Comparison of extraction techniques for isolation of steroid oestrogens in environmentally relevant concentrations from sediment

The comparison of four extraction techniques for isolation of five native and one labelled steroid oestrogens from sediment was described. The three conventional extraction techniques Soxhlet warm extraction (SWE), accelerated solvent extraction (ASE), microwave-assisted extraction (MAE) and a promising technique QuEChERS were tested for isolation of low environmentally relevant oestrogen concentrations using different extraction conditions. The least expensive and time-consuming method QuEChERS provided the best extraction recoveries (53–84%) from all techniques. MAE achieved the highest recovery from conventional techniques for less polar oestrogens using dichloromethane: acetone 3:1 mixture as an extraction solvent (50–71%), but for extraction of the whole group of oestrogens including more polar estriol acetone or methanol must be used. ASE provided higher extraction recoveries using dichloromethane at 60°C (53–74%) for less polar oestrogens. However, the repeatability of results was unsatisfactory and recoveries using other extraction conditions were lower than for MAE. The most time-consuming SWE achieved the worst extraction recoveries and for isolation of low oestrogen concentrations from sediments, it is completely unsuitable.     

Application of water as a solvent in microwave-assisted extraction for analysis of PCBs and CBzs in fly ash

Polychlorinated biphenyls (PCBs) and chlorobenzenes (CBzs) are two classes of dioxin precursors formed in municipal solid waste incinerators (MSWIs); they produce negative health effects similar to those of dioxins. Reducing the analytical time required for determining the concentrations of these compounds in MSWIs is important for quickly evaluating their importance and assessing associated health risks. In the present study, water is used as a safe and environmentally friendly solvent in microwave-assisted extraction (MAE) for PCB and CBz analyses. MAE is compared with traditional Soxhlet extraction (SE) to determine the extraction efficiencies. The evaluation of extraction efficiencies shows that MAE has a high extraction efficiency compared with that of SE when water content is lower than 60%. Furthermore, the extraction time and organic solvent consumption are reduced with MAE compared with SE.     

Comparison of extraction methods for sampling of low molecular compounds in polymers degraded during recycling

The demand for mechanical recycling of plastic waste results in an increasing amount of recycled polymeric materials available for development of new products. In order for recycled materials to find their way into the material market, high quality is demanded. Thereby, a complete and closed loop of polymeric materials can be achieved successfully. The concept of high quality for recycled plastics imply that besides a pure fraction of e.g. polyethylene (PE) or polypropylene (PP), containing only minor trace amount of foreign plastics, knowledge is required about the type and amount of low molecular weight (LMW) compounds. During long-term use (service-life), products made of polymeric materials will undergo an often very slow degradation where a series of degradation products are formed, in parallel, additives incorporated in the matrix may also degrade. These compounds migrate at various rates to the surrounding environment. The release rate of LMW products from plastics depends on the initiation time of degradation and the degradation mechanisms. For polymers the formation of degradation products may be initiated already during processing, and subsequent use will add products coming from the surrounding environment, e.g. fragrance and aroma compounds from packaging. During recycling of plastics, emissions which contain a series of different LMW compounds may reach the environment leading to unwanted exposure to additives and their degradation residues as well as degradation products of polymers.Several extraction techniques are available for sampling of LMW compounds in polymers before chromatographic analysis. This paper reviews and compares polymer dissolution, accelerated solvent extraction (ASE), microwave assisted extraction (MAE), ultrasound assisted extraction (UAE), super critical fluid extraction (SFE), soxhlet extraction, head-space extraction (HS), head-space solid phase micro extraction (HS-SPME), and head-space stir bar sorptive extraction (HSSE) as appropriate sampling methods for LMW compounds in recycled polymers. Appropriate internal standards useful for these kinds of matrices were selected, which improved the possibility for later quantification. Based on the review of extraction methods, the most promising techniques were tested with industrially recycled samples of HDPE and PP and virgin HDPE and PP for method comparison.     

