Accelerated Solvent Extraction Research Articles

Exploring traditional and modern approaches for extracting bioactive compounds from Ferulago trachycarpa

For more than two millennia, Ferulago species have been revered as therapeutic herbs, maintaining their significance in present-day folk medicine practices. Therefore, the present study was conducted to investigate the phytochemical composition, inhibitory effects on metabolic enzymes, and possible therapeutic applications of F. trachycarpa, specifically focusing on its efficacy in diabetes management, anticholinergic effects, and antioxidant capabilities. The current investigation comprised an evaluation of a range of extracts acquired via conventional and modern methodologies, such as soxhlet (SOX), maceration (MAC) accelerated solvent extraction (ASE), homogenizer-assisted extraction (HAE), supercritical fluid extraction (SFE), microwave-assisted extraction (MW), and ultrasound-assisted extraction (UAE). Various techniques were employed to assess their antioxidant capacity and enzyme inhibition. Furthermore, the research utilized ultra-high performance liquid chromatography-MS/MS (UHPLC-MS/MS) to ascertain the principal phenolic compounds that are responsible for the antioxidant capacity observed in the various F. trachycarpa extracts. Among these, extracts from HAE, ASE, and MW revealed the most promise across all methodologies tested for their antioxidant potential. Furthermore, SFE and MAC extracts inhibited the most enzymes, including cholinesterases, tyrosinase, α -amylase, and α -glycosidase, indicating their potential as efficient natural treatments for several health-related issues.

Improved analysis of 230 pesticide residues in three fermented soy products by using automated one-step accelerated solvent extraction coupled with GC–MS/MS

Consumer concerns over healthy diets are increasing as a result of the toxicity and persistence of pesticide residues in foodstuffs. Developing sensitive and high-throughput monitoring techniques for these trace residues is seen as an essential step in ensuring food safety. An automatic and sensitive multi-residue analytical method was developed and validated for the simultaneous determination of 230 compounds, including pesticides and their hazardous metabolites, in fermented soy products. The method included preparing the sample using on-line extraction and clean-up system based on accelerated solvent extraction (ASE), then determining the analytes using GC–MS/MS techniques. The homogenized samples (soy sauce, douchi, and sufu) were automatically extracted at 80 °C and 10.3 MPa and at the same time, in situ cleaned by 300 mg of primary secondary amine (PSA) combined with 20 mg of hydroxylated multi-walled carbon nanotubes in an extraction cell. The method obtained excellent calibration linearity (r > 0.9220) and a satisfactory analysis of the targeted compounds, which were evaluated with matrix-matched calibration standards over the range of 5–500 μg L−1. The limit of detections (LODs) of analytes were in the range of 0.01–1.29 μg kg−1, 0.01–1.39 μg kg−1, and 0.01–1.34 μg kg−1 in soy sauce, douchi, and sufu, respectively. The limit of quantifications (LOQs), which defined as the lowest spiking level, were set at 5.0 μg kg−1. The recoveries were within 70–120 % for over 95 % of the analytes, and the relative standard deviations (RSDs) were below 13.6 %. Moreover, a positive detection rate of 47 % were obtained when the proposed method was used on 15 real fermented soy products. These results suggested that the developed high-throughput method is highly feasible for monitoring of these target analytes in trace level.

Quantification of quaternary ammonium compounds by liquid chromatography-mass spectrometry: Minimizing losses from the field to the laboratory

