Extraction Solvent Research Articles

The Effect of Various Extraction Methods and Solvents on the Phytochemical Contents and Antioxidant Capacities of Safflower Florets (Carthamus Tinctorius L.) from South Sulawesi

Safflower is a traditional medicine commonly applied for the treatment of varicella in South Sulawesi. The aim of this study is to study the effect of extraction methods and solvents on phytochemical content and antioxidant capacity in the extraction of safflower. The study began with sample extraction with various solvents, i.e., water, ethanol 70, methanol, ethyl acetate and hexane and various methods, i.e., reflux, Soxhlet, hot maceration, cold maceration and room temperature maceration. Each extract was standardized for its phytochemical content, i.e., phenolics, flavonoids and carotenoids and the antioxidant capacities were also determined by the radical scavenging 2,2-diphenyl-1-picrylhydrazyl, total antioxidant capacity, cupric ion reducing antioxidant capacity and Ferric reducing antioxidant power. The results indicated that the optimum total phenolic content was obtained when the florets were refluxed with methanol, flavonoids were refluxed with 70 % ethanol and carotenoids were Soxhleted with methanol. The research data also showed that 70 % ethanol and methanol have maximal antioxidant capacity. The results conclude that 70 % ethanol and methanol as solvents have the potential to extract the highest levels of phytochemical content and antioxidant substances. HIGHLIGHTS The phytochemical content and antioxidant capacity of safflower floret extract are influenced by the selection of solvent and extraction method. Polar solvents (70 % ethanol or methanol) can efficiently extract higher levels of phytochemical components and antioxidant substances from safflower florets. The hot extraction approach exhibits a higher potential for extracting phytochemical content compared to the cold extraction method, but its antioxidant capacity exhibits the opposite. The application of cold maceration, combined with methanol or 70 % ethanol as solvents, has been identified as a promising method for the extraction of phytochemical compounds and antioxidant substances. GRAPHICAL ABSTRACT

Ultrasound-Assisted Extraction of Phenolic Compounds from Celtuce (Lactuca sativa var. augustana) Leaves Using Natural Deep Eutectic Solvents (NADES): Process Optimization and Extraction Mechanism Research.

Natural deep eutectic solvents (NADESs), as emerging green solvents, can efficiently extract natural products from natural resources. However, studies on the extraction of phenolic compounds from celtuce (Lactuca sativa var. augustana) leaves (CLs) by NADESs are still lacking. This study screened the NADES L-proline-lactic acid (Pr-LA), combined it with ultrasound-assisted extraction (UAE) to extract phenolic compounds from CLs, and conducted a comparative study on the extraction effect with traditional extraction solvents. Both SEM and FT-IR confirmed that Pr-LA can enhance the degree of fragmentation of cell structures and improve the extraction rate of phenolic compounds. Molecular dynamics simulation results show that Pr-LA can improve the solubility of phenolic compounds and has stronger hydrogen bonds and van der Waals interactions with phenolic compounds. Single-factor and Box-Behnken experiments optimized the process parameters for the extraction of phenolic compounds from CLs. The second-order kinetic model describes the extraction process of phenolic compounds from CLs under optimal process parameters and provides theoretical guidance for actual industrial production. This study not only provides an efficient and green method for extracting phenolic compounds from CLs but also clarifies the mechanism of improved extraction efficiency, which provides a basis for research on the NADES extraction mechanism.

Hydrophobic deep eutectic solvent-based vortex-assisted dispersive liquid–liquid microextraction with UV–visible spectrophotometry for copper determination in waste printed circuit boards

ABSTRACT Nearly all electronic devices utilise Printed Circuit Boards (PCBs), which contribute significantly to the generation of electronic waste (e-waste). They are rich in metal content, with copper being present in higher percentages. In this work, a simple, efficient and environment-friendly pre-concentration technique was developed, using hydrophobic deep eutectic solvent as an extractant in vortex-assisted dispersive liquid–liquid microextraction. This pre-concentration technique is coupled with spectrophotometry for the determination of copper in PCBs. The complexing agent, sodium diethyl di-thiocarbamate (DDTC), and copper formed a complex in the 2–3 pH range. The Cu-DDTC complex was vortexed for 1 min at 2800 rpm to extract in hydrophobic DES. The sediment was analysed using a UV–Visible spectrophotometer at λ max 435 nm. The optimisation parameters, including pH, extraction solvent selection and its volume, concentration and volume of chelating agent, interference of forein ios, etc., have been assessed. Analytical figures of merit such as limit of detection (1.98 μg/L), limit of quantification (5.9 μg/L), relative standard deviation (3.4%) and enrichment factor (10) have been obtained under optimal experimental conditions. The method was validated by a certified copper solution and applied successfully to determine copper in waste PCBs of personal computers.