Optimization and Comparative Study of Different Extraction Methods of Sixteen Fatty Acids of Potentilla anserina L. from Twelve Different Producing Areas of the Qinghai-Tibetan Plateau

In this study, supercritical fluid extraction (SFE), ultrasonic-assisted extraction (UAE), and microwave-assisted extraction (MAE) were applied to explore the most suitable extraction method for fatty acids of Potentilla anseris L. from 12 different producing areas of the Qinghai-Tibetan Plateau. Meanwhile, the important experimental parameters that influence the extraction process were investigated and optimized via a Box-Behnken design (BBD) for response surface methodology (RSM). Under optimal extraction conditions, 16 fatty acids of Potentilla anserina L. were analyzed via high-performance liquid chromatography (HPLC) with fluorescence detection, using 2-(4-amino)-phenyl-1-hydrogen-phenanthrene [9,10-d] imidazole as the fluorescence reagent. The results showed that the amounts of total fatty acids in sample 6 by applying SFE, UAE, and MAE were, respectively, 16.58 ± 0.14 mg/g, 18.11 ± 0.13 mg/g, and 15.09 ± 0.11 mg/g. As an environmental protection technology, SFE removed higher amounts of fatty acids than did MAE, but lower amounts of fatty acids than did UAE. In addition, the contents of the 16 fatty acids of Potentilla anserina L. from the 12 different producing areas Qinghai-Tibetan Plateau were significantly different. The differences were closely related to local altitudes and to climatic factors that corresponded to different altitudes (e.g., annual mean temperature, annual mean precipitation, annual evaporation, annual sunshine duration, annual solar radiation.). The temperature indices, photosynthetic radiation, ultraviolet radiation, soil factors, and other factors were different due to the different altitudes in the growing areas of Potentilla anserina L., which resulted in different nutrient contents.     

Comparison of accelerated solvent extraction with microwave-assisted extraction and Soxhlet for the extraction of chlorinated biphenyls in soil samples

The extraction and determination of chlorinated biphenyls (CBs) in soils and solid wastes is an ongoing subject of study. This is an overview article that compares the microwave-assisted extraction (MAE) and accelerated solvent extraction (ASE) techniques. The extraction of CBs by ASE has been optimised taking into account the variation of pressure, temperature and extraction time by means of experimental design and the Simplex approach. The recoveries obtained under the optimum conditions are compared and discussed with those obtained from MAE and Soxhlet extractions.     

Evaluation of Soxhlet extraction, accelerated solvent extraction and microwave-assisted extraction for the determination of polychlorinated biphenyls and polybrominated diphenyl ethers in soil and fish samples

Three commonly applied extraction techniques for persistent organic chemicals, Soxhlet extraction (SE), accelerated solvent extraction (ASE) and microwave-assisted extraction (MAE), were applied on soil and fish samples in order to evaluate their performances. For both PCBs and PBDEs, the two more recent developed techniques (ASE and MAE) were in general capable of producing comparable extraction results as the classical SE, and even higher extraction recoveries were obtained for some PCB congeners with large octanol-water partitioning coefficients (K_ow). This relatively uniform extraction results from ASE and MAE indicated that elevated temperature and pressure are favorable to the efficient extraction of PCBs from the solid matrices. For PBDEs, difference between the results from MAE and ASE (or SE) suggests that the MAE extraction condition needs to be carefully optimized according to the characteristics of the matrix and analyte to avoid degradation of higher brominated BDE congeners and improve the extraction yields.     

Dispersive solid-phase extraction clean up combined with Soxhlet extraction for the determination of 16 PAHs in soil samples by GC-MS

Dichloromethane soil samples extracts were prepared using Soxhlet extraction technique, and after clean-up step, gas chromatography-mass spectrometry analysis of 16 priority polycyclic aromatic hydrocarbons (PAHs) was carried out. A comparison of dispersive solid-phase extraction (dSPE) and column chromatography (cC), as clean-up techniques, was evaluated. Six different sorbents (silica, diatomaceous earth, primary–secondary amine, C18, clinoptilolite and florisil) were tested as dispersive clean-up sorbents versus activated silica and alumina for cC. Best results for three concentration levels among dSPE were obtained using diatomaceous earth, with recovery values in the range of 75–112% for 13 of 16 analysed compounds, while cC recoveries were in the range of 75–111% for all analysed PAHs. Analysis of 12 soil samples from urban area of Ni? (Serbia) singled out acenaphthene as the most abundant compound.     

