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•Tuber melanosporum is a potential source of bioactive compounds.•PLE (16.7 MPa, 180 °C, 30 min) can extract polysaccharides and fungal sterols.•(1 → 3)-β-glucans and heteropolymers ...were identified in truffles.•Extracted polysaccharides reduced pro-inflammatory cytokines secretion.
Truffles, besides the appreciated aromatic compounds, contain other molecules with interesting bioactive properties. A screening of fungal sterols and β-glucans within different truffle species and locations was carried out. These compounds were extracted with pressurized liquids (PLE) generating enriched fractions. Extraction efficiency was studied with a full-factorial experimental design (Response surface methodology, RSM), using water and ethanol as extraction solvents. Polysaccharides from truffle powder (TP) and the optimal PLE extract (EP) obtained were precipitated and analysed by NMR and GC–MS. THP-1 cell cultures were utilized to test immunomodulatory properties. With the optimal PLE conditions (16.7 MPa, 180 °C, 30 min) 64 and 22.5% yields were obtained respect, with water and ethanol, generating fractions containing respect, 9.1% β-glucan and 4.5% ergosterol. NMR analyses detected (1 → 3)-β-glucan structures in truffle. The EP induced a reduction of 40% IL-1β and 60% IL-6 pro-inflammatory cytokines secretion suggesting potential immunomodulatory activity.
A rapid and simultaneous method for residue identification and quantification for seven pesticides in agricultural soils has been developed to study a realistic situation in vineyard. The target ...compounds are two insecticides, two herbicides and three fungicides, from different chemical families. The procedure is based on a pressurized liquid extraction (PLE) with acetone, before a multiresidue GC–MS analysis. The recovery of PLE is between 53.8
±
2.4 and 99.9
±
4.4% according to pesticide. A limit of detection (LOD) between 1.4 and 4.6
μg
kg
−1 of dry soil was obtained for five analytes. This procedure for testing soil contamination is sensitive and easy to perform.
Curcuma longa (Zingiberaceae) is a native plant of southern Asia and is cultivated extensively throughout the warmer parts of the world.
Jianghuang and
Yujin are rhizome and tuberous root of
C. ...longa, respectively, which were traditionally used as two Chinese medicines. In this paper, pressurized liquid extraction (PLE) and gas chromatography–mass spectrometry (GC–MS) were developed for quantitative determination/estimation of eight characteristic compounds including β-caryophyllene, ar-curcumene, zingiberene, β-bisabolene, β-sesquiphellandrenendrene, ar-turmerone, α-turmerone and β-turmerone in
Jianghuang and
Yujin. A HP-5MS capillary column (30
m
×
0.25
mm i.d.) coated with 0.25
μm film 5% phenyl methyl siloxane was used for separation and selected ion monitoring (SIM) method was used for quantitation. Hierarchical cluster analysis based on characteristics of eight identified peaks in GC–MS profiles showed that 10 samples were divided into two main clusters,
Jianghuang and
Yujin, respectively. Four components such as ar-curcumene, ar-turmerone, α-turmerone and β-turmerone were optimized as markers for quality control of rhizome (
Jianghuang) and tuberous root (
Yujin), which are two traditional Chinese medicines, from
Curcuma longa.
Gas chromatography coupled to ion trap tandem mass spectrometry (GC–ITMS-MS) is proposed for the analysis of methoxylated polybrominated diphenyl ethers (MeO-PBDEs) in fish and shellfish. MS–MS ...operating parameters related to the isolation and fragmentation of the precursor ions were optimized to achieve maximum sensitivity and selectivity. This new method allows the determination of both MeO-PBDEs and PBDEs in a single run. Low limits of detection (0.4–2.5
pg injected) and high precision (RSD
<
13%) were achieved. A sample treatment based on a selective pressurized liquid extraction (PLE) using Florisil as fat retainer was applied for the analysis of these compounds in fish samples. Method limits of quantification ranged from 0.11 to 0.95
ng
g
−1 lipid weight for MeO-PBDEs and between 0.18 and 0.50
ng
g
−1 lipid weight for PBDEs. In addition, good repeatability of the whole method was achieved (RSD
<
15%). The suitability of the method was evaluated by analyzing a certified reference material (SRM 1945, whale blubber) with satisfactory results. The developed method was applied to the simultaneous analysis of MeO-PBDEs and PBDEs in fish and shellfish samples from the Mediterranean Sea.