Optimization of Extraction Solvents on the Antioxidant Properties of Coconut Waste

Cocos nucifera L. (family Arecaceae) commonly known as coconut is considered as an important fruit crop in tropical countries and are widely used for therapeutic and domestic purpose. They have effective properties such as antioxidant, antitumor, antiseptic and antimicrobial. The growing demand for green coconut water consumption and food industries cause the dumping of the shell and husk of this fruit, generating large amount of solid waste. This study utilized part of coconut waste to study the impacts of solvent type on the phenolic content. Six different polarities of solvent were chosen. Total phenolic content was performed using Folin-Ciocalteu assay and free radical scavenging activity with 2,2-diphenyl-1-picrilhydrazil (DPPH) method. Total phenolic content for coconut shell was the highest at 71.57 ± 0.275 mg GAE/g for propanol extract and 74.10 ± 0.741 mg GAE/g for acetone extract of coconut husk. The antioxidant activity of all sample extracts was analysed using DPPH assay. Highest radical scavenging activity of coconut husk was observed by propanol extract with 93.82 ± 0.052 % while the lowest scavenging activity was demonstrated by chloroform extract with percentage of 57.77 ± 2.255%. Acetone extract of the shell exhibited the highest scavenging activity of 91.23 ± 0.073%, while chloroform extract of coconut shell demonstrated the lowest antioxidant activity of 70.627 ± 0.467%.

Separation and Detection of Catechins and Epicatechins in Shanxi Aged Vinegar Using Solid-Phase Extraction and Hydrophobic Deep Eutectic Solvents Combined with HPLC.

This research presents a new, eco-friendly, and swift method combining solid-phase extraction and hydrophobic deep eutectic solvents (DES) with high-performance liquid chromatography (SPE-DES-HPLC) for extracting and quantifying catechin and epicatechin in Shanxi aged vinegar (SAV). The parameters, such as the elution solvent type, the XAD-2 macroporous resin dosage, the DES ratio, the DES volume, the adsorption time, and the desorption time, were optimized via a one-way experiment. A central composite design using the Box-Behnken methodology was employed to investigate the effects of various factors, including 17 experimental runs and the construction of three-dimensional response surface plots to identify the optimal conditions. The results show that the optimal conditions were an HDES (tetraethylammonium chloride and octanoic acid) ratio of 1:3, an XAD-2 macroporous resin dosage of 188 mg, and an adsorption time of 11 min. Under these optimal conditions, the coefficients of determination of the method were greater than or equal to 0.9917, the precision was less than 5%, and the recoveries ranged from 98.8% to 118.8%. The environmentally friendly nature of the analytical process and sample preparation was assessed via the Analytical Eco-Scale and AGREE, demonstrating that this method is a practical and eco-friendly alternative to conventional determination techniques. In summary, this innovative approach offers a solid foundation for the assessment of flavanol compounds present in SAV samples.

Optimization of Desulfurization Process via Choline Phosphotungstate Coupled with Persulfate Using Response Surface Methodology

Using a simple acid-base neutralization method, a Ch-PW solid catalyst was synthesized by mixing choline hydroxide (ChOH) and phosphotungstic acid (HPW) at a 2:1 molar ratio in an aqueous solution. This catalyst was combined with a 20 wt.% potassium peroxymonosulfate (PMS) solution, using acetonitrile (ACN) as the extraction solvent to create an extraction catalytic oxidative desulfurization system. The optimal desulfurization conditions were determined through response surface methodology, targeting the highest desulfurization rate: 0.99 g of Ch-PW, 1.07 g of PMS, 2.5 g of extraction solvent, at a temperature of 50.48 °C. The predicted desulfurization rate was 90.79%, compared to an experimental rate of 93.64%, with a deviation of 3.04%. A quadratic model correlating the desulfurization rate with the four conditions was developed and validated using ANOVA, which also quantified the impact of each factor on the desulfurization rate: PMS > ACN > Ch-PW > temperature. GC-MS analysis identified the main oxidation product as DBTO2, and the mechanism of desulfurization in this system was further explored.