Coupled solid phase extraction–supercritical fluid extraction–on-line gas chromatography of explosives from water

A method has been developed for the quantitative extraction of nitrotoluenes (2,3-dinitrotoluene, 2,4-dinitrotoluene and trinitrotolugene) from water using a Bakerbond^TM phenyl sorbent. The average solid phase extraction recoveries for spiked standards ranged from 80 to 95 percent for reagent water and 52 to 95 percent from well and surface water in the low ppb and ppt levels. After the nitrotoluenes had been trapped on the solid sorbent they were quantitatively eluted using SFE. Adding toluene to the extraction cell increased the rate of extraction, but did not improve analyte recovery versus unmodified CO₂. The extracts were analyzed off-line with GC–ECD using an internal standard. Extraction losses were due to analyte breakthrough, and not from poor SFE recoveries. This demonstrates that supercritical fluid extraction is a suitable elution technique for analytes trapped on solid phase extraction sorbents. Also, a method for the direct on-line coupling of SPE to GC, using SFE, has been developed and evaluated. Supercritical CO₂ is ideal for directly coupling SPE to GC, since carbon dioxide is a gas under ambient conditions. One potential problem of on-line SPE–SFE–GC is the presence of residual water trapped on the active sites of the Bakerbond¹³ phenyl sorbent. This problem was dealt with by using a split interface previously described by Hawthorne. From the results of this study, the relative standard deviation of the on-line SPE–SFE–GC interface was determined to be between 4 and 10 percent. In addition, there was no significant difference in the precision of the method with or without the use of an internal standard. A calibration curve was also constructed (r² = 0.995) from spiked controls, demonstrating that the method is quantitative.     

Comparison of extraction techniques for quantitative analysis of pendimethalin from soil and rice grain

The paper exploits the development, optimization, and comparison of fast, efficient, quantitative analytical extraction techniques such as ultrasonic-assisted extraction (UAE) and matrix solid-phase dispersion (MSPD) for proficient extraction of pendimethalin from soil and rice samples. Residues of pendimethalin were quantified using high-performance liquid chromatography. Impact of several experimental parameters of UAE and MSPD techniques on extraction of pendimethalin from soil and rice samples was also evaluated. Under the optimized conditions, the mean percent recoveries obtained from both methods were in the range of 80.3–101.3 and 81.7–103.1, respectively, with relative standard deviation <10. Linearity was in the range of 0.003–5.0?µg?mL^?1 with limit of detection and limit of quantification as 0.001 and 0.003?µg?g^?1, respectively. MSPD method was found superior in terms of low solvent consumption, small sample size, and reduced matrix coextracts due to simultaneous extraction and cleanup steps. Both extraction methodologies were successfully applied in monitoring routine soil and rice samples, in which pendimethalin residues (0.003–0.007?µg?g^?1) were detected in few rice samples while residues in soil samples were below the quantification limit.     

Extraction of polycyclic aromatic hydrocarbons and organochlorine pesticides from soils: a comparison between Soxhlet extraction, microwave-assisted extraction and accelerated solvent extraction techniques

The methods of simultaneous extraction of polycyclic aromatic hydrocarbons (PAHs) and organochlorine pesticides (OCPs) from soils using Soxhlet extraction, microwave-assisted extraction (MAE) and accelerated solvent extraction (ASE) were established, and the extraction efficiencies using the three methods were systemically compared from procedural blank, limits of detection and quantification, method recovery and reproducibility, method chromatogram and other factors. In addition, soils with different total organic carbon contents were used to test the extraction efficiencies of the three methods. The results showed that the values obtained in this study were comparable with the values reported by other studies. In some respects such as method recovery and reproducibility, there were no significant differences among the three methods for the extraction of PAHs and OCPs. In some respects such as procedural blank and limits of detection and quantification, there were significant differences among the three methods. Overall, ASE had the best extraction efficiency compared to MAE and Soxhlet extraction, and the extraction efficiencies of MAE and Soxhlet extraction were comparable to each other depending on the property such as TOC content of the studied soil. Considering other factors such as solvent consumption and extraction time, ASE and MAE are preferable to Soxhlet extraction.     