Quaternary Ammonium Compounds (QACs) are widely used in household, medical and industrial settings. As a consequence, they are ubiquitously found in the environment. Although significant efforts have been put into the development of sensitive and reproducible analytical methods, much less effort has been dedicated to the monitoring of QACs upon sample storage and sample preparation. Here we studied the effect of storage, concentration, and extraction procedures on the concentrations of QACs in samples. Thirteen QACs selected amongst benzalkonium compounds (BACs), dialkyldimethylammonium compounds (DADMACs) and alkyltrimethylammonium compounds (ATMACs) were quantified in aqueous and solid samples using LC-MS/MS. Most QACs adsorbed on container walls could be recovered using a short washing step with MeOH containing 2 % v/v formic acid. Concentrations of QACs from aqueous solutions using solid phase extraction (SPE) with Strata-X cartridges and elution with acidified MeOH utilized to wash the emptied containers gave highly satisfactory recoveries (101–111 %). Good recoveries (89–116 %) were also obtained when extracting a spiked organic-rich synthetic soil using accelerated solvent extraction (ASE) with acidified MeOH at low solid/solvent ratio (0.4 g/20 mL). Applying the recommended methodologies to real samples collected from a Canadian wastewater treatment plant (WWTP) gave QAC concentrations in the ranges of 0.01–30 µg/L, < 1.2 µg/L, and 0.05–27 mg/kg for the influent, effluent and biosolids samples, respectively.

UHPLC-MS/MS analysis, cytotoxic, enzyme inhibition, and antioxidant properties of Lantana camara L. extracts obtained by conventional and nonconventional methods.

Lantana camara is widely known as a garden plant, but its use for various medicinal purposes is widespread in traditional medicine. In the frame of this study, L. camara was subjected to several different extraction techniques, including supercritical carbon dioxide extraction, accelerated solvent extraction (ASE), homogenizer-assisted extraction, microwave-assisted extraction, ultrasound-assisted extraction, maceration, and Soxhlet extraction. The investigation encompasses the analysis of the chemical composition alongside assessments of biological activities, such as antioxidant and enzyme-inhibition potential and cytotoxicity of the obtained extracts. The obtained results showed that the extract obtained by accelerated-solvent extraction was the richest in the content of total phenols and of individual compounds. Of the 17 components identified in total, hispidulin was detected in the highest concentration (5.43-475.97 mg/kg). In the antioxidant assays, the extracts obtained by accelerated-solvent and microwave extraction possessed the highest level of antioxidant and antiradical protection. All obtained extracts showed enzyme-inhibitory action on amylase, glucosidase, tyrosinase, and cholinesterase, showing a high potential for application against diseases induced by excessive activity of these enzymes. Cytotoxic analysis was performed on normal and tumor cells, whereby the obtained IC50 values were in the range of 7.685-79.26 µg/mL, showing the high cytotoxicity of the obtained extracts. Using Z score analysis, ASE resulted in an optimal combination of tested quality characteristics of the L. camara extracts.

Determination of per- and polyfluoroalkyl compounds in paper recycling grades using ultra-high-performance liquid chromatography–high-resolution mass spectrometry

Globally, per- and polyfluoroalkyl substances (PFAS)–related research on paper products has focused on food packaging with less consideration on the presence of PFAS at different stages of the paper recycling chain. This study analysed the prevalence of PFAS in paper grades used for the manufacture of recycled paperboard. The presence of PFAS was attributed to the use of PFAS-containing additives, consumer usage, exposure to packed goods as well as contamination during mingling, sorting, collection, and recovery of paper recycling material. Q Orbitrap mass spectrometry was used to analyse the paper samples after accelerated solvent extraction and solid phase extraction. The distribution and possible propagation of 22 PFAS were determined in pre-consumer, retail and post-consumer paper products. Post-consumer samples had the highest combined average concentration (ΣPFAS) at 213 ng/g, while the ΣPFAS in retail (159 ng/g) and pre-consumer samples (121 ng/g) was detected at lower concentrations. This study showed that waste collection and recycling protocols may influence PFAS propagation and that measures must be developed to minimise and possibly eliminate exposure opportunities.

Identifying organic micropollutants' transformation products from the soil dissipation experiment by non-targeted high-resolution mass spectrometry approach: Can we gain more than transformation product identity?