Oil produced from Ghana Shea Nut crop for prospective industrial applications

Though little research has been done, shea nut oil (Shea Butter), is a promising shea product with great potential for use in industrial shea product manufacture. To assess the oil obtained from the shea nuts for personal, commercial, and industrial use, this study focuses on the extraction process, the optimal solvent for extraction, thermodynamics and kinetic studies, and characterization of the oil. Using different solvents as well as extraction temperatures and times, the oil was extracted using the solvent extraction method. Moreover, models of thermodynamics and kinetics were used in examining the Shea nut oil extraction at different durations and temperatures. At the highest temperature of 333 K (at 130min), the highest oil yields of 70.2 % and 59.9 % for n-hexane and petroleum ether, respectively, were obtained, following first order kinetics. For both petroleum ether and n-hexane, the regression coefficient (R2) was 1. For the extraction with n-hexane and petroleum ether, the mass transfer coefficient (Km), activation energy (Ea), entropy change (ΔS), enthalpy change (ΔH), and Gibb's free energy (ΔG) were, respectively, (0.0098 ± 0.0061 and 0.0123 ± 0.0084) min−1, 74.59 kJ mol−1 and 88.65 kJ mol−1, (−236.15 ± 0.16 and −235.63 ± 0.17) J/mol K, (71.88 ± 0.06 and 85.94 ± 0.06) kJ/mol, and (148.75 ± 1.52 and 162.46 ± 1.52) kJ/mol. These values favor an irreversible, forward, endothermic, and spontaneous process. Gas chromatography analysis was used to identify the principal fatty acids in the oil, which include stearic acid (52 %), oleic acid (30 %), and linoleic acid (3 %), as well as various minor fatty acids. The oil's potential bonds and functional groups were identified using Fourier Transform Infrared analysis, and the physicochemical parameters such as the iodine value, peroxide value, acid and free fatty acid values were found to be within acceptable ranges for use in domestic, commercial, and industrial settings.

A simple and green offline-online capillary electrophoresis stacking strategy for the simultaneous determination of hydrophobic compounds in complicated samples using sodium dodecyl sulfate as the solubilizer and pseudophase

BackgroundCapillary electrophoresis is a powerful analytical method featured with high separation efficiency, minimal sample requirements, and reduced organic solvents consumption. However, its low sensitivity hinders its wide application in determination of trace analytes especially for the weakly ionized hydrophobic compounds. Offline and Online capillary electrophoresis stacking methods are more favored to enhance detection sensitivity of analytes. The determination of two sesquiterpenes and an alkaloid from the dried root of Lindera aggregata merged as an example for developing a simple, sensitive and green method for the simultaneous determination of two hydrophobic compounds in complicated matrix samples. ResultsAn offline-online capillary electrophoresis stacking strategy by integrating micro matrix solid phase dispersion with field-amplified sample stacking and micelle to cyclodextrin stacking has been developed for the simultaneous determination of dehydrocostus lactone, linderane, norisoboldine in complex matrices. The optimized parameters were set at 65 mM sodium dihydrogen phosphate, 35 % methanol, 180 s for sample injection and 210 s for cyclodextrin injection, 20 mM sodium dodecyl sulfate of sample matrix for online stacking; 1:1 sample to MCM-48, 180 s grinding time, and 1000 μL of 20 mM sodium dodecyl sulfate elution for offline procedure. Under the optimum conditions, the method showed good linearity with correlation coefficients (R2 ≥ 0.9927), low limits of detection within the range of 25–50 ng mL−1, satisfactory repeatability and reproducibility below 3.98 %, and acceptable recoveries between 94 % and 97 %. The developed method was successfully applied to two real samples, the root of L. aggregata and rat feces. SignificanceSodium dodecyl sulfate is firstly used as an eluent in micro matrix solid phase dispersion and plays a dual role throughout the analytical procedure, including extraction solvent in sample preparation and micelle pseudophase during online stacking. It brings great procedure convenience to the method. The sensitivity of this method can improve up to 1283-folds compared with the normal mode. Moreover, the overall strategy indicates satisfied green potential evaluated by greenness assessment tools.