Supercritical fluid extraction of oxadixyl from food crops

Summary This work describes the study of a degradation curve of Oxadixyl in field-treated potato and tomato samples. The residues were extracted using classical and supercritical fluid (SFE) extraction methods and analyzed by HRGC/ECD. The extraction techniques were compared and the results indicate the advantages of using SFE as an alternative method for pesticide analyses in these samples.     

Supercritical fluid extraction of polychlorinated dibenzo-p-dioxins from municipal incinerator fly ash

The supercritical fluid extraction of polychlorinated dibenzo-p-dioxins from an incinerator fly ash sample has been investigated; supercritical nitrous oxide and its mixtures with methanol and toluene were employed as mobile phases. Recoveries of individual polychlorinated dibenzo-p-dioxins congeners were calculated from results of analysis of ¹³C-labeled dioxins by high resolution GC-MS employing selected ion monitoring. The extraction procedure was compared with extraction in a Soxhlet apparatus, which is currently used as a standard method for removing chlorinated dibenzo-p-dioxins from fly ash samples: the results indicated that the time required for the extraction and clean-up can be reduced from 24 to 2.5 hours/sample. Quantitative recovery of the chlorinated dibenzo-p-dioxins was achieved at μg/kg levels, the relative standard deviation was between 1.8 and 5.8%. The use of a virtually inert fluid such as pure nitrous oxide provides significant improvement over conventional extraction procedures because no solvent residue is left in the processed extract.     

Direct injection of seawater for the analysis of nitroaromatic explosives and their degradation products by micellar electrokinetic chromatography

Practical considerations for the injection and separation of nitroaromatic explosives in seawater sample matrices are discussed. The use of high surfactant concentrations and long electrokinetic injections allows for improved detection limits. Sensitivity was enhanced by two mechanisms, improved stacking at the detector-side of the sample plug and desorption of analyte from the capillary wall by surfactant-containing BGE from the inlet side of the sample plug. Calculated limits of detection (S/N = 3) for analytes prepared in pure seawater were 70–800 ppb with injection times varying from 5 to 100 s.     

Comparison of the Phytochemical Composition and Antibacterial Activities of the Various Extracts from Leaves and Twigs of Illicium verum

Previous studies have revealed the numerous biological activities of the fruits of Illicium verum; however, the activities of its leaves and twigs have remained undiscovered. The study aimed to investigate the phytochemical components and antibacterial activity of the various extracts from the leaves and twigs of Illicium verum. The herbal extracts were prepared by supercritical CO₂ extraction (SFE) and 95% ethanol extraction, followed by partition extraction based on solvent polarity. Analysis of antimicrobial activity was conducted through the usage of nine clinical antibiotic- resistant isolates, including Staphylococcus aureus, Pseudomonas aeruginosa and Acinetobacter baumannii. Among the tested samples, the SFE extracts exhibited broader and stronger antibacterial activities against the test strains, with a range of MIC between 0.1–4.0 mg/mL and MBC between 0.2–4.5 mg/mL. Observations made through scanning electron microscopy revealed potential mechanism of the antimicrobial activities involved disruption of membrane integrity of the test pathogens. Evaluation of the chemical composition by gas chromatography-mass spectrometry indicated the presence of anethole, anisyl aldehyde, anisyl acetone and anisyl alcohol within the SFE extracts, demonstrating significant correlations with the antibacterial activities observed. Therefore, the leaves and twigs of Illicium verum hold great potential in being developed as new natural antibacterial agents.     

Comparison of Extraction Techniques and Surfactants for the Isolation of Total Polyphenols and Phlorotannins from the Brown Algae Lobophora variegata