Risk assessment of environmental hazards originating from xenobiotics extensively used worldwide (e.g., pharmaceuticals, bisphenols, or preservatives) requires a combined study of their effects, mobility, dissipation mechanisms, and subsequent transformation product identification and evaluation. We have developed an efficient accelerated solvent extraction method for a broad range of micropollutants of variable physical-chemical properties in soils to enable more accurate hazard characterisation. Micropollutant recoveries from freeze-dried soils were 60–120%, with the exception of atorvastatin, fexofenadine, and telmisartan, which had reduced recoveries (40–66%). The observed matrix effect ranged from −26% to 17% and was corrected by the matrix matching standard for quantitative analysis. The method allows sensitive and reliable determination of a wide range of analytes in soil samples and, consequently, qualitative analysis of transformation products (TP) with variable physicochemical properties. We identified TPs of five compounds (venlafaxine, telmisartan, valsartan, atorvastatin, and sertraline) by applying suspect and non-targeted data analyses. To our knowledge, the transformation product of atorvastatin was reported for the first time. All others were found in soil or other matrices. Valsartan (formed valsartan acid) and atorvastatin (transformed probably by oxidative decarboxylation of beta, delta dihydroxy heptanoic acid chain to propionic acid) were modified to a relatively large extent. All other compounds identified were only hydroxylated (sertraline and telmisartan) or demethylated (venlafaxine). We estimated the stability and presence of the identified TPs based on the constructed time trends and the ratio between TP formation and degradation rates. We demonstrated how valuable a non-targeted approach can be for complex evaluation of the fate and effect of soil pollutants.

Eco-Friendly Extraction: A green approach to maximizing bioactive extraction from pumpkin (Curcubita moschata L.)

The research focused on optimizing the accelerated solvent extraction (ASE) of carotenoids and polyphenols from pumpkin powder. The study optimized accelerated solvent extraction (ASE) of carotenoids and polyphenols from pumpkin powder. Using a mix of standard score (SS) and artificial neural network (ANN) methods, the extraction process was fine-tuned. The ANN model assessed extraction parameters' significance, achieving high predictability for total carotenoid content (TCC), total phenolic content (TPC), and free radical scavenging capacity (DPPH and ABTS methods). The analysis highlighted the most effective extraction at 50 % concentration, 120 °C temperature, 5 min duration, and 2 cycles, yielding high carotenoid and phenolic content (TCC 571.49 µg/g, TPC 7.85 mg GAE/g). HPLC-DAD profiles of the optimized ASE extract confirmed major carotenoids and phenolic compounds. Strong correlations were found between bioactive compounds and antioxidant activity, emphasizing potential health benefits.

Silicon's Influence on Polyphenol and Flavonoid Profiles in Pea (Pisum sativum L.) under Cadmium Exposure in Hydroponics: A Study of Metabolomics, Extraction Efficacy, and Antimicrobial Properties of Extracts.

The current study aimed to investigate the impact of silicon (Si) supplementation in the form of Na2SiO3 on the metabolome of peas under normal conditions and following exposure to cadmium (Cd) stress. Si is known for its ability to enhance stress tolerance in various plant species, including the mitigation of heavy metal toxicity. Cd, a significant contaminant, poses risks to both human health and the environment. The study focused on analyzing the levels of bioactive compounds in different plant parts, including the shoot, root, and pod, to understand the influence of Si supplementation on their biosynthesis. Metabolomic analysis of pea samples was conducted using a targeted HPLC/MS approach, enabling the identification of 15 metabolites comprising 9 flavonoids and 6 phenolic acids. Among the detected compounds, flavonoids, such as flavon and quercetin, along with phenolic acids, including chlorogenic acid and salicylic acid, were found in significant quantities. The study compared Si supplementation at concentrations of 1 and 2 mM, as well as Cd stress conditions, to evaluate their effects on the metabolomic profile. Additionally, the study explored the extraction efficiency of three different methods: accelerated solvent extraction (ASE), supercritical fluid extraction (SFE), and maceration (MAC). The results revealed that SFE was the most efficient method for extracting polyphenolic compounds from the pea samples. Moreover, the study investigated the stability of polyphenolic compounds under different pH conditions, ranging from 4.0 to 6.0, providing insights into the influence of the pH on the extraction and stability of bioactive compounds.

