The current study demonstrates the synthesis of fatty acids (FAs) capped silver nanoparticles (AgNPs) using aqueous poly-herbal drug Liv52 extract (PLE) as a reducing, dispersing and stabilizing ...agent. The NPs were characterized by various techniques and used to investigate their potent antibacterial, antibiofilm, antifungal and anticancer activities. GC-MS analysis of PLE shows a total of 37 peaks for a variety of bio-actives compounds. Amongst them, n-hexadecanoic acid (21.95%), linoleic acid (20.45%), oleic acid (18.01%) and stearic acid (13.99%) were found predominately and most likely acted as reducing, stabilizing and encapsulation FAs in LIV-AgNPs formation. FTIR analysis of LIV-AgNPs shows some other functional bio-actives like proteins, sugars and alkenes in the soft PLE corona. The zone of inhibition was 10.0 ± 2.2-18.5 ± 1.0 mm, 10.5 ± 2.5-22.5 ± 1.5 mm and 13.7 ± 1.0-16.5 ± 1.2 against
,
and
, respectively. LIV-AgNPs inhibit biofilm formation in a dose-dependent manner i.e., 54.4% ± 3.1%-10.12% ± 2.3% (
)
72.7% ± 2.2%-23.3% ± 5.2% (
) and 85.4% ± 3.3%-25.6% ± 2.2% (
), and SEM analysis of treated planktonic cells and their biofilm biomass validated the fitness of LIV-AgNPs in future nanoantibiotics. In addition, as prepared FAs rich PLE capped AgNPs have also exhibited significant (
< 0.05 *) antiproliferative activity against cultured HCT-116 cells. Overall, this is a very first demonstration on employment of FAs rich PLE for the synthesis of highly dispersible, stable and uniform sized AgNPs and their antibacterial, antifungal, antibiofilm and anticancer efficacy.
The identification and quantification of selected plastics (polystyrene (PS), polycarbonate (PC), poly-(methyl methacrylate) (PMMA), polypropylene (PP), polyethylene terephthalate (PET), polyethylene ...(PE) and polyvinyl chloride (PVC)) in biosolids (treated sewage sludge) was performed by pressurized liquid extraction (PLE) combined with double-shot pyrolysis gas chromatography–mass spectrometry. Validation of the method yielded recoveries of between 85 and 128% (mean RSD 11%) at a linear range of between 0.01 and 2 μg. The distribution of plastics within 25 biosolid samples from a single wastewater treatment plant in Australia was assessed. The mass concentration of PE, PVC, PP, PS and PMMA was between 0.1 and 4.1 mg/g dry weight (dw) across all samples, with a total plastic concentration ƩPlastics of between 2.8 and 6.6 mg/g dw (median = 4.1 mg/g dw). PE was the predominant plastic detected (mean concentration of 2.2 mg/g dw), contributing to 50% of the total of all plastics. Overall, this study demonstrates that pressurized liquid extraction (PLE) combined with double-shot pyrolysis gas chromatography–mass spectrometry can be used to identify and quantify PE, PP, PVC, PS, and PMMA in biosolids.
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•Alternative and complementary quantitative analytical method for the analysis of selected plastics in complex environmental samples.•Pressurized liquid extraction (PLE) combined with double-shot pyrolysis gas chromatography-mass spectrometry (Pyr-GC/MS) allows for the identification and quantification of polyethylene, polystyrene, poly-methyl methacrylate, polypropylene and polyvinyl chloride.•The double-shot feature allows for the effective thermal desorption of potentially interfering co-extracted compounds from complex organic rich samples.•Total plastic concentration of between 2.8 and 6.6 mg/g dw (median = 4.1 mg/g dw) in Australian biosolids•PE was the predominant plastic detected (mean concentration of 2.2 mg/g dw), contributing to 50 % of the total of all plastics.
