Oily Matrix Research Articles

Oil-Based Curcuminoid Phospholipid Formulation Mimicking Natural Digestion Enhances Oral Bioavailability of Curcuminoids in Healthy Subjects.

Curcumin, the fat-soluble active ingredient and major compound of curcuminoids contained in the curcuma root, is known for its physiological low absorption and bioavailability. Various formulations and galenic technologies are currently available on the market. In this study, the product tested was provided as a soft gelatin capsule containing curcuminoids in an oily matrix mixed with phospholipids (oil/phospholipids [PL]-based, no new technologies applied or artificial excipients added). This was intended to improve bioavailability of curcuminoids as well as to mimic the natural digestion process of fat-soluble substances. In particular, the oral bioavailability of curcuminoids in the oil/PL-based formulation was compared with the pure curcuminoids extract alone (reference product), in a randomized, cross-over, single oral dose study design. Twelve healthy subjects were administered 200 mg curcuminoids under fasting conditions. Pharmacokinetic parameters were analyzed from individual concentration-time curves of total curcuminoids, as well as the curcumin metabolite tetrahydrocurcumin (THC). Results showed significantly higher AUC0-8h levels after the intake of the oil/PL-based formulation for total curcuminoids (205.60 vs. 112.50 ng/mL*h, P = .0001) as well as for THC (347.30 vs. 118.90 ng/mL*h, P < .0001) in comparison to the pure curcuminoids extract. Cmax was also significantly higher for both parameters analyzed (total curcuminoids: 47.54 vs. 21.16 ng/mL, P = .0001; THC: 96.69 vs. 29.83 ng/mL, P < .0001). In addition, the uptake kinetic of total curcuminoids was significantly fastened with the oil/PL-based curcuminoids formulation compared with the pure curcuminoids extract (P = .0446). These data suggest an improved impact on curcuminoids uptake of the oil/PL-based formulation and confirms its good tolerability.

Comprehensive analysis of vitamin D3 impurities in oily drug products using supercritical fluid chromatography-mass spectrometry.

Vitamin D3, an essential micronutrient, often requires supplementation via medicines or food supplements, which necessitate quality control (QC). This study presents the development of a method for detecting and quantifying seven impurities of vitamin D3 in oily drug products using supercritical fluid chromatography-mass spectrometry (SFC-MS). Targeted impurities include two esters of vitamin D3 and five non-esters including four that are isobaric to vitamin D3. Firstly, a screening study highlighted the Torus 1-AA column and acetonitrile modifier as adequate for the separation, followed by optimization of the SFC conditions. Secondly, make-up solvent composition and MS settings were optimized to reach high sensitivity. For both the separation and MS response, the screening design of experiments proved useful. Lastly, a fast saponification and liquid-liquid extraction method was developed, enabling efficient sample cleanup and impurities recovery from the complex oily matrix. The SFC-MS method suitability was assessed in two validation studies. The first study employed the ICH Q2 guideline for impurity limit test to demonstrate method specificity and establish a limit of detection (LOD) and a limit of quantification (LOQ) at 0.2% and 0.5%, respectively, for ester impurities. The second study conducted a comprehensive quantitative assessment for three non-ester impurities using a total error approach, determining method validity through accuracy profiles. The validated method exhibited reliable performance across impurity concentrations from 0.1% to 2.0%, with estimated LODs ranging from 2 to 7ng/mL. This study further promotes SFC-MS as a valuable, versatile, and green tool for routine pharmaceutical QC.