Phytochemical, Pharmacological, and Toxicological Prospection of Morus nigra L.: A Systematic Review

Introduction: Morus nigra L. has industrial relevance due to the presence of specialized metabolites, which possess pharmaceutical potential in various parts and preparations. This review presents updated information on traditional, phytochemical, and pharmacological applications, as well as toxicity data, pertaining to different parts of Morus nigra L. Method: Phytochemical research and ethnobotanical studies were conducted using reviewed databases. Mulberry leaves have demonstrated several biological activities, attributed to the presence of phenolic acids, flavonoids, and fatty acids. Stems and roots contain additional compounds such as stilbenes and benzofurans. Morus nigra L. exhibits various biological activities, including hepatoprotective, hypolipidemic, anti-inflammatory, antioxidant, antimicrobial, neuroprotective, hypoglycemic, skin whitening, cytotoxic, antiatherosclerotic, and antiobesity effects. The choice of extraction technique and plant part is crucial to obtain a diverse range of compounds necessary for specific indications. Result: Accelerated solvent extraction (ASE) has proven to be the most advantageous method compared to supercritical fluid maceration and extraction (SFE), yielding a wide variety of compounds. Conclusion: Overall, this review aims to provide scientists and companies interested in Morus nigra L. with opportunities and challenges for innovation in this field.

Comparative Study on the Impact of Different Extraction Technologies on Structural Characteristics, Physicochemical Properties, and Biological Activities of Polysaccharides from Seedless Chestnut Rose (Rosa sterilis) Fruit.

Seedless chestnut rose (Rosa sterilis S. D. Shi, RS) is a fresh type of R. roxburghii Tratt with copious functional components in its fruit. Polysaccharides are recognized as one of the vital bioactive compounds in RS fruits, but their antioxidant and hypoglycemic properties have not been extensively explored. Hence, in this study, accelerated solvent extraction (RSP-W), citric acid (RSP-C), 5% sodium hydroxide/0.05% sodium borohydride (RSP-A), and 0.9% sodium chloride (RSP-S) solution extraction were individually utilized to obtain RS fruit polysaccharides. The physicochemical properties, structural characteristics, and biological activities were then compared. Results indicated that extraction methods had significant influences on the extraction yield, uronic acid content, monosaccharide composition, molecular weight, particle size, thermal stability, triple-helical structure, and surface morphology of RSPs apart from the major linkage bands and crystalline characteristics. The bioactivity tests showed that the RSP-S, which had the greatest amount of uronic acid and a comparatively lower molecular weight, exhibited more potent antioxidant and α-glucosidase inhibitory property. Furthermore, all RSPs inhibited α-glucosidase through a mixed-type manner and quenched their fluorescence predominantly via a static quenching mechanism, with RSP-S showing the highest binding efficiency. Our findings provide a theoretical basis for utilizing RSPs as functional ingredients in food industries.

An Eco-Friendly Extraction and Purification Approach for Obtaining Active Ingredients for Cosmetics from Two Marine Brown Seaweeds.

Brown seaweeds are attracting attention due to their richness in bioactive compounds, in particular, their phlorotannins. We present here a case study of two Fucales, Ascophyllum nodosum and Halidrys siliquosa, sustainably collected, to produce active polyphenols for the cosmetics sector. Phenolic contents of crude extracts, obtained by Accelerated Solvent Extraction (ASE), were more elevated in H. siliquosa at 100.05 mg/g dry weight (DW) than in A. nodosum (29.51 mg/g DW), considering 3 cycles with cell inversion. The temperature of extraction for a high phenolic content and high associated antioxidant activities close to positive controls was 150 °C for both algae and the use of only one cycle was enough. A semi-purification process using Solid-phase Extraction (SPE) was carried out on both ASE crude extracts (one per species). The majority of phlorotannins were found in the ethanolic SPE fraction for A. nodosum and the hydroethanolic one for H. siliquosa. The SPE process allowed us to obtain more concentrated fractions of active phenolic compounds (×1.8 and 2 in A. nodosum and H. siliquosa, respectively). Results are discussed in regard to the exploitation of seaweeds in Brittany and to the research of sustainable processes to produce active natural ingredients for cosmetics.

