Analysis of polycyclic aromatic hydrocarbons in sediment reference materials by microwave-assisted extraction

The microwave-assisted extraction (MAE) of polycyclic aromatic hydrocarbons (PAHs) from harbor sediment reference material EC-1, marine sediment reference material HS-2 and PAH-spiked river bed soil was conducted. The extraction conditions for EC-1 were carried out at 70 degrees C and 100 degrees C under pressure in closed vessels with cyclohexane acetone (1:1), cyclohexane-water (3:1), hexane acetone (1:1), and hexane-water (3:1) for 10 min. A comparison between MAE and a 16-h Soxhlet extraction (SX) method showed that both techniques gave comparable results with certified values. MAE has advantages over the currently used Soxhlet technique due to a faster extraction time and lower quantity of solvent used. The consumption of organic solvent of the microwave method was less than one-tenth compared to Soxhlet.     

不同萃取方法对长江口边滩多环芳烃萃取效果的影响

选取索氏提取法和加速溶剂萃取仪(ASE)提取法,对长江口边滩样品进行多环芳烃萃取实验,并利用气相色谱/质谱仪对萃取出来的多环芳烃进行定量分析,研究了不同萃取方法以及不同溶剂条件下多环芳烃的总量、分布特征.结果表明,长江口边滩多环芳烃最高值出现在吴淞口;索氏提取法在多环芳烃萃取效果上优于加速溶剂萃取仪提取法;混合溶剂萃取...     

Study of factors affecting on the extraction efficiency of polycyclic aromatic hydrocarbons from soils using open-vessel focused microwave-assisted extraction

As part of an evaluation of focused microwave-assisted extraction (FMAE) using an open-vessel system, the effects of matrix, moisture content, ageing, and solvent have been studied on the extraction efficiency of polycyclic aromatic hydrocarbons (PAHs) from spiked soils. PAHs were spiked onto three different uncontaminated air dried and originally wet soil matrices with 1- and 20-day ageing periods. Solvents used were hexane–acetone (1:1), cyclohexane–acetone (1:1) and dichloromethane. FMAE only required a small amount of solvent (20 ml) and short extraction time (10 min) in the open cell under 90 W of microwave power. The results revealed that the extraction efficiency strongly depends on the nature of soil matrix; moisture content may enhance the recoveries of PAHs for many cases; and, the influence of the type of solvent is not significant. A comparison between microwave extraction and 16-h Soxhlet extraction has been made on spiked soils. It evidenced that the microwave method under ambient pressure is a suitable alternative to Soxhlet method for the analysis of PAHs in soils. For the evaluation of the developed FMAE method, three reference materials were used. The PAHs recovered from three reference materials were in a good agreement with reference values.     

A comparative study on the recovery of polycyclic aromatic hydrocarbons from fly ash and lignite coal

The recovery of polycyclic aromatic hydrocarbons (PAHs) from lignite coal burnt in Greek power stations and the fly ash produced is examined comparatively using Soxhlet, ultrasonic and accelerated solvent extraction procedures with various organic solvents. Soxhlet using toluene/methanol mixture and accelerated solvent extraction/toluene were found to be the most efficient methods for fly ash PAHs, yielding average recoveries of about 80%. The accelerated solvent extraction/toluene procedure was superior for lignite PAHs, yielding 96% average recovery, whereas ultrasonic and Soxhlet extraction yielded relatively lower recoveries (75% and 67%, respectively).     

Improved extraction procedures for polychlorinated biphenyls in solid samples with aqueous sodium hydroxide under autoclave conditions

The efficacy of the extraction of polychlorinated biphenyls (PCBs) from varnish-infiltrated insulating papers as a model of solid materials with an aqueous sodium hydroxide (NaOH) by autoclaving at 121 degrees C for 30 min was compared with those for the conventional procedures, i.e., saponification with 1 N ethanolic NaOH in a boiling water bath for 60 min and extraction with benzene in a Soxhlet apparatus. The newly invented autoclaving method was found to be superior to the conventional ones, yielding approximately 5- to 6-fold cumulative PCB congeners without being accompanied by extended decomposition. Therefore, the autoclave-based sample treatment is recommended for more accurate determination of PCBs in the case of PCB-impregnated solid materials such as hardened oils and resin-coated or -infiltrated papers instead of being treated conventionally.     