Abstract

Surfactant-mediated extraction (SME), pressurized liquid extraction (PLE), and enzyme-assisted extraction (EAE) have been compared to improve the isolation of phlorotannins from the brown algae Lobophora variegata. Enzymatic treatment with Alcalase 2.4?L FG, Carezyme 4500?L, protease from Streptomyces griseus, pectinase from Aspergillus niger, Celluclast 1.5?L, protease from Bacillus licheniformis; surfactant extraction with triacetin and guaiacol and PLE with ethanol:water as extracting solvent, have been studied in terms of total phenolic content by the Folin–Ciocalteu method and total phlorotannin content using the DMBA assay. The results showed that SME yields the highest amount of phenols and phlorotannins by using food grade guaiacol as the surfactant. An extraction protocol was developed to maximize the amount of extract obtained from L. variegata. The effects of various parameters such as the type of surfactant, efficacy of surfactant, and optimum pH, on the extraction efficiency of polyphenols were examined. The simultaneous use of the enzyme and surfactant was also investigated. However, a synergistic effect between the enzymes and the surfactant for the extraction of polyphenols has not been observed. Considering total phenols and total phlorotannins in the extract, the extraction yield were obtained for total phenols as SME?>?EAE?>?PLE and for total phlorotannins as SME?>?PLE?>?EAE.     

微波辅助萃取-气相色谱/串联质谱法快速测定纺织品中禁用有机磷阻燃剂

以丙酮为萃取溶剂,采用微波辅助萃取技术对纺织品中禁用有机磷阻燃剂进行萃取,萃取液进行气相色谱/串联质谱测定,从而建立了一种微波萃取-气相色谱/串联质谱分析方法,对纺织品中禁用有机磷阻燃剂进行了测定。6种禁用有机磷阻燃剂三-(1-氮杂环丙烯基)氧化膦(TEPA)、三-(2-氯乙基)磷酸酯(TCEP)、三-(2,3-二氯丙基)磷酸酯(TDCP)、二-(2,3-二溴丙基)磷酸酯(DDBPP)、三-(邻甲苯基)磷酸酯(TOCP)和三-(2,3-二溴丙基)磷酸酯(TRIS)的线性范围分别为9.17~366.80、0.95~75.98、1.04~83.20、41.60~832.00、3.80~75.90、40.48~809.60 ?g/L,在S/N=10的条件下,检出限分别为3.0、0.2、0.3、25.0、2.5、29.0 ?g/kg。方法精密度为3.80~8.79 %,回收率为82.62~96.88 %。气相色谱/串联质谱母离子和子离子一一对应的多反应监测模式有效地去除了基体杂质干扰和假阳性现象。该方法简便快速、灵敏度高,定性准确,可完全满足纺织品中禁用有机磷阻燃剂的检测要求。     

Development of a method for the rapid determination of pentachlorophenol in leather using supercritical fluid extraction with in situ derivatization

Pentachlorophenol (PCP) was extracted from leather with supercritical carbon dioxide and in situ acetylated under static SFE conditions in the presence of triethylamine. During the dynamic extraction step, the derivatives were removed from the matrix and collected with either a pure liquid (light petroleum) or a liquid-solid (light petroleum-solid sorbent (C18, alumina, Florisil or Celite)) trap. To prevent restrictor plugging, a suitable restrictor was designed. The clean-up of the extracts was optimized in this study. Different internal standards were tested and it was shown that not all of them were usable. The SFE results were compared with those obtained by Soxhlet extraction with methanol. With SFE instead of conventional Soxhlet extraction, the overall time required for determination of PCP in leather can be reduced from about 2 days to approx. 3 hours.     

Optimization of microwave-assisted extraction for alizarin and purpurin in Rubiaceae plants and its comparison with conventional extraction methods

A simple and rapid microwave-assisted extraction (MAE) procedure was developed and optimized for two common color pigments, alizarin and purpurin, in various samples of Rubiaceae plants. Several variables that can potentially affect the extraction efficiency, namely temperature, methanol concentration in the extractant mixture, time, and solvent volume were optimized by means of a central composite design approach. The results suggest that temperature and methanol concentration in the solvent mixture are statistically the most significant factors. The separation and quantitative determination of the pigments was carried out in less than 6 min by a developed high-performance liquid chromatographic method with UV detection at 250 nm. Under optimum operating conditions, MAE showed significantly higher recoveries than those obtained by the conventional extraction methods (ultrasonic and reflux extraction), ranging from 84 to 94%. In addition, a drastic reduction of the extraction time (20 min versus 6 h) and solvent consumption (20 versus 100 mL) was achieved with a reproducibility (RSDs < 10%) comparable with that provided by the reflux extraction as a reference method.