Extraction of Antioxidant Compounds from Eugenia uniflora L. Leaves by Energized Dispersive Guided (EDGE) System

The leaves of Pitanga (Eugenia uniflora L.) present recognized antioxidant potential that has practical applications in pharmaceuticals, food, perfume, agrochemical, and cosmetic industries. The Energized Dispersive Guided Extraction (EDGE) system, which combines dispersive solid-phase extraction with the Accelerated Solvent Extraction system, was employed in "combined mode" with extraction cycles to obtain antioxidant compounds from Pitanga leaves. The results showed that extraction cycles with different solvents produce similar extraction yields. At the same time, their ability to scavenge free DPPH radicals exhibited variations according to the polarity of the extraction solvent. Thus, acetone was the optimal solvent for extracting antioxidant compounds from E. uniflora leaves in the combined mode.

Optimization of accelerated solvent extraction of zeaxanthin from orange paprika using response surface methodology and an artificial neural network coupled with a genetic algorithm

Optimization of accelerated solvent extraction of zeaxanthin from orange paprika using response surface methodology and an artificial neural network coupled with a genetic algorithm

Halogenated organic pollutants (HOPs) in marine fish collected from central-northern coastal waters in Vietnam

ABSTRACT In this work, three groups of halogenated organic pollutants (HOPs) including polybrominated diphenyl ethers (PBDEs), polychlorinated biphenyls (PCBs) and organochlorine compounds (OCPs) were analysed simultaneously in twenty-six fish species from coastal waters along the North and Central of Vietnam. Samples were randomly collected, dry-free freeze for pre-treatment, extracted by accelerated solvent extraction combined with cleaning up on multi-layers silica gel column before analysing on the GC-MS/MS system. The concentration of analytes was quantified by internal standard method and controlled with corresponding label standards. The decreasing order of HOP concentrations was ∑20OCPs (mean/median: 158/139 ng/g-wet weight (ww), range: 31.1-406 ng/g-ww) > ∑28PCBs (mean/median: 46.6/36.5 ng/g-ww, range: 5.92-225 ng/g-ww) > ∑8PBDEs (mean/median: 28.7/4.76 ng/g-ww, range: 0.26-212 ng/g-ww). The mean concentration of BDE-209 was the highest distribution (76.5%) in PBDE group, followed by BDE-154 (6.6%), and BDE-153 (5.7%). For PCBs group, hexa-CBs were the most contribution among PCBs and up to 26.1%, followed by Penta-CBs (24.4%), and Tetra-CBs (18.2%) in concentration. The mean concentration of ∑DDTs, accounting to 61.6% of total OCPs, contributed the highest level in this OCP group. The ratio of (DDE+DDD)/DDT in all samples was higher than 1, showing that DDTs were mainly derived from historical. The equivalent toxicity (TEQ) values of 12 dl-PCBs in all samples ranged between 1.1-5.9 ng TEQ/g-ww. The estimated daily intake (EDI) is lower than the Acceptable Daily Intake (ADI) set by FAO/WHO, 1975 (20,000 ng/kg-bw/d for DDTs and 5,000 ng/kg-bw/d for γ-BHC). Intakes of HOPs through the consumption of the marine fish from the studied areas might not subject about health risks to residents living of the coastal areas. However, it is important to know current pollution status and further control marine food pollution in Vietnam as well as propose the appropriate solutions to improve this issue.