Extraction of ofloxacin from water using hydrophobic eutectic solvents

Wastewater treatment plants do not cope well with emerging micropollutants, such as pharmaceuticals, because they are not effective to remove them. Therefore, this work aims to develop a process for the extraction of ofloxacin (OFX) based on a liquid-liquid extraction using hydrophobic eutectic solvents (HES), coupled with the Conductor-like Screening Model for Real Solvent (COSMO-RS) for solvent screening. First, COSMO-RS was used to predict the partition coefficient of OFX for four HES families: L-menthol: fatty acid, L-menthol: fatty alcohol, fatty acid: fatty acid and fatty acid: fatty alcohols, at three different molar ratios (2:1, 1:1, and 1:2). These results showed that HES formed by fatty acids, especially those with a longer alkyl chain and a higher fatty acid molar ratio, were the most suitable solvents for OFX extraction. Then, the most promising HES to extract OFX was evaluated experimentally. The HES decanoic acid: dodecanoic acid (C10 acid: C12 acid) in a molar ratio of 2:1 being the system with best extraction results of OFX was selected to optimize the extraction conditions of OFX, namely pH, HES: water ratio (v/v), and OFX concentration, using a response surface methodology (RSM). The results obtained showed that at a pH of 5.2, HES-water ratio (v/v) of 1.3, and 2.5 mg/ml of OFX that an extraction efficiency of OFX of (98.8 ± 0.9)% could be achieved. The results show that one-step OFX extraction is possible, but is significantly influenced by both the extraction parameters and the hydrophobic properties of the HES.

Eremostachys laevigata Bunge responses to different extraction solvents and methods: physiological, biochemical, and antibacterial attributes

This study examined the biochemical composition of Eremostachys laevigata Bunge's aerial and underground organs using various solvents (methanol, water, N-hexane, chloroform, and acetone) and their impact on antibacterial activity against eight bacterial strains (Escherichia coli, Staphylococcus aureus, Salmonella enterica, Pseudomonas aeruginosa, Klebsiella pneumoniae, Shigella dysenteriae, Proteus mirabilis, and Bacillus cereus). Soxhlet and maceration extraction methods were used, and the minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) were determined using the tube dilution method. The study found that N-Hexane and water solvents had the highest total phenol content, while methanol, acetone, and chloroform had the lowest. Additionally, N-Hexane and methanol solvents showed the highest and lowest flavonoid content, respectively. The methanol extract from underground organs using the Soxhlet method exhibited the strongest antibacterial activity, whereas the acetone extract showed the weakest antimicrobial effect. Staphylococcus aureus displayed both the MIC and MBC, and Salmonella enterica showed the highest susceptibility to the well diffusion method, while both Escherichia coli and Staphylococcus aureus were highly susceptible to the disk diffusion method. The underground organs contained 6.87 mg.g-1 of phenolic compounds and 0.19 mg.g-1 of flavonoids. Two iridoid glycosides, pholoyoside and sesamoside, were separated from the methanol extract of the underground organs using reversed-phase HPLC. The research highlights E. laevigata Bunge's potential as a natural reservoir of antimicrobial compounds, with phenolic and flavonoid compounds, along with iridoid glycosides, presumed to contribute to its antibacterial properties.

Miniaturized matrix solid-phase dispersion assisted by deep eutectic solvent for acrylamide determination in bread samples.

