particles were packed more tightly than for PVA-2. These results clearly showed that the affinity between polymer molecules and suspended particles affected both crack formation and packing structures. We also found that adsorption of polymer molecules did not necessarily suppress crack formation. When we added polyvinyl pyrrolidone (PVP) to silica suspensions, we observed much more cracks than in the sample without polymer even though PVP molecules adsorbed on the silica particles. We conclude that adsorption of polymer molecules on suspended particles is preferable, but does not necessarily suppress crack formation. Miscibility between polymer molecules and particles would be a key issue in crack formation and packing structure of colloid-polymer films. [ABSTRACT FROM AUTHOR]

Microreactors intensify chemical processes due to improved flow regimes, mass and heat transfer. In the present study, the effect of the volume flow rate on reactor performance in different reactors (the T-shaped reactor, the interdigital microreactor and the chicane microreactor) was investigated. For this purpose, the saponification reaction in these reactor systems was considered. Experimental results were verified using the obtained kinetic model. The reactor system with a T-shaped reactor shows good performance only at high flow rates, while the experimental setups with the interdigital and the chicane microreactors yield good performance throughout the whole range of volume flow rates. However, microreactors exhibit a higher pressure drop, indicating higher mechanical flow energy consumption than seen using a T-shaped reactor. [ABSTRACT FROM AUTHOR]

This paper addresses energy generated in a passive anion‐exchange membrane micro fuel cell (PAEMμFC) using glycerol from several kinds of sources: high‐purity glycerol (HPG), saponification process‐derived glycerol (SPDG), crude glycerol from sunflower oil biodiesel (CGSOB) and crude glycerol from cooking oil biodiesel (CGCOB). Spectrophotometry, volumetric Karl Fischer, gas chromatography, calorimetry, Fourier transform infrared, and cyclic voltammetry were employed for the glycerol samples characterization. The PAEMμFC was tested using 0.1M glycerol of each type, achieving power densities of 1.008, 0.932, 0.871, and 0.865 mW cm−2 for HPG, SPDG, CGSOB and CGCOB, respectively. On the other hand, commercially available software from ANSYS, Inc. was used to determine the fuel velocity and pressure in the fuel reservoir and current collector as a complementary evaluation of the PAEMμFC. The results obtained for the prices of the energy of each glycerol sample were presented in order to demonstrate that the cost of energy generated through HPG is approximately 16.5 times the SPDG energy cost and 130 times the CGCOB energy cost. [ABSTRACT FROM AUTHOR]

Highlights • RG-I and RG-II domains were isolated from ginseng and structurally characterized. • Ginseng RG-I contained arabinan, galactan and AG-II as side chains. • Both low-branched and high-branched side chains linked to ginseng RG-I backbone. • RG-II domain in ginseng root was first isolated and analyzed. Abstract Rhamnogalacturonan I (RG-I) and rhamnogalacturonan II (RG-II) domains were isolated from ginseng pectin by alkali saponification and endo-polygalacturonase hydrolysis, then purified by anion-exchange and size-exclusion chromatography. Monoclonal antibody detection indicated that ginseng RG-I contained →4)-α-GalpA-(1→2)-α-Rhap-(1→ repeating units as backbone, with arabinan, galactan and type II arabinogalactan (AG-II) as side chains. The use of galactose- and arabinose-releasing enzymes, mass spectrometry analysis of the oligosaccharides generated by rhamnogalacturonan hydrolase, and glycosidic linkage analyses provided evidence that ginseng RG-I contains both single galactose-branched subunits and highly branched subunits with arabinan and AG-II side chains. RG-II was analyzed by sequential acid hydrolysis followed by mass spectrometry. Ginseng RG-II contains 9 galacturonic acid units as backbone. Side chain A is an octasaccharide with 0 ∼ 1 methyl ether group. Side chain B is a nonasaccharide with 0 ∼ 1 acetyl group. These results provide useful information for further investigation of structure-activity relationship of ginseng pectin. [ABSTRACT FROM AUTHOR]