Optimization of accelerated solvent extraction, ultrasound assisted and supercritical fluid extraction to obtain carnosol, carnosic acid and rosmarinic acid from rosemary

Antioxidant activities of rosemary (Rosmarinus officinalis L.) are related to the amount of phenolic compounds, mainly carnosol (C), carnosic acid (CA) and rosmarinic acid (RA). In this study, it was aimed to optimize the process conditions of accelerated solvent extraction (ASE), ultrasound assisted extraction (UAE), supercritical CO2 extraction (SFE) of rosemary to obtain the high amount of total C and CA in extract. A Box-Behnken design was applied to investigate and optimize the process variables. De-oiled rosemary by hydrodistillation, was used in the extractions. The amounts of C+CA were 18.92 mg/100 mg for ASE, 17.63 mg/100 mg for UAE, and 26.96 mg/100 mg for SFE at optimum conditions, respectively. The extract yields were 13.98% for ASE, 13.73% for UAE and %19.40 for SFE at optimum conditions. The results of antioxidant activity tests were almost the same for ASE and UAE, these were almost 2 fold higher for SFE than that of ASE and UAE. ASE, UAE and SFE were clean and environmentally friendly, green extraction techniques for extraction of C+CA in rosemary.

Novel Sustainable Alternatives for the Study of the Chemical Composition of Cork

Cork is a natural and renewable material extracted from the cork oak Quercus suber L. (1) Background: The cellular structure and chemical composition of the plant wall give cork its physical and mechanical properties. Chemically, the composition of cork is principally dominated by the presence of suberin as the main structural cell wall component and affected by its close association with other components. The usual chemical analysis of cork has been partially adapted from wood and other lignocellulosic analytical methods and it is a method with extensive procedures. This study aims to (i) find quicker and more sustainable methods for testing the cork chemical composition, (ii) conduct extraction tests using alternative techniques, (iii) optimize alternative methodologies, and (iv) validate the proposed sustainable methodologies. (2) Methods: Microwave-assisted extraction (MAE) and accelerated solvent extraction (ASE) are explored as alternative systems to the traditional method. The percentages of the extractives obtained via MAE are lower than the percentages obtained by means of the classical composition. (3) Results: However, the percentages of suberin are very similar in both methods: 46.39% in the case of the classical composition and 45.11% in the case of microwave-assisted extraction. No significant differences are observed between the content of the extractives in the dichloromethane, ethanol, and water obtained via ASE and the results obtained with the classical methodology. (4) Conclusions: MAE and ASE are faster methods; they use less solvents and provide more reproducible results than the classical chemical composition methodology. These data pave the way for novel sustainable alternatives relative to the studies of the chemical composition of cork.

Evaluating the Antioxidant and Antidiabetic Properties of Medicago sativa and Solidago virgaurea Polyphenolic-Rich Extracts.

The present study evaluated the antioxidant and antidiabetic properties of Medicago sativa and Solidago virgaurea extracts enriched in polyphenolic compounds. The extracts were obtained by accelerated solvent extraction (ASE) and laser irradiation. Then, microfiltration was used for purification, followed by nanofiltration used to concentrate the two extracts. The obtained extracts were analyzed to determine their antioxidant activity using DPPH radical scavenging and reducing power methods. The antidiabetic properties have been investigated in vitro on a murine insulinoma cell line (β-TC-6) by the inhibition of α-amylase and α-glucosidase. M. sativa obtained by laser irradiation and concentrated by nanofiltration showed the highest DPPH• scavenging (EC50 = 105.2 ± 1.1 µg/mL) and reducing power activities (EC50 = 40.98 ± 0.2 µg/mL). M. sativa extracts had higher inhibition on α-amylase (IC50 = 23.9 ± 1.2 µg/mL for concentrated extract obtained after ASE, and 26.8 ± 1.1), while S. virgaurea had the highest α-glucosidase inhibition (9.3 ± 0.9 µg/mL for concentrated extract obtained after ASE, and 8.6 ± 0.7 µg/mL for concentrated extract obtained after laser extraction). The obtained results after evaluating in vitro the antidiabetic activity showed that the treatment with M. sativa and S. virgaurea polyphenolic-rich extracts stimulated the insulin secretion of β-TC-6 cells, both under normal conditions and under hyperglycemic conditions as well. This paper argues that M. sativa and S. virgaurea polyphenolic-rich extracts could be excellent natural sources with promising antidiabetic potential.