A polymeric-ceramic hybrid membrane with a self-cleaning and super-wettable surface decorated with polypyrrole-G-C3N4 photocatalyst for oily wastewater treatment

Treating oily wastewater is an enormous challenge as it leads to excessive membrane fouling due to the deposition of components of oily feed onto the membrane surface. Hence, the current work has been focused on developing a polymeric-ceramic hybrid membrane with photocatalytic self-cleaning antifouling properties. To yield the desired membrane, a polypyrrole-graphitic carbon nitride (PPy-G-C3N4) photocatalyst was decorated in the polyamide (PA) active layer of the membrane by interfacial polymerization (IP) onto the surface of alumina support. The chemistry of the active layer of the PPy-G-C3N4/PA@Alumina ceramic membrane led to the special wettability feature of being underwater superoleophobic which is reflected by underwater oil contact angle of θO, W = 159.9°. Even though the membrane surface features do not allow the oil to wet the membrane surface during filtration, the membrane surface fouling was inevitable during filtration experiments. With distilled water as feed, the permeate flux of PPy-G-C3N4/PA@Alumina ceramic membrane reached 650 L m−2 h−1 (LMH) at a pressure of 8 bar. A separation efficiency of >99 % was observed by using a feed of 100 ppm oil-in-water (O/W) emulsion. However, the permeate flux declined while using O/W emulsion as feed, where a 92 LMH to 50 LMH was observed after 60 min of continuous filtration. The performance of the membrane was recovered after exposure to solar-simulated light owing to the presence of PPy-G-C3N4 photocatalyst in the active layer where a recovery of ∼90 % of permeate flux was recorded. Hence, the current approach of fabricating a hybrid membrane proved to be useful for efficiently treating a challenging feed consisting of a complex oily matrix.

Combination of a solid phase extraction and a two-dimensional LC-UV method for the analysis of vitamin D3 and its isomers in olive oil

The current HPLC methods for the quantification of vitamin D3 (VitD3) and its two isomers previtamin D3 (PreVitD3) and trans-vitamin D3 (trans-VitD3) in olive oil preparations present some limitations mainly due to peak overlapping of the oily matrix components with the compounds of interest. The use of two-dimensional liquid chromatography (2D-LC) with different retention mechanism can reach higher resolving power thus allowing the analysis of complex samples.The present paper proposes a new alternative method including a solid phase extraction sample preparation step and a two-dimensional liquid chromatographic analysis using routine instrumentation, fitting the needs of quality assurance and quality control laboratories of pharmaceutical companies. The extraction protocol was demonstrated to provide a clean-up of the sample and a quantitative recovery of the species of interest. The 2D method proved its suitability in the isolation of vitamins from oil components in the first dimension and the separation and quantification of the analytes in the second dimension thanks to the orthogonal selectivities of phenyl and porous graphitic carbon (PGC) stationary phases.The method was validated following ICH guidelines and possesses an adequate sensitivity to quantify the impurity trans-VitD3 in pharmaceuticals considering the limits imposed by regulatory agencies. The applicability of the phenyl x PGC 2D-LC-UV method to quality control of medicinal products based on VitD3 in olive oil was confirmed by the successful quantification of vitamins in olive oil formulations.

Gas Chromatography-Mass Spectrometry Detection of Thymoquinone in Oil and Serum for Clinical Pharmacokinetic Studies.

Thymoquinone (TQ) is the primary component of Nigella sativa L. (NS) oil, which is renowned for its potent hepatoprotective effects attributed to its antioxidant, anti-fibrotic, anti-inflammatory, anti-carcinogenic, and both anti- and pro-apoptotic properties. The aim of this work was to establish a method of measuring TQ in serum in order to investigate the pharmacokinetics of TQ prior to a targeted therapeutic application. In the first step, a gas chromatography-mass spectrometry method for the detection and quantification of TQ in an oily matrix was established and validated according to European Medicines Agency (EMA) criteria. For the assessment of the clinical application, TQ concentrations in 19 oil preparations were determined. Second, two serum samples were spiked with TQ to determine the TQ concentration after deproteinization using toluene. Third, one healthy volunteer ingested 1 g and another one 3 g of a highly concentrated NS oil 30 and 60 min prior to blood sampling for the determination of serum TQ level. After the successful establishment and validation of the measurement method, the highest concentration of TQ (36.56 g/L) was found for a bottled NS oil product (No. 1). Since a capsule is more suitable for oral administration, the product with the third highest TQ concentration (No. 3: 24.39 g/L) was used for all further tests. In the serum samples spiked with TQ, the TQ concentration was reliably detectable in a range between 5 and 10 µg/mL. After oral intake of NS oil (No. 3), however, TQ and/or its derivatives were not detectable in human serum. This discrepancy in detecting TQ after spiking serum or following oral ingestion may be attributed to the instability of TQ in biomatrices as well as its strong protein binding properties. A pharmacokinetics study was therefore not viable. Studies on isotopically labeled TQ in an animal model are necessary to study the pharmacokinetics of TQ using alternative modalities.