Pressurized liquid extraction (PLE) was applied for the first time to extract bioactive low molecular weight carbohydrates (iminosugars and inositols) from mulberry (Morus alba) leaves. Under ...optimized conditions, PLE provided a similar yield to the conventional process used to extract these bioactives, but in less time (5 vs 90 min). To remove carbohydrates that interfere with the bioactivity of iminosugars from PLE extracts, two fractionation treatments were evaluated: yeast (Saccharomyces cerevisiae) incubation and cation-exchange chromatography (CEC). Both methods allowed complete removal of major soluble carbohydrates (fructose, glucose, galactose, and sucrose), without affecting the content of mulberry bioactives. As an advantage over CEC, the yeast treatment preserves bioactive inositols, and it is an affordable methodology that employs food grade solvents. This work found PLE followed by yeast treatment to be an easily scalable and automatable procedure that can be implemented in the food industry.
In this study, levels of several groups of environmental contaminants represented by PAHs, PCBs, organochlorine pesticides and polybrominated diphenyl ethers were determined in various types of ...canned smoked and non-smoked fish and seafood products (54 samples) obtained from the Czech market. PAHs were detected in all of the studied samples, and at least one of the target halogenated persistent organic pollutants was present above the LOQ in 85% of the samples. The levels of PAHs, PCBs, organochlorine pesticides (mainly DDTs) and polybrominated diphenyl ethers found in the canned products varied in the range of 1.4-116 µg kg
−1
, 0.6-59.6 µg kg
−1
, 0.6-82.7 µg kg
−1
and 0.1-2.1 µg kg
−1
can content, respectively. Smoked sprats were the most contaminated fish product (n = 12) in which the highest levels of both PAHs and persistent organic pollutants were found. In 67% of the samples of smoked sprats in oil, the level of benzoapyrene exceeded the maximum level of 5 µg kg
−1
established for smoked fish by European Union legislation. The distribution of target analytes between oil and fish fractions was also assessed. Significantly higher levels of PAHs were measured in the oil fraction.
► A method to identify and quantify organic compounds in marine sediments is proposed. ► PLE extraction enables extraction of sediment with a minimal solvent consumption. ► Preconcentration with SBSE ...allows reaching ppb detection and quantification limits. ► The LOQ obtained ranged from 0.014 to 1.0ngg−1, with LOD below pgg−1 levels. ► GC–MS/MS allows the identification and quantification of compounds in complex matrices.
A multiresidue method for the analysis of 86 persistent pollutants in marine sediments at ultra-trace level has been developed and validated using pressurized liquid extraction (PLE) and stir-bar sorptive extraction (SBSE) coupled with thermal desorption and gas chromatography–triple quadrupole mass spectrometry (TD–GC–MS/MS QqQ). The compounds analyzed belong to various families such as polychlorinated biphenyls, polycyclic aromatic hydrocarbons, polybrominated diphenylethers, organophosphorus and organochlorine pesticides and other pesticides such as urons, and triazines. The analytes have very different polarities and logKow values, which is an important parameter in the optimization of a SBSE method. Due to PLE high efficiency and throughput rates, along with the proven ability for multiresidue analysis and excellent sensitivity of SBSE, we present an efficient method. The limits of quantification obtained ranged from 0.014 to 1.0ngg−1, with detection limits below pgg−1 levels. In order to validate the proposed methodology, quality parameters such as recovery, linearity and reproducibility were studied. Recoveries ranged from 63% to 119%, reproducibility (in terms of Relative Standard Deviation for ten determinations) was lower than 35% in all cases, and determination coefficients higher than 0.990 for all analytes. The main factors that affect PLE, SBSE and GC–MS/MS procedures were optimized. The method was applied to the analysis of nine marine sediments obtained from the nine main submarine wastewater discharge points (emissaries) presents along the coast of Tenerife Island (Canary Islands, Spain).