Acrylamide determination is important to state its quantity in baked food preventing any potential carcinogenic effects. Matrix solid-phase dispersion (MSPD) extraction is an extraction procedure based on a homogenization phase between a solid sample and a solid dispersing material to break sample increasing analyte extraction yield, often used for acrylamide determination. The addition of a green deep eutectic solvent (DES) during the MSPD homogenization phase improves the analyte extraction, giving the possibility to reduce the amount of organic solvent used. In this work, a miniaturized MSPD extraction assisted by a DES was developed to determine acrylamide in bread, using high-performance liquid chromatography coupled with mass spectrometry detection. The optimized procedure provides 1:1 (w/w) matrix-to-dispersing material ratio, 2mL of methanol as extraction solvent, and 50 μL of choline chloride-glycerol DES added during the homogenization phase. Method validation ensured good results with minimum recoveries of 90%, high precision with a maximum intra-day error of 4%, and inter-day error of 6%. Limit of detection and limit of quantification resulted to be 16μg/kg and 35μg/kg, respectively. This miniaturized extraction procedure represents a good alternative to those reported in the literature, guaranteeing great performance and respecting green chemistry principles.

Choline chloride-L-lactic acid mixtures as solvents for extraction of Coumarin from cinnamon-containing foods

The determination of coumarin in generally available cinnamon-containing foods such as biscuits, cereals is important to ensure that the populations consuming these foods more frequently are not exposed to higher levels and are not at risk. This study describes the development of an analytical method for determination of coumarin in foods containing cinnamon. Solid-liquid phase extraction with conventional stirring-assisted and ultrasound-assisted extraction (UAE) procedures were used to prepare sample extracts for liquid chromatography analysis. The green solvent, a mixture of choline chloride:L-lactic acid (1:4, mol/mol)/water (50:50 v/v), as a deep eutectic solvent-like mixture, was selected as an extraction solvent. The extraction conditions were optimized by using the design of the experiment strategy obtaining parameters, temperature 47 °C, time 36 min, solvent volume 4 mL, sample amount 0.8 g, stirring speed 20 rpm for rotary stirring-assisted extraction procedure, and temperature 30 °C, time 5 min, solvent volume 3.5 mL, sample amount 0.8 g for UAE. High-performance liquid chromatography separation with a total analysis time of 12 min was performed with a stationary phase of octadecyl type and a gradient of mobile phase of methanol-1 % acetic acid. The methods were successfully validated to show the detection limit of 0.13 μg.mL−1, the linearity range of 0.4–50 µg.mL−1 (R2 = 0.999), recovery values more than 80 %, and the RSDs of less than 7 %. Rotary stirring-assisted extraction showed moderately higher recovery values than UAE, while lower RSD % was observed for UAE.

Development and application of a protocol for extractables profiling from central venous catheters in neonates

Peripherally inserted central catheters (PICC-lines) used in neonatology are made of thermoplastic polyurethane (TPU) or silicone. These materials usually contain substances that may leach into drug vehicles or blood. In this extractables study, we determined the optimal extraction conditions using TPU films containing defined amounts of butylhydroxytoluene (BHT) and then applied them on unused and explanted PICC-lines. Maceration and sonication tests were carried out with hexane, acetone and water as the extraction solvents. The analyses were performed using gas and liquid chromatography coupled with mass spectrometry detectors, as well as inductive coupled plasma optical emission spectroscopy to detect a wide range of extractables. We selected a limited list of substances to be sought from the usual adjuvants and monomers, related to their carcinogenic, mutagenic or reprotoxic properties and/or existence in endocrine disruptors lists. The TPU-film experiments showed that acetone was slightly better than hexane, and maceration better than sonication. When applied to PICC-lines, the extraction methods were almost similar but acetone was clearly better than hexane for TPU. From the 48 peaks initially observed in GC-MS, we ended up with 37 peaks to follow in TPU PICC-lines, among which were those of BHT and 4,4′-Methylenebis(cyclohexyl isocyanate) isomers. For silicone PICC-lines, out of 41 peaks initially observed in GC-MS, we followed 20 peaks, most of them being identified as cyclosiloxanes. Barium was the main inorganic element extracted for both PICC-lines. For TPU PICC-lines, the inter-batch variability was higher than for intra-batch, but in silicone devices both were similar. When compared to new PICC-lines, explanted TPU PICC-lines extracted peaks had a lower area under the curve (AUC), while the AUCs of the peaks were higher for the majority of silicone PICC-lines extract compounds. No identified substances were detected above their toxicological threshold, but isocyanates and cyclosiloxanes toxicity was mostly studied for other exposition routes than intravenous. The methods defined in this study were efficient in producing extractable profiles from both PICC-lines.