Sonoprocessing of oil: Asphaltene declustering behind fine ultrasonic emulsions

Despite the transition toward carbon-free energy carriers, liquid fossil fuels are expected to occupy an important market share in the future. Therefore, it is crucial to develop innovative technology for better combustion reducing the emissions of pollutants associated with their utilization. Water in oil (w/o) emulsions contribute to greener combustion, increasing carbon efficiency and reducing emissions. Water content, emulsions stability, and droplet size distributions are key parameters in targeting the efficient use of emulsions as combustibles. In particular, for fixed water content, the finer the emulsion, the better its beneficial effect on combustion. In this work, two emulsions, mechanically and ultrasonically generated, were compared. Cryogenic scanning electron microscopy (cryo-SEM) allowed the visualization of water droplets inside the oily matrix. No surfactants were added to the oil, due to its high asphaltenic content. Asphaltene molecular aggregates, namely clusters, act as natural surfactants stabilizing the emulsions by arranging at w/o interface and forming a rigid film. The asphaltenic rigid film is clearly visualized in this work and compared for the two emulsions. The results showed finer water droplets in the ultrasonically generated emulsion, together with a reduction in the thickness of the asphaltenic film. Ultrasonically induced cavitation favored the de-clustering (breakage of intermolecular forces) of asphaltene molecules. Thus, smaller clusters allowed to stabilize smaller water droplets resulting in an ultra-fine emulsion, which improves the combustion performances of the fuel.

Cryptic Epoxytiglianes from the Kernels of the Blushwood Tree (Fontainea picrosperma).

The kernels of the Australian blushwood tree (Fontainea picrosperma) are the source of the veterinary anticancer drug tigilanol tiglate (2a, Stelfonta) and contain a concentration of phorboids significantly higher than croton oil, the only abundant source of these compounds previously known. The oily matrix of the blushwood kernels is composed of free fatty acids and not by glycerides as found in croton oil. By active partitioning, it was therefore possible to recover and characterize for the first time a cryptic tigliane fraction, that is, the diterpenoid fraction that, because of its lipophilicity, could not be obtained by solvent partition of crude extracts. The cryptic tigliane fraction accounted for ca. 30% of the tigliane kernel titer and was quantified by 1H NMR spectroscopy and profiled by HPLC-MS. Long-chain (linoleates and/or oleates) 20-acyl derivatives of the epoxytigliane diesters tigilanol tiglate (EBC-46, 2a), EBC-47 (4a), EBC-59 (5a), EBC-83 (6a), and EBC-177 (7a) were identified. By chemoselective acylation of EBC-46 (2a) and EBC-177 (7a) the natural triesters 2b and 7b and a selection of analogues were prepared to assist identification of the natural compounds. The presence of a free C-20 hydroxy group is a critical requirement for PKC activation by phorbol esters. The unexpected activity of 20-linoleoyl triester 2b in a cytotoxicity assay based on PKC activation was found to be related mainly to its hydrolysis to tigilanol tiglate (2a) under the prolonged conditions of the assay, while other esters were inactive. Significant differences between the esterification profile of the epoxytigliane di- and triesters exist in F. picrosperma, suggesting a precise, yet elusive, blueprint of acyl decoration for the tigliane polyol 5-hydroxyepoxyphorbol.