An analytical method for the determination of free 3-monochloropropane-1,2-diol (3-MCPD) in grilled meat using pressurized liquid extraction, derivatisation using phenylboronic acid, and gas ...chromatography/high resolution mass spectrometry was developed. The limit of quantification was 1 μg/kg. Using this method, the contents of 3-MCPD in grilled steaks (collar) were analysed for different grilling conditions. Charcoal, an electric grill, and a gas grill were used for grilling collars. Further parameters investigated were the pre-treatment of meat (untreated, salted, marinated with oil or emulsion marinade), the use of aluminium grill trays, and a lid. For grilled steaks, contents of 3-MCPD in the range of <1 to 365 μg/kg (median 16 μg/kg) were detected. The highest contamination was found for a steak pre-treated with an oily marinade grilled on a charcoal grill with a closed lid. Consuming such a steak will exhaust the tolerable daily intake of 2 μg/kg body weight for 3-MCPD to about 26 %.
A novel valorization strategy is proposed in this work for the sustainable utilization of a major mango processing waste (i.e. mango seed kernel, MSK), integrating green pressurized-liquid extraction ...(PLE), bioactive assays and comprehensive HRMS-based phytochemical characterization to obtain bioactive-rich fractions with high antioxidant capacity and antiproliferative activity against human colon cancer cells. Thus, a two steps PLE procedure was proposed to recover first the non-polar fraction (fatty acids and lipids) and second the polar fraction (polyphenols). Efficient selection of the most suitable solvent for the second PLE step (ethanol/ethyl acetate mixture) was based on the Hansen solubility parameters (HSP) approach. A comprehensive GC- and LC-Q-TOF-MS/MS profiling analysis allowed the complete characterization of the lipidic and phenolic fractions obtained under optimal condition (100% EtOH at 150 °C), demonstrating the abundance of oleic and stearic acids, as well as bioactive xanthones, phenolic acids, flavonoids, gallate derivatives and gallotannins. The obtained MSK-extract exhibited higher antiproliferative activity against human colon adenocarcinoma cell line HT-29 compared to traditional extraction procedures described in literature for MSK utilization (e.g. Soxhlet), demonstrating the great potential of the proposed valorization strategy as a valuable opportunity for mango processing industry to deliver a value-added product to the market with health promoting properties.
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•Powerful analytical strategy for mango seed kernel valorization•Green extraction procedure in two steps to recover lipidic and phenolic fractions•Phytochemical profiling of obtained PLE fractions by LC/GC-q-TOF-MS(/MS)•Antiproliferative activity of the phenolic extracts against colon cancer cells
The brominated flame retardants hexabromocyclododecane (HBCD) and tetrabromobisphenol A (TBBPA) are high-production-volume chemicals. In recent years, their presence has been reported in sediment and ...biota from the marine environment. In this study, an analytical method was developed for the simultaneous determination of HBCD, TBBPA, and the possible metabolite dimethyl-TBBPA. The method was applied in a preliminary screening of egg, liver, and adipose tissue of marine biota from Greenland and the Faroe Islands. α-HBCD was detected in 35 of 36 analysed samples from the Arctic, indicating a ubiquitous presence of α-HBCD in the environment. β- and γ-HBCD were found in 10 and 14 samples, respectively. TBBPA and dimethyl-TBBPA were not detected in any of the samples indicating limited or no transport of these compounds to remote areas.
A simultaneous multiresidue method to determine 14 different pesticides, namely: flufenoxuron, fenitrothion, chlorfluazuron, chlorpyrifos, hexythiazox, methidathion, chlorfenapyr, tebuconazole, EPN, ...bifenthrin, cyhalothrin, spirodiclofen, difenoconazole, and azoxystrobin in green tea using pressurized liquid extraction (PLE) is described and compared with that of liquid-liquid extraction (LLE). For PLE, the extraction conditions were not optimized. Rather they were selected based upon previous successful investigations published by our laboratory. Analysis was performed by GC with electron capture detector (GC-ECD), and the pesticide identity of the positive samples was confirmed by GC-MS in a selected ion-monitoring (SIM) mode. Calibration curves showed an excellent linearity for concentrations ranging from 0.006 to 36.049 ppm, with r² >0.995. Green tea spiked at each of the two fortification levels, yielded average recoveries in the range of 87-112% and 71-109% for PLE and LLE, respectively. Precision values, expressed as RSDs, were below 6% at various spiking levels. With respect to the existing procedures, both methods gave LOQs that were lower than the maximum residue limits (MRLs) established by the Korea Food and Drug Administration (KFDA). Both methods have been successfully applied to the analysis of real samples, and bifenthrin was the only pesticide residue quantified in incurred green tea samples, with concentrations ranging from 0.093 ppm (LLE) to 0.1 ppm (PLE). These concentration levels were relatively low compared to KFDA-MRL (0.3 ppm). According to the validation data and performance characteristics, both methods are appropriate for multiresidue analysis of pesticide residues in green tea. PLE methodology showed superiority in recoveries of some pesticides, acceptable accuracy and precision while minimizing environmental concerns, time, and labor, and can be applied in routine analytical laboratories.