Aqueous Solution of Ionic Liquid Is an Efficient Substituting Solvent System for the Extraction of Alginate from Sargassum tenerrimum

Three ionic liquids (ILs) and three deep eutectic solvents (DESs) with identical counterparts, as well as their aqueous solutions, were prepared for the selective extraction of alginate from Sargassum tenerrimum, a brown seaweed. It was found that the ILs and their hydrated systems were only able to extract alginate from the seaweed directly, while the DESs were not, as confirmed by molecular docking studies. When the quality of the polysaccharide was compared to that produced using the hydrated IL system with the widely used conventional method, it was discovered that the physicochemical and rheological characteristics of the alginate produced using the ILs as solvents were on par with those produced using the conventional method. The ILs can be seen as acceptable alternative solvents for the simple extraction of the polysaccharide straight from the seaweed given the consistency of the extraction procedure used in conventional extraction processes. The hydrated ILs were discovered to be more effective than their non-hydrated counterparts. The yield was also maximized up to 54%, which is much more than that obtained using a traditional approach. Moreover, the ionic liquids can also be recovered and reused for the extraction process. Additionally, any residual material remaining after the extraction process was converted into cellulose, making the process environmentally friendly and sustainable.

Coupled one-pot oxidative extractive desulfurization of a model fuel catalyzed by nanostructured-ZIF-67/Biomass-derived activated carbon composite

The simultaneous oxidation and extraction of refractory sulfur compounds, such as DBT, has emerged as one of the most efficient complementary procedures for the HDS process in achieving ultradeep desulfurization of fuels. In this paper, a bio-based activated carbon (AC) obtained from the waste of date palm bark has been utilized as an abundant, green, and low-cost support for synthesizing a stable metal-organic framework, zeolitic imidazolate framework-67 (ZIF-67), on its structure to reach a novel nanocomposite catalyst (AC/ZIF-67) for the removal of DBT from a model fuel through the extractive oxidative desulfurization method. The accuracy of the AC/ZIF-67 catalyst formation was comprehensively characterized using XRD, FTIR, FESEM, BET, and TGA analytical techniques. Subsequently, the newly synthesized nanocomposite catalyst was employed efficiently for removing DBT from a toluene solution, acting as a model fuel. The impact of various operating variables, i.e. catalyst dosage, the temperature of reaction, oxidant-to-sulfur (O/S) molar ratio, contact time, initial concentration of DBT, and volume of extraction solvent on the removal efficiency has been thoroughly investigated. The results revealed that employing only 25 mg of the AC/ZIF-67 catalyst could achieve a remarkably high efficiency of around 98 % after one hour oxidation of a 25 ppm DBT solution in the presence of TBHP, followed by extraction using acetonitrile. This was achieved while maintaining a constant temperature of 60 °C and an O/S ratio of 20. The obtained results confirm the potential application of ACs for supporting MOF catalysts in various catalytic processes such as desulfurization.

Development of a highly sensitive method based on QuEChERS and GC-MS/MS for the determination of polycyclic aromatic hydrocarbons in infant foods.