Role of yeasts in the qualitative structuring of extra virgin olive oil.

This review sought to describe the role played by some components of the microbiota of extra virgin olive oil (EVOO), particularly yeasts, in structuring the physicochemical and sensorial quality of freshly produced olive oil. Yeasts can survive during the entire storage period of the product. To date, approximately 25 yeast species isolated from oil produced in more than six countries have been identified, eight of which are classified as new species. Some yeast species improve the health qualities of oil, whereas many others improve the chemical composition and sensory characteristics based on β-glucosidase and esterase enzymes, which are involved in the hydrolysis of the bitter glucoside known as oleuropein. However, some species, which are typically favoured by the high water content in the oily matrix, such as lipase-producing yeasts, can worsen the initial chemical characteristics of EVOO oil during storage. Some physical treatments that are compatible with the EVOO production specification affect the biotic component of the oil by reducing the concentration of yeasts. The possibility of minimizing the invasive action on the biotic component of the oil by appropriately selecting the physical treatment for each oil is discussed.

QuEChERS Method Combined with Gas- and Liquid-Chromatography High Resolution Mass Spectrometry to Screen and Confirm 237 Pesticides and Metabolites in Cottonseed Hull

Cottonseed hull is a livestock feed with large daily consumption. If pesticide residues exceed the standard, it is easy for them to be introduced into the human body through the food chain, with potential harm to consumer health. A method for multi-residue analysis of 237 pesticides and their metabolites in cottonseed hull was developed by gas-chromatography and liquid-chromatography time-of-flight mass spectrometry (GC-QTOF/MS and LC-QTOF/MS). After being hydrated, a sample was extracted with 1% acetic acid in acetonitrile, then purified in a clean-up tube containing 400 mg MgSO4, 100 mg PSA, and 100 mg C18. The results showed that this method has a significant effect in removing co-extracts from the oily matrix. The screening detection limit (SDL) was in the range of 0.2–20 μg/kg, and the limit of quantification (LOQ) was in the range of 0.2–20 μg/kg. The recovery was verified at the spiked levels of 1-, 2-, and 10-times LOQ (n = 6), and the 237 pesticides were successfully verified. The percentages of pesticides with recovery in the range of 70–120% were 91.6%, 92.8%, and 94.5%, respectively, and the relative standard deviations (RSDs) of all pesticides were less than 20%. This method was successfully applied to the detection of real samples. Finally, this study effectively reduced the matrix effect of cottonseed hull, which provided necessary data support for the analysis of pesticide residues in oil crops.

Dispersion of bioactive substances in oils by supercritical antisolvent technology (BIOSAS process)

This work presents the novel method named BIOSAS to formulate homogenous dispersions of bioactive substances in an oily matrix. The method is based on the carbon dioxide supercritical antisolvent (SAS) technique to produce small drops of a solution containing the bioactive substances, in the presence of a lipid substance. Ethanolic and aqueous solutions were used to solubilize complex mixtures of phytochemicals depending on the polarity of compounds. Ethanol was removed entirely from the droplets by SAS effect, and solid bioactive particles with mean diameters below 1 μm were uniformly dispersed in the lipid matrix; for aqueous solutions, the water droplets produced were high-pressure mixed with the lipid phase containing an emulsifier, and stable emulsions were obtained. BIOSAS permits particle size control and can be used to formulate lipid-based nutraceuticals or food supplements in an inert atmosphere and at low temperatures, contributing to reducing the oxidation and thermal degradation of bioactive substances and lipid matrix.