Highlights • The additives and sonication both influenced the physicochemical properties. • The effects of ultrasound pretreatment varied by the basicity of the solution. • The ultrasound raised the weight loss rate in water and borax environments. • The main volatile products of samples are different in different pretreatment. • The crystallinity of treated samples increased from 6.34% to 11.29%. Abstract This work investigated the physicochemical properties of Chinese fir after ultrasound-assisted pretreatments with borax and sodium hydroxide additives in an aqueous solution. TGA, FTIR, and XRD were used to analyze the thermal degradation processes, changes in chemical structures, and crystallinity of the treated samples, respectively. Additionally, the release of volatiles from wood pyrolysis was measured on-line by the TG-FTIR apparatus. In thermal analysis, all samples showed main degradation stages at 220–500 °C, and alkaline compounds could efficiently shift the process to lower temperatures with lower maximum weight loss rate (MWLR) and more residues. From TG-FTIR, it was observed that CO 2 was the primary gas product from pyrolysis in the alkaline-treated samples, while there were more carbonyl compounds released in the control and deionized water groups. Due to the destruction and removal of hemicellulose and lignin after alkaline treatments, the related peaks changed greatly. Changes in the ester groups caused by saponification also accounted for one of the most significant differences between samples. Moreover, except for the deionized water group without sonication, the crystallinity of the samples increased from 6.34% to 11.29%. Overall, comparing the samples treated with or without ultrasound, the results showed that the ultrasound treatment did influence the samples' physicochemical properties, and its' effects varied by the basicity of the solution. This in-depth investigation offers a better understanding of ultrasound-assisted and alkaline pretreatments of wood materials. [ABSTRACT FROM AUTHOR]

The synthesis of highly luminescent non-toxic nanocrystals (NCs) and the subsequent phase transfer to aqueous solution by hydrolysis of the crystal-bound ester are presented. Therefore, the synthesis of the spherical semiconductor system InP/ZnS was modified by changing the sulfur precursor in the synthesis from 1-dodecanethiol to dodecyl 3-mercaptopropionate (D3MP). By employing D3MP both as sulfur precursor for the ZnS shell growth and as stabilizing ligand, the phase transfer from organic to aqueous solution can be performed easily. Instead of the usually employed ligand exchange with mercaptopropionic acid, the NCs are only shaken with a sodium borate buffer in order to obtain aqueous soluble NCs by hydrolysis of the ester. In future work, the NCs must be protected against aggregation and the long term stability has to be increased. The optical properties of the samples are investigated by UV/Vis and photoluminescence spectroscopy, and the morphology of the nanoparticles (NPs) before and after phase transfer is determined by transmission electron microscopy. [ABSTRACT FROM AUTHOR]

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

• LA-RNH 2 extraction system have pronounced synergistic effect on Sm. • This study provides a new idea for the saponification of acidic extractant. • Ion association mechanism of the saponification strategy was investigated. • This ionic liquid saponification strategy can avoid saponification wastewater. • It has revealed application potential for the recovery of SmCo magnets. Acidic extractant is a kind of extractants commonly used in critical metal recovery industry, but the saponification wastewater generated during the saponification process inevitably causes environmental pollution. In order to develop a sustainable separation strategy for rare earth, the synergistic effect between lauric acid (LA) and primary amine N1923 (RNH 2 , with R = C 19 -C 23) was investigated in this paper. The study revealed that the hydrogen bond between LA and RNH 2 was helpful to realize the saponification of LA, thereby significantly improving the extraction and separation performance of LA. Unlike the quaternary ammonium or quaternary phosphonium in ionic liquid saponification studied in the previous study, RNH 2 can independently combine hydrogen ions to achieve the deprotonation of LA without adding alkali or basic resin, which makes the extraction and separation process more environmentally friendly. Aiming at the recovery of samarium cobalt (SmCo) magnet, the separation of Sm and Co in chloride medium was systematically studied. When LA and RNH 2 were combined in equal molar proportions to extract Sm, the extraction system demonstrated a high synergistic coefficient of 61.94, and separation coefficient of Sm and Co was remarkably high at 5326.2. It showed that the LA-RNH 2 extraction system for recovering Sm and Co from actual SmCo magnets could achieve 93.19 % recovery of Co, 90.53 % recovery of Sm and 16,222 Sm/Co separation factor. The LA-RNH 2 extraction system has shown potential applications in Sm/Co separation and waste SmCo magnet recovery processes. It also provides a novel strategy for the saponification of acidic extractant without alkali consumption and saponification wastewater discharge. [ABSTRACT FROM AUTHOR]