The quantification of microplastics (MP) in environmental samples is currently a challenging task. To enable low quantification limits, an analytical method has been developed combining pressurized ...liquid extraction (PLE) and pyrolysis GC-MS. The automated extraction includes a pre-extraction step via methanol followed by a subsequent PLE using tetrahydrofuran. For the most frequently used synthetic polymers polyethylene (PE), polypropylene (PP), and polystyrene (PS), limits of quantification were achieved down to 0.007 mg/g. Recoveries above 80% were attained for solid matrices such as soil and sediments. The developed method was applied for MP quantification in environmental samples such as sediment, suspended matter, soil, and sewage sludge. In all these matrices, PE and PP were detected with concentrations ranging from 0.03 to 3.3 mg/g. In sewage sludge samples, all three polymers were present with concentration levels ranging between 0.08 ± 0.02 mg/g (PP) and 3.3 ± 0.3 mg/g (PE). However, especially for solid samples, the analysis of triplicates revealed elevated statistical uncertainties due to the inhomogeneous distribution of MP particles. Thus, care has to be taken when milling and homogenizing the samples due to the formation of agglomerates.
Graphical abstract
Piperaceae family is original from tropical regions and it shows more than 700 species around the world.
Piper gaudichaudianum Kunth is the specie more abundant in Brazil, occurring from Northeast to ...South Brazil. In this paper, it was investigated the influence of some experimental parameters on the pressurized liquid extraction (PLE) of
P. gaudichaudianum Kunth leaves, using petroleum ether as extractor solvent. The optimization of the main variables involved in the PLE process (extraction temperature and time) has been done by response surface methodology (RSM) using, as responses, the extraction yield and the chromatographic profile (GC/MS) of the extracts. The optimized procedure employed 3
g of ground leaves, 10
min of extraction and one cycle of extraction at 85
°C. The major compounds present in the petroleum ether extracts were: palmitic acid, stearic acid and nerolidol. The results presented in this work show the possibility of using a fast and easy process to recover compounds from
P. gaudichaudianum Kunth.
•Simultaneous analysis of different classes of UV filters in personal care products.•First time that PLE GC–MS/MS is implemented for UV filters in cosmetics.•Micro-PLE enables to minimize the amounts ...of sample, solvent and sorbent required.•The use of a matrix matched approach (using cosmetic oil) avoided matrix effects.•The method was successfully applied to a broad range of cosmetic formulations.
A methodology based on pressurized liquid extraction (PLE) followed by gas chromatography–tandem mass spectrometry (GC–MS/MS) has been developed for the simultaneous analysis of different classes of UV filters including methoxycinnamates, benzophenones, salicylates, p-aminobenzoic acid derivatives, and others in cosmetic products. The extractions were carried out in 1mL extraction cells and the amount of sample extracted was only 100mg. The experimental conditions, including the acetylation of the PLE extracts to improve GC performance, were optimized by means of experimental design tools. The two main factors affecting the PLE procedure such as solvent type and extraction temperature were assessed. The use of a matrix matched approach consisting of the addition of 10μL of diluted commercial cosmetic oil avoided matrix effects. Good linearity (R2>0.9970), quantitative recoveries (>80% for most of compounds, excluding three banned benzophenones) and satisfactory precision (RSD<10% in most cases) were achieved under the optimal conditions. The validated methodology was successfully applied to the analysis of different types of cosmetic formulations including sunscreens, hair products, nail polish, and lipsticks, amongst others.
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