CBD oils on the Belgian market: A validated MRM GC-MS/MS method for routine quality control using QuEChERS sample clean up

Quality control of CBD oils on the Belgium market showed that the CBD content not always corresponds to the label claim. There is a pressing need to develop new analytical methods specifically developed to the assay of such oily samples. Analytical issues are, however, encountered for routine analyses due to the matrix complexity, high cost of cannabinoid standards and low Δ9-THC concentrations. An oily matrix could cause technical damages to analytical instruments and reduce the lifetime of the chromatographic columns. This paper proposes a procedure combining a sample cleanup by QuEChERS, removing the oily matrix, followed by a validated MRM GC-MS/MS method for the routine analysis of CBD oil samples. Eighteen CBD samples were selected on the Belgium market for analysis. This method allows the quantification of CBD, the legality check for the Δ9-THC content by a CBN standard and the screening of seven other cannabinoids namely CBN, CBDV, CBT, CBC, Δ8-THC, THCV and CBG. The method was validated at three concentration levels (0.5–1–2% (w/v)) for CBD and (0.05–0.1–0.2% (w/v)) for CBN. The detection limits for CBT, CBD, CBC, Δ8-THC, CBN and for the other cannabinoids of interest, were 10 and 14 ng/mL respectively. The accuracy profile values for CBD and CBN showed that the β-expectation tolerance intervals did not exceed the acceptance limits of ± 20%, meaning that 90% of future measurements will be included within this error range.

Economical irregular silica as an effective dispersive solid-phase extraction sorbent for the quantification of calcitriol in soft capsules

Calcitriol is an active product of vitamin D produced by the liver and kidney hydroxylase metabolism with strong physiological activity. It is the preferred form of medicine for patients with insufficient bone mineralization due to chronic kidney disease. Calcitriol soft capsule is one of the common preparation forms, the main drug content of which is very low (1.55 μg g−1), and the pharmaceutical excipients interfere greatly, especially the oily matrix medium-chain triglycerides. Therefore, removing the interference of oily matrix is ​​the main challenge in the content determination. At present, the commonly used sample purification method for the determination of calcitriol in soft capsules is liquid-liquid extraction, but it usually consumes a lot of toxic organic solvents and it is costly. The adoption of SPE purification method, on the one hand, requires specific experimental equipment, and on the other hand, the organic solvent used in the experiment may cause the dissolution of SPE column tube materials, which will interfere with the subsequent detection. Herein, in order to achieve a cost-effective and reliable determination of calcitriol soft capsule content, we developed a dispersive solid-phase (DSPE) extraction method that directly uses irregular silica as sorbent, which is followed by high-performance liquid chromatography equipped with a UV detector(HPLC-UV)analysis. Selective retention of calcitriol is achieved by the polar interaction between calcitriol and silica, what’s more, sufficient contact between washing solvent and sorbent can be guaranteed. Therefore, after pretreatment with DSPE, the interference of oily matrix on detection can be mostly removed and then improve the accuracy of the method compared to the SPE method. Under the optimal conditions of DSPE, calcitriol showed a good linear relationship in the range of 0.15−2.99 μg g−1, the R2 was 0.997. Satisfactory recoveries ranging from 101.1%–102.0% for calcitriol were achieved in the oily matrix at the levels of 0.75, 1.50 and 2.24 μg g−1. And the intra-day and inter-day RSD were less than 2.5 % and 3.2 %. Meanwhile, the LOD and LOQ of calcitriol was 0.01 μg g−1 and 0.02 μg g−1, which is in full compliance with the regulatory level fixed by the EU, China or other countries. This method was further verified to determine the content of calcitriol in commercial calcitriol soft capsules and the recoveries of three batches of products was 86.2 %–94.4 %. Based on these characteristics, the proposed method makes it possible to determine the low content of weakly polar drugs in the oily matrix in a simple, low-cost and reliable way.