Polycyclic aromatic hydrocarbons (PAHs) are environmental contaminants that can be found in various food products, including those intended for infants. Due to their potential health risks, it is crucial to develop sensitive analytical methods for the accurate determination of PAHs in infant foods. This study describes the development and validation of a highly sensitive method for the quantification of European PAH markers, namely benzo[a]pyrene, benzo[a]anthracene, chrysene, and benzo[b]fluoranthene, using gas chromatography-tandem mass spectrometry (GC-MS/MS), in baby food samples. The first step was the optimization of the sample preparation procedure, performed using different methods based on the QuEChERS approach, also testing different extraction solvents. Several factors such as extraction efficiency, selectivity, and recovery were evaluated to choose the most effective procedure for sample preparation. Furthermore, the GC-MS/MS method was optimized, evaluating parameters such as linearity, sensitivity, accuracy, and robustness using spiked infant food samples. The method demonstrated excellent linearities with a correlation coefficient higher than 0.999 over a wide concentration range, and limits of detection and limits of quantification in the range 0.019-0.036 μg/kg and 0.06-0.11 μg/kg, respectively. Extraction recoveries were between 73.1 and 110.7%, with relative standard deviations always lower than 8%. These findings are compliant with the indications of the European Commission (Reg. 836/2011). To assess the applicability of the method to official control activities, a survey was conducted on commercially available infant food products. Four markers were determined in commercial samples belonging to different food categories for infants and young children. The outcome of this monitoring showed that PAH contamination, in all samples, was below the quantification limits. In conclusion, the developed GC-MS/MS method provides a highly sensitive and reliable approach for the determination of PAHs in baby foods. The optimized sample preparation, instrumental parameters, and validation results ensure accurate quantification of 4 PAHs even at trace levels. This method could contribute to the assessment of PAH exposure in infants and it could support regulatory efforts to ensure the safety and quality of infant food products with regular monitoring.

Cyclodextrin-based ternary supramolecular deep eutectic solvents for efficient extraction and analysis of trace quinolones and sulfonamides in wastewater by adjusting pH

BackgroundAntibiotics residues can accelerate the growth of drug-resistant bacteria and harm the ecological environment. Under the effect of enrichment and biomagnification, the emergence of drug-resistant pathogenic bacteria may eventually lead to humans being ineffective to drugs in the face of bacterial or fungal disease infections in the future. It is urgent to develop an efficient separation medium and analytical method for simultaneous extraction and determination of antibiotics in the water environment. ResultsThis work doped 2,6-Di-O-methyl-β-cyclodextrin, randomly methyl-β-cyclodextrin, 2-hydroxypropyl-β-cyclodextrin with thymol:fatty acid respectively to construct non-covalent interaction-dominated pH-responsive ternary supramolecular deep eutectic solvents (SUPRADESs), which can undergo a hydrophilic/hydrophobic transition with aqueous phase to achieve an efficient microextraction. Semi-empirical method illustrated that SUPRADESs have a wide range of hydrogen bond receptor sites. We developed a SUPRADES-based analytical method combined with liquid chromatography-triple quadrupole mass spectrometry for the extraction and determination of trace quinolones and sulfonamides in wastewater. The overall limits of detection of the method were 0.0021–0.0334 ng mL−1 and the limits of quantification were 0.0073–0.1114 ng mL−1. The linearity maintained good in the spiked level of 0.01–100 ng mL−1 (R2 > 0.99). The overall enrichment factors of the method were 157–201 with lower standard deviations (≤8.7). SignificanceThe method gave an extraction recovery of 70.1–115.3 % for 28 antibiotics in livestock farming wastewater samples from Zhejiang, China, at trace levels (minimum 0.5 ng mL−1). The results demonstrated that inducing the phase transition between SUPRADES and aqueous phase by adjusting pH for extraction is a novel and efficient pretreatment strategy. To our knowledge, this is the first application of cyclodextrin-based ternary SUPRADESs with pH-responsive reversible hydrophobicity-hydrophilicity transition behavior in wastewater analysis.

A faster and more accessible method for the analysis of acephate and methamidophos in water samples by LC-MS/MS

ABSTRACT Pesticide pollution on environmental matrices has attracted increasing attention worldwide. Pesticide runoff from agricultural crops into surface waters may impact ecosystems and human health through drinking water consumption in pesticide-polluted areas. This study aims to develop and validate a simpler, faster, and more accessible methodology for the analysis of organophosphate pesticides, such as acephate and methamidophos, using HPLC-ESI-MS (QqQ). Acephate and methamidophos are two of the most common and efficient systemic pesticides in the organophosphate family, known for their high effectiveness against insects and pests. Firstly, different extractions were tested: liquid-liquid extraction (LLE), low-temperature partitioning extraction (LTPE) and solid-phase extraction (SPE) with a usual and accessible cartridge, C18. LLE and LTPE showed low sensitivities, probably because acephate and methamidophos are extremely hydrophilic compounds, like many organophosphorus pesticides. Thus, they have low interaction with the extractor solvent, resulting in low extraction rates. SPE with C18 cartridge led to the best extraction of acephate and methamidophos in water matrices and was chosen for the validated process. The selected method ensured acceptable recoveries, within the same range found in the scientific literature (9–49%) and within relative standard deviations below 20%. However, future efforts regarding other types of cartridges are encouraged. The limit of detection (LOD) and limit of quantification (LOQ) of the analytical method were 0.2 µg/L and 0.5 µg/L for acephate and methamidophos, values lower than those reported in the scientific literature. The developed method was used to quantify the levels of such organophosphate pesticides in samples from Brazilian surface water and none of the target pesticides were detected in these aquatic matrices.