Evaluation of Polyphenolic Profile and Antioxidant Activity of Sea Buckthorn (Elaeagnus rhamnoides (L.) A. Nelson) Leaf and Berry Extracts Obtained via Optimized Microwave-Assisted and Accelerated Solvent Extraction

The aim of this study was to optimize parameters of microwave-assisted extraction (MAE) and accelerated solvent extraction (ASE) in terms of extraction temperature and time, microwave power and cycle numbers on the phenolic content of sea buckthorn leaves and berries, using 70% ethanol (v/v) as an extraction solvent. The characterization of phenolic composition in leaf and berry extracts obtained at optimal MAE and ASE conditions was performed with UPLC/ESI-MS2, while antioxidant activity was determined using the ORAC method. The optimal extraction conditions for MAE were 60 °C, 500 W and 15 min for leaves and 60 °C, 300 W, and 10 min for berries. The optimal extraction conditions for ASE from both leaves and berries were 120 °C, 15 min, and 3 cycles. Total phenolic content (TPC) in MAE and ASE extracts from leaves was similar to the TPC determined in extracts obtained by conventional extraction (60 °C/30 min); however, ASE contributed to the higher TPC of the berry extracts. The flavonols kaempferol-3-rutinoside in the leaves and kaempferol in the berries were the most abundant phenols of sea buckthorn. A higher antioxidant activity was found in the leaf extracts obtained by ASE and it correlated with the phenolic content. In general, ASE favored the extraction of all polyphenols from leaves, while MAE was more suitable for the extraction of flavonols from berries, suggesting that the choice of the optimal extraction method is crucial with regard to the target molecules and future applications.

Matrix solid-phase dispersion extraction of organophosphorus flame retardants in soil based on response surface methodology