Ethanol-extraction SERS strategy for highly sensitive detection of poisons in oily matrix

The sensitive detection and identification of toxicants in oily matrices have suffered from difficulty in poisoning incidents, therefore it is necessary to develop the rapid and efficient analytical method to realize the on-site screening and analyzing. In this report, the surface-enhanced Raman spectroscopy (SERS) method was used to detect paraquat and diquat poisons in various oily matrix coupled with solvent extraction. The solvent extraction not only remove interfering impurities of oily substrates, but also can enrich and separate the poisons from oily matrix. It was demonstrated that the ethanol as the extractant was suitable for the rapid separation of poisons such as paraquat (PQ) and diquat (DQ) in oily matrix (soy sauce, pasta sauce, sesame oil, chili oil). Moreover, combined with a handheld Raman spectrometer, the entire detection process was completed within 8 min with the level of 10 ppb PQ and 100 ppb DQ. Furthermore, double-blind experiments verify the reliability of this method. The results demonstrate that this rapid and convenient method could be used for the effective enrichment and sensitive detection of poisons in several oily matrix and has the grate potential application in emergency response and public safety.

Analyses of used engine oils via atomic spectroscopy – Influence of sample pre-treatment and machine learning for engine type classification and lifetime assessment

The analysis of used engine oils from industrial engines enables the study of engine wear and oil degradation in order to evaluate the necessity of oil changes. As the matrix composition of an engine oil strongly depends on its intended application, meaningful diagnostic oil analyses bear considerable challenges. Owing to the broad spectrum of available oil matrices, we have evaluated the applicability of using an internal standard and/or preceding sample digestion for elemental analysis of used engine oils via inductively coupled plasma optical emission spectroscopy (ICP OES). Elements originating from both wear particles and additives as well as particle size influence could be clearly recognized by their distinct digestion behaviour. While a precise determination of most wear elements can be achieved in oily matrix, the measurement of additives is performed preferably after sample digestion. Considering a dataset of physicochemical parameters and elemental composition for several hundred used engine oils, we have further investigated the feasibility of predicting the identity and overall condition of an unknown combustion engine using the machine learning system XGBoost. A maximum accuracy of 89.6% in predicting the engine type was achieved, a mean error of less than 10% of the observed timeframe in predicting the oil running time and even less than 4% for the total engine running time, based purely on common oil check data. Furthermore, obstacles and possibilities to improve the performance of the machine learning models were analysed and the factors that enabled the prediction were explored with SHapley Additive exPlanation (SHAP). Our results demonstrate that both the identification of an unknown engine as well as a lifetime assessment can be performed for a first estimation of the actual sample without requiring meticulous documentation.

A novel vortex assisted dispersive solid phase extraction of some trace elements in essential oils and fish oil

In this paper, a novel vortex assisted solid phase extraction procedure combined with inductively coupled plasma optic emission spectrometry was presented for determination of Mn, Cu, Ni, Cr, Cd and Pb directly in oily matrix. The suggested separation and preconcentration method was based on simultaneous sorption of the target analytes from real essential oil matrix onto γ-Al2O3 functionalized with fluorescein (Al-Flr) and transfer to aqueous eluent prior to quantification. The effect of different parameters including sorption and elution time, sample volume, eluent type and concentration and interfering ions were investigated. The working conditions were given as follows, vortex agitation for sorption and elution 40 s, sample volume 20 mL, eluent type HCl, eluent concentration 0.3 mol L−1. The detection limits were found to be 0.7 μg L−1 for Mn, 4.1 μg L−1 for Cu, 1.0 μg L−1 for Ni, 1.6 μg L−1 for Cr, 0.7 μg L−1 Cd and 1.0 μg L−1 Pb. The evaluation of the accuracy and precision of the method was tested via metallo-organic certified reference material. The recovery values have warranted the accuracy and found between 98.4 and 103.3% with 2.6–6.4% relative standard deviation (RSD, %). The sampling frequency of the procedure was calculated as 11.25 h−1.Finally, the proposed analytical method was successfully applied on analyte spiked and unspiked apricot, black cumin, pine turpentine, thyme, mint essential oils and fish oil samples without any need of performing mineralization pretreatments.