Anti-black pod disease activity of leaf extract of Carica papaya Linn

BackgroundTheobroma cacao (Cocoa) is a major foreign exchange earner for Ghana. Over the recent decades, there has been a consistent decline in cocoa production in the country. A major contributing factor is the cocoa black pod disease caused by Phytophthora species. Synthetic fungicides have been used to control the pathogens over the years. However, recent calls for organic cocoa devoid of residues from synthetic fungicides, which are known to pose several health challenges as well as a negative impact on the environment, have gained attention. Thus, inviting investigations into more environmentally friendly and sustainable alternatives to synthetic fungicides. ObjectiveThis study explored the inhibitory potential of crude extract from Carica papaya against cocoa black pod disease caused by Phytophthora spp. Material and methodsAn in-silico study was done using known phytochemicals from Carica papaya as ligands against a Phytophthora effector protein. Crude extracts were obtained from the plant materials using 70 % ethanol as the extraction solvent. The crude Green Leaf Extract (GLE), Aging Induced Chlorophyll Deficient Leaf Extract (AICDLE), and Matured Black Seed Extract (SDE) were tested in-vitro against pre-cultured P. palmivora and P. megakarya using the poison food technique. GLE was modulated with Delco, a synthetic fungicide, at different ratios which were tested in-vitro and in-vivo. ResultsA total of 16 ligands showed binding affinity higher or equal to the standard ligand, alliin, suggesting Carica papaya as a repository of anti-phytophthora agents. Assessment of crude extracts at concentrations 5–20 mg/ml showed fungistatic activity against P. palmivora and P. megakarya in-vitro. Modulation of GLE with Delco produced some combinations that made GLE fungicidal in-vitro against P. palmivora and P. megakarya with fractional inhibition concentration indices between 0.51 and 0.65, interpreted as partially synergistic. The in-vivo assessment of combination D (Delco and GLE in a 0.3 mg:3 mg per ml ratio) performed as well as Delco alone at the recommended dose of 5 mg/ml. Thus, combination D reduces the requirement for copper-based fungicide by over 90 %. ConclusionThis study shows Carica papaya in a new light as a potential material that could be formulated into a natural product-based fungicide for combating Phytophthora-induced black pod disease.

Extraction of Natural Food Color from Tomato, Carrot and Turmeric

The demand for natural and healthier food products has increased dramatically in recent years due to growing consumer awareness of the impact food has on health as well as evidence of adverse effects from various ingredients, including some additives. This study evaluates the extraction method, solvent effects, precipitation, identification, purification, and lycopene, carotene, and curcumin content from turmeric, carrot, and tomato. Along-side, tomato, carrot, and turmeric samples were subjected to two different extraction and purification processes: solvent extraction for lycopene and carotene, and alkalization for curcumin. The samples were extracted and purified at room temperature (30ºC) and chilled (4ºC) for a period of three weeks. Tomato extracts had lycopene contents ranging from 0.0153 to 0.0362 mg/100g. obtained carotene content, which was then extracted using a solvent in the range of 61.43 to 81.72 mg/100g. The alkalization process produced a curcumin concentration of 91.17 to 110.41 mg/100g. Comparing the ethyl acetate extraction technique to the anti-solvent method, a greater amount of lycopene (red) and carotene (orange) precipitation was obtained. The maximum amount of curcumin precipitation obtained in lower pH solution. Lower pH is important to maintain the stability of curcumin precipitation. The experience of this research work suggested that lycopene from tomatoes, carotene from carrots, and curcumin from turmeric might be an excellent source to meet the increasing need for natural colorants.