[Display omitted] • Unheated oils age differently than heated oils. • The container in which the oils are heated affects their ageing process. • Unheated oils develop secondary oxidation products at a slower rate. • Heating in copper produces more secondary oxidation than other containers. • The acid values of only unheated oils decrease between 6 months to 1 year. • The saponification values of unheated oils increase faster during the first six months. This study compares the ageing process of heated oil with unheated oil and assesses the effect of container used in heating on ageing. Four types of oils were heated on glass, copper and iron. The samples were allowed to age for 1 year. Unheated oils generally produce peroxide faster (for unheated maximum increase in 6-month is 2907 % from 1.351 to 40.627 but for heated maximum increase is 6574 % from 1.91 to 127.476). But they develop secondary oxidation products slowly (for unheated maximum increase in 6-month is 884 % from 1.553 to 15.29 but for heated maximum increase is 191 % from 6.42 to 18.72). For most oil heating in copper produce more p-anisidine value during ageing. The acid value of only unheated oils decreases between 6 months to 1 year. For the 1st six-month rate of increase in saponification value in unheated oil is much higher. The DPPH inhibition activity also changes differently. [ABSTRACT FROM AUTHOR]

Herein, a series of α -hydroxyalkyl phosphinic acids were designed and first introduced in Mn2+ extraction and Mn2+-Mg2+ separation. The extraction tests indicate that the α -hydroxy-2-ethylhexyl phosphinic acid (α -H-2-EHA) possesses superior extraction ability compared to di-2-ethylhexyl phosphinic acid (P204) for Mn2+ and Mg2+, and the partition coefficient (β) is 28.2 at a saponification ratio of 30%. The results of quantum chemical calculation, FT-IR spectrum and slope analysis method reveal that the α -H-2-EHA can form stable four-membered ring structure with metal ions during the extraction process through P–OH and P O bonds. Furthermore, the HOMO composition results suggest that α -OH might also promote the interaction between extractant and metal ions. Finally, a three-stage countercurrent extraction—washing—stripping process was proposed and Mn2+ can be enriched from 11.2 g/L to 36.6 g/L, with Mg2+ decreased from 30.3 g/L to 0.6 g/L, which provides an efficient strategy for the preparation of high-purity manganese. [Display omitted] • α -Hydroxyalkyl phosphinic acids were synthesized and first introduced as extractants. • The partition coefficient (β) of Mn2+ and Mg2+was 28.24. • An extraction—washing—stripping process was performed to separate Mn2+ from Mg2+. • α-H-2-EHA chelates with Mn2+ by forming a four-membered ring complex. [ABSTRACT FROM AUTHOR]

Traditional saponification methods lead to large amounts of alkali consumption and saline wastewater discharge. Herein, a novel saponification strategy was proposed via the extraction and reduction of Ce(IV) in nitrate solution. Several key parameters were investigated to explore the influence on extraction and reduction. The results showed that the concentration of NO 3 - and acidity had insignificant influence on the extraction, indicating that Ce(IV) could be effectively extracted without saponification even in highly acidic solution. The theoretical amount of H 2 O 2 was selected for the reduction process, and the corresponding reduction rate was nearly 99 %. The concentration of Ce(III) in the reductive organic phase was 0.15 mol/L, and the extraction rate of Yb(III) was up to 84.62 % for one-stage extraction. The extraction and reduction mechanisms were established using the slope method and FT-IR spectrometric analysis, and the complexes of the organic phase before and after reduction were determined. Based on the new saponification strategy and the circulation of Ce and nitrate, the alkali consumption and wastewater discharge would be avoided thoroughly. • A novel saponification strategy was proposed via the extraction and reduction of Ce(IV) in nitrate solution. • The reduction rate of 99 % was achieved when 100 % of theoretical amount of H 2 O 2 was added in organic phase. • Basing the new saponification technology, the alkali consumption and wastewater discharge would be avoided. • An integral extraction process was designed driven by the oxidation and reduction of Ce, for which only reductant and electric energy were consumed. [ABSTRACT FROM AUTHOR]

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.

Vitamin D and its analogues are fat-soluble vitamins that carry out important functions in human and animal organisms. Many studies have pointed out the relationship between the deficiency of these substances and the development of both skeletal- and extra-skeletal diseases. Although vitamin D is fundamentally derived from the bio-transformation of its precursor, 7-dehydrocholesterol, through the action of UV-B radiation in the skin, dietary intake also plays an important role in the regulation of its status in an organism. For this reason, the application of reliable methodologies that enable monitoring the content of vitamin D and its analogues in food and supplements constitutes an aspect of special relevance to establish adequate habits, which avoid the deficiency of these substances in organisms and, consequently, the appearance of related diseases. The use of chromatographic techniques in combination with conventional and novel sample pre-treatments has become a suitable strategy to achieve this aim. This review compiles the most relevant methodologies reported in the last ten years for vitamin D analogues analysis in food matrices. Particular attention has been paid to provide a general overview of the most suitable approaches in terms of reliability, sensitivity and simplicity, used in the field of food analysis.