Design of Experiment Centered Multivariate Optimization Strategy for RP-HPLC Method to Quantitate Retapamulin in Topical Cream and Microemulsion

Background: Retapamulin is the first pleuromutilin antibacterial approved for the treatment of impetigo. The objective of the current research was to utilize the design of experiments approach for development and optimization of robust RP-HPLC method for the quantitation of Retapamulin in marketed cream and in-house developed microemulsion based formulations with an oily matrix. Methods: The impact of various chromatographic conditions (independent variables) was assessed using Plackett–Burman design on critical analytical attributes (response) to screen initial experimental conditions. The Box-Behnken design was employed to optimize the selected chromatographic factors on the responses. Further, validation of optimized RP-HPLC was carried out as per the ICHQ2(R1) guideline. Results: Pareto ranking analysis showed that % organic phase, flow rate, and volume of injection were found statistically significant (p &lt; 0.05) variables influencing the retention time, number of plates, and tailing of the Retapamulin peak. The optimized RP-HPLC method with the stationary phase, C18 (250 mm × 4.6 mm, 5 μm) column, and mobile phase as a mixture of methanol and potassium dihydrogen orthophosphate buffer (50 mM, pH 7.0, 90:10 % v/v, isocratic), the flow rate of 1.0 mL/min, 10 μL injection volume, 25°C column oven temperature, 247 nm as detection wavelength, was successfully validated based on ICHQ2(R1) guideline. Conclusion: RP-HPLC method was successfully used to separate (retention time 4.34 ± 0.2 min)and assay Retapamulin in microemulsion and marketed cream. The outcomes of the investigation exhibited the effective application of a multivariant approach in the optimization of the RP-HPLCfor routine analysis of Retapamulin.

Development of an Efficient Extraction Method for Separating Solasodine, an Steroidal Alkaloid, From an Oily Matrix: A Comparison Between LLE and SPE

Aims: In many references of Traditional Iranian Medicine (TIM), there are methods to produce medicinal products from plant fruit based on extraction of active substances into oils. One of these recommendations is to import cucurbit or pumpkin seed oil into an entirely ripe fruit of Solanum melongena plant. In this study for the first time, the extraction of solasodine from the oily matrix has been investigated to find a precise method with suitable extraction recovery.&#x0D; Study Design: Original Research Article.&#x0D; Place and Duration of Study: The study took place in herbal and traditional medicines research center of Kerman, Iran from February 2015 to November 2017.&#x0D; Methodology: Solasodine, an active steroidal alkaloid metabolite of the plant, was used for standardization of the product. Two methods of (Liquid-liquid extraction) LLE and (Solid phase extraction) SPE were evaluated and their conditions were optimized by assessment of seven effective factors at five levels using HPLC as the method of choice for solasodine determination.&#x0D; Results: Results showed that LLE and SPE in optimized conditions had recoveries of about 76.5 and 94.7%, respectively. For the extraction of low concentrations of the analyte, the SPE method had better accuracies (88 to 105%), but its precision was less than that of LLE method. In contrast, the LLE method had a higher precision in the whole range while its relevant accuracy was lower. The LOD and LOQ of SPE-HPLC method were 0.2 and 0.6 μg/ml and those of the LLE-HPLC method were 0.2 and 0.7 μg/ml, respectively.&#x0D; Conclusion: In general, both methods of LLE-HPLC and SPE-HPLC showed acceptable validation parameters including linearity, precision, accuracy, LOD, and LOQ; and they can be used for routine extraction and determination of solasodine in traditional medicine products.

Assessment of the moisturizing properties of a magnetic mask containing iron oxide particles.