Organophosphorus flame retardants (OPFRs) are widely used in commercial products owing to their exceptional flame-retarding and plasticizing properties. However, OPFRs are also well recognized as emerging persistent organic pollutants (POPs) because of their environmental persistence, biological concentration, and potential toxicity. Thus, the accurate detection of OPFRs in environmental media is critical for analyzing their fate, transport, and ecological risk. However, very few OPFR detection methods are currently available, and the types of OPFRs detected may vary from site to site. In this study, matrix solid-phase dispersion extraction (MSPD), a simple, rapid, and versatile technique for preparing solid, semisolid, liquid, and viscous samples, was combined for the first time with gas chromatography-tandem mass spectrometry (GC-MS/MS) to analyze 10 OPFRs in soil, namely, tripropyl phosphate (TPrP), tri-n-butyl phosphate (TnBP), tri-iso-butyl phosphate (TiBP), tris(2-chloroisopropyl) phosphate (TCIPP), tris(2-chloroethyl) phosphate (TCEP), tris(1,3-dichloro-2-propyl) phosphate (TDCPP), triphenyl phosphate (TPHP), 2-ethylhexyl diphenyl phosphate (EHDPP), triphenylphosphine oxide (TPPO), and trimethylphenyl phosphate (TCP). The GC-MS/MS system was equipped with a Bruker-5MS capillary column coupled with a triple quadrupole mass spectrometer operated in multiple reaction monitoring (MRM) mode. Prior to detection, a mixed standard solution was fortified with 10 ng of13C-PCB208 as an internal standard. The optimal conditions under which MSPD could achieve high selectivity for OPFRs were determined. In addition, single-factor analysis was used to examine the influence of the sorbent (i. e., C18, PSA, Florisil, GCB, and multiwalled carbon nanotubes (MWCNTs)) as well as the dosage, type, and volume of the eluent on the extraction efficiency of the method for the 10 OPFRs. When GCB and ethyl acetate were used as the adsorbent and solvent, respectively, during elution, high extraction recoveries for the OPFRs were achieved. Optimization via response surface methodology (RSM) was adopted to further analyze the impact of three key factors, namely, the adsorbent dosage, eluent volume, and grinding time, as well as their interactions, on OPFR recoveries. Under the optimal conditions of 0.3 g of GCB as the adsorbent, 10 mL of ethyl acetate as the eluent, and 5 min of grinding time, the relative average recovery of the OPFRs was 87.5%. Furthermore, the 10 OPFRs showed good linear relationships under five concentration gradients, with correlation coefficients greater than 0.998. The limits of detection (LODs) and quantification (LOQs) were calculated as signal-to-noise ratios (S/N) of 3 and 10, respectively, and found to be in the ranges of 0.006-0.161 and 0.020-0.531 ng/g, respectively. The performance of the proposed method was verified by determining the recoveries and relative standard deviations (RSDs) of the OPFRs in soils spiked at low, medium, and high levels (10, 20, and 100 ng/g, respectively). The recoveries of the OPFRs ranged from 70.4% to 115.4%, with RSDs ranging from 0.7% to 6.7%. Compared with the conventional accelerated solvent extraction (ASE) method, MSPD presents higher efficiency, simpler operation, and less solvent requirements. The developed method was applied to determine OPFRs in soil samples collected from different sites in Suzhou, including an electronics factory, an auto-repair factory, a paddy field, and a school field. The results revealed that the contents of OPFRs in the soils from the electronics and auto-repair factories were significantly higher than those in the soils from the paddy and school fields. The main pollutants in the soil samples collected from the electronics and auto-repair factories were TCIPP, TPPO, TCEP, and TDCPP. Moreover, the contents of these compounds were 5.30, 4.44, 4.54, and 4.20 ng/g, in soils from the electronics factory and 2.70, 3.93, 7.60, and 5.04 ng/g, in soils from the auto-repair factory. To the best of our knowledge, this study is the first to determine high concentrations of TPPO in industrial soils. Thus, the combination of MSPD and GC-MS/MS adopted in this study can provide useful insights into the detection of the 10 OPFRs in soil.

Cellulose fibers and ellagitannin-rich extractives from rambutan (Nephelium Lappaceum L.) peel by an eco-friendly approach

This study assesses the viability of an accelerated solvent extraction technique employing environmentally friendly solvents to extract ellagitannins while producing cellulose-rich fibers from rambutan peel. Two sequential extraction protocols were investigated: 1) water followed by acetone/water (4:1, v:v), and 2) acetone followed by acetone/water (4:1, v:v), both performed at 50 °C. The first protocol had a higher extraction yield of 51 %, and the obtained extractives featured a higher total phenolic (531.4 ± 22.0 mg-GAE/g) and flavonoid (487.3 ± 16.9 mg-QE/g) than the second protocol (495.4 ± 32.8 mg-GAE/g and 310.6 ± 31.4 mg-QE/g, respectively). The remaining extractive-free fibers were processed by bleaching using either 2 wt% sodium hydroxide with 3 wt% hydrogen peroxide or 4–5 wt% peracetic acid. Considering bleaching efficiency, yield, and process sustainability, the single bleaching treatment with 5 wt% of peracetic acid was selected as the most promising approach to yield cellulose-rich fibers. The samples were analyzed by methanolysis to determine the amount and type of poly- and oligosaccharides and studied by 13C solid-state nuclear magnetic resonance spectroscopy and thermal gravimetric analysis. The products obtained from the peels demonstrate significant potential for use in various sectors, including food, nutraceuticals, cosmetics, and paper production.