Gas chromatography-mass spectrometry (GC/MS) was employed for the determination of 30 widely used pesticides including various transformation products and alkylphenols in water and agricultural soils ...with the aim of assessing the impact of these compounds in agricultural soils and the underlying aquifer. The extraction, clean-up, and analytical procedures were optimized for both water and soil samples to provide a highly robust method capable of determining target analytes at the ppb-ppt level with high precision. For water samples, different solid-phase extraction cartridges and conditions were optimized; similarly, pressurized liquid extraction conditions were tested to provide interference-free extracts and high sensitivity. Instrumental LODs of 3-4 pg were obtained. The multi-residue extraction procedures were applied to the analysis of groundwaters and agricultural soils from the Ebro river basin (NE Spain). Most ubiquitous herbicides detected were triazines but some acetanilides and organophosphorus pesticides were also found; the pesticide additive tributylphosphate was found in all water samples. Levels varied between 0.57 and 5.37 μg/L in groundwater, whereas nonylphenol was the sole compound detected in soil. Alkylphenols are used as adjuvants in pesticide formulations and are present in sludges employed as soil fertilizers. Occurrence was found to be similar to other environmental studies.
The presence of benzothiazoles (BTHs) and organic ultraviolet filters (UV filters) in aquatic ecosystems has emerged as a significant environmental issue, requiring urgent and efficient determination ...methods. A new, rapid, and sensitive determination method using gas chromatography triple quadrupole mass spectrometer (GC–MS/MS) was developed for the simultaneous extraction and analysis of 10 commonly used BTHs and 10 organic UV filters in surface water, wastewater, sediment, and sludge. For aqueous samples, solid-phase extraction (SPE) method was employed with optimizing of SPE cartridge type, pH, and elution solvent. For solid samples, ultrasonic extraction-solid-phase extraction purification (UE-SPE) and pressurized liquid extraction (PLE) methods were compared. And extraction conditions for ultrasonic extraction method (extraction solvents and extraction times) and PLE method (extraction temperatures and extraction cycles) were optimized. The limits of quantification for the 20 target compounds in surface water and wastewater were 0.01–2.12 ng/L and 0.05–6.14 ng/L, while those for sediment and sludge with UE-SPE method were 0.04–5.88 ng/g and 0.22–6.61 ng/g, respectively. Among the 20 target compounds, the recoveries ranged from 70 to 130% were obtained for 16, 15, 15, and 15 analytes in the matrix-spiked samples of surface water, wastewater, sediment, and sludge with three levels, respectively. And the precision was also acceptable with relative standard deviation (RSD) below 20% for all analytes. The developed methods were applied for the determination and quantification of target compounds in surface water, sediment, wastewater, and sludge samples collected from two wastewater treatment plants (WWTPs) and the Pearl River in Guangzhou, China. BTHs were frequently detected in surface water and wastewater, while UV filters were mainly found in sediment and sludge. Benzotriazole (BT) and 2-hydroxybenzothiazole (2-OH-BTH) were the two major BTHs in influent wastewater and surface water, respectively, with concentrations up to 966 and 189 ng/L. As for sediment and sludge, 2-(2′-hydroxy-5′-octylphenyl)-benzotriazole (UV-329) was a predominant chemical, detected at concentrations of 111 and 151 ng/g, respectively.
Graphical abstract
A method for the quantitative determination of ten musk fragrances extensively used in personal care products from sewage sludge was developed by using a pressurized liquid extraction (PLE) followed ...by an automated ionic liquid‐based headspace single‐drop microextraction and gas chromatography‐tandem mass spectrometry. The influence of main factors on the efficiency of PLE was studied. For all musks, the highest recovery values were achieved using 1 g of pretreated sewage sludge, H2O/methanol (1:1) as an extraction solvent, a temperature of 80°C, a pressure of 1500 psi, an extraction time of 5 min, 2 cycles, a 100% flush volume, a purge time of 120 s, and 1 g Florisil as in‐cell clean‐up extraction sorbent. The use and optimization of an in‐cell clean‐up sorbent was necessary to remove fatty interferents of the PLE extract that make the subsequent ionic liquid‐based headspace single‐drop microextraction difficult. Validation parameters, namely LODs and LOQs, ranged from 0.5–1.5 to 2.5–5 ng/g, respectively. Good levels of intra‐ and interday repeatabilities were obtained analyzing sewage sludge samples spiked at 10 ng/g (n = 3, RSDs < 10%). The method applicability was tested with sewage sludge from different wastewater treatment plants. The analysis revealed the presence of all the polycyclic musks studied at concentrations higher than the LOQs, ranging from 6 to 530 ng/g. However, the nitro musk concentrations were below the LOQs or, in the case of musk xylene, was not detected.