Moisturizer is an important component of many cosmetic products. It helps to maintain the skin's integrity and its barrier functions. Recently, magnetic masks that seek to improve the properties of the skin have been developed and have become a new cosmetic trend. However, scientific proof of their stated properties is lacking. To test whether iron oxide contained in a face mask with magnetic properties in an oily matrix with a freeze-dried aloe-vera base increases moisturization of the skin and improves skin barrier function. Formulations were prepared containing an oil phase (67.3% wt.) and a solid phase (32.7% wt.). The moisturizing properties of the mask were tested by measuring in vivo electrochemical impedance spectroscopy, contact angle, and visual appearance. Meanwhile, human panel tests were performed to evaluate the sensory perception of potential users. The moisturizing effect of the iron oxide mask is clearly superior to that of the other tested samples. Water retention and low transepidermal water loss (TEWL) were evidenced for the iron oxide magnetic mask. Its occlusive action on the skin resulted in larger water contact angles and enhances the barrier effect. A favorable sensory perception on the part of the users was obtained for the iron oxide magnetic mask. The presence of iron oxide and the magnetic property of the mask enhance occlusive behavior, diminishing the TEWL. Sensory analysis of the iron oxide magnetic mask performed by human panel tests shows that they possess characteristics including neutral odor, and easy, pleasant-feeling application.

Changes of Properties of Bitumen Binders by Additives Application

Requirements for properties of bituminous binders are determined in the European standards. The physico-chemical behaviour of bitumen depends on its colloidal structure (asphaltenes dispersed into an oily matrix constituted by saturates, aromatics and resins) that depends primarily on its crude source and processing. Bitumen properties are evaluated by group composition, elementary analysis, but more often conventional or functional tests. Bitumen for road uses is assessed according to the physical characteristics. For the purpose of improving the qualitative properties of bitumen and asphalts the additives are applied e.g. to increase elasticity, improving the heat stability, improving adhesion to aggregate, to decrease viscosity, increasing the resistance to aging, to prevent binder drainage from the aggregate surface, etc. The objective of presented paper is to assess and compare effect of additives on properties of bitumen binders. In paper, the results of bitumen properties, penetration, softening point, and dynamic viscosity of two paving grade bitumen 35/50, 50/70 and polymer modified bitumen PmB 45/80-75 are analyzed and also the changes of these properties by the application of selected additives (Sasobit, Licomont BS100, Wetfix BE and CWM) to improve adhesion to aggregate and improve workability. Measurements of properties have been performed according to the relevant European standards. The laboratory tests showed significantly increasing the softening point of paving grade bitumen 50/70 and 35/50 by 13 to 45°C. The effect of various additives on bitumen softening point is different. Penetration varies according to type of bitumen and type of used additive. The penetration values of modified bitumen PmB 45/80-75 with additives Sasobit and Licomont BS100 show increase of bitumen stiffness of 16 0.1mm and a shift in the gradation. The changes in penetration and in softening point significantly shown when calculating on Penetration index as a parameter of temperature susceptibility. The additives changed the viscosity of bitumen to lower values mostly with modified bitumen. In case of the additive Wetfix BE mix in 35/50caused the viscosity increase. The additive changes the properties of original bituminous binders, and that can affect the properties of asphalt mixtures and asphalt layers.

Effect of an olive phenolic extract added to the oily phase of a tomato sauce, on the preservation of phenols and carotenoids during domestic cooking

The protective effect of a phenolic extract from olive vegetation water on carotenoids and other phytonutrients has been evaluated during a home-cooking procedure to prepare tomato sauce. To specifically investigate on the complex mechanisms involved in the thermal degradation and solubilization of carotenoids, the olive phenols were added to a refined olive oil, chosen as control fat, in order to distinguish the effect of the simple oily matrix from that of the phenols occurring in virgin olive oils.Three sauces were prepared using a commercial tomato “passata”, carrots, celery and onion. Two sauces contained refined olive oil to which was added a phenolic extract at 40 or 60 mg/100 g of polyphenols, the third was the control with refined olive oil. The results revealed positive effect of the phenolic extract on the phytonutrient content of the tomato sauce. In the experimental sauces for the hydrophilic phenols, an improvement of approximately 100% was observed at both levels of phenolic extract addition in comparison to the control. There was a greater than 50% increase in a-tocopherol and a 43% increase in carotenoids with the lower level of phenols addition, and greater than 58% with the higher level of enrichment.