Effect of condensed organic matter on solvent extraction and aqueous leaching of polycyclic aromatic hydrocarbons in soils and sediments

The contents of nonhydrolyzable organic matter (NHC) and black carbon (BC) were measured in soils and sediments from the Pearl River Delta, South China. Polycyclic aromatic hydrocarbons (PAHs) were extracted respectively by Soxhlet and an accelerated solvent extraction device (ASE) using different solvents. In addition, sequential aqueous leaching at different temperatures was carried out. The PAH content extracted with the sequential three solvent ASE is two times higher than that using the Soxhlet extraction method. The relationship of the PAH content with the NHC content is very significant. The PAH concentrations measured at various temperature steps fit well to the Van't Hoff equation and the enthalpy was estimated. The investigation indicates that condensed organic matter such as kerogen carbon, aged organic matter, and BC is relevant for the extraction and distribution of native PAHs in the investigated field soils and sediments.     

Fatty acid profile and elemental content of avocado (Persea americana Mill.) oil –effect of extraction methods

Interest in vegetable oil extracted from idioblast cells of avocado fruit is growing. In this study, five extraction methods to produce avocado oil have been compared: traditional solvent extraction using a Soxhlet or ultrasound, Soxhlet extraction combined with microwave or ultra-turrax treatment and supercritical fluid extraction (SFE). Traditional Soxhlet extraction produced the most reproducible results, 64.76 ± 0.24 g oil/100 g dry weight (DW) and 63.67 ± 0.20 g oil/100 g DW for Hass and Fuerte varieties, respectively. Microwave extraction gave the highest yield of oil (69.94%) from the Hass variety. Oils from microwave extraction had the highest fatty acid content; oils from SFE had wider range of fatty acids. Oils from Fuerte variety had a higher monounsaturated: saturated FA ratio (3.45–3.70). SFE and microwave extraction produced the best quality oil, better than traditional Soxhlet extraction, with the least amount of oxidizing metals present.     

Fatty acid profile and elemental content of avocado (Persea americana Mill.) oil--effect of extraction methods

Interest in vegetable oil extracted from idioblast cells of avocado fruit is growing. In this study, five extraction methods to produce avocado oil have been compared: traditional solvent extraction using a Soxhlet or ultrasound, Soxhlet extraction combined with microwave or ultra-turrax treatment and supercritical fluid extraction (SFE). Traditional Soxhlet extraction produced the most reproducible results, 64.76 ± 0.24 g oil/100 g dry weight (DW) and 63.67 ± 0.20 g oil/100 g DW for Hass and Fuerte varieties, respectively. Microwave extraction gave the highest yield of oil (69.94%) from the Hass variety. Oils from microwave extraction had the highest fatty acid content; oils from SFE had wider range of fatty acids. Oils from Fuerte variety had a higher monounsaturated: saturated FA ratio (3.45-3.70). SFE and microwave extraction produced the best quality oil, better than traditional Soxhlet extraction, with the least amount of oxidizing metals present.     

含油污泥中油水含量的 3 种测定方法比较简

利用索氏提取-减量法、减量法和自行开发的高效抽提法,对一系列已知组成的含油污泥进行了油、水含量的测定。测定结果表明,高效抽提法在油、水含量的测定精度方面优于其他2种方法,对于不同组成的含油污泥,由其测定的油含量与含油污泥样品实际油含量的相对偏差均小于5%,由其测定的水含量与含油污泥样品实际水含量的相对偏差均小于7%。在测定效率方面,高效抽提法也优于其他2种方法,40 min即可完成10 g油-水-固质量比为3：2：5含油污泥中油、水含量的测定。     

An alternative supercritical fluid extraction system for aqueous matrices and its application in pesticides residue analysis

Supercritical fluid extraction (SFE) is a rapid and convenient method for the isolation of organic compounds from environmental samples. This paper describes a supercritical carbon dioxide (CO2) extraction system that uses a newly designed extraction cell to recover organic compounds from an aqueous matrix. Analysis of the extracts by gas chromatography-electron capture detector (GC-ECD) indicated that the herbicide trifluralin (2,6-dinitro-N,N-dipropyl-4-trifluoromethylaniline) could be quantitatively extracted by using the SFE system proposed with small amounts of sample. The percentage of recovery obtained with the SFE system described was twice as high as the result obtained using a conventional solid-phase extraction technique. Extraction by SFE was completed in a short period of time using a simple and low-cost home-made system that did not require the use of organic solvents.     

Treatment system for solid matrix contaminated with fluoranthene. I--Modified extraction technique.

A laboratory-scale ultrasonication technique was developed for fluoranthene extraction from soils and sediments where the utilized organic solvent would be recovered after the extraction process. Therefore, the remedied soils and sediments would be free from toxicant and trace of added chemicals. The developed ultrasonication technique outlined here is an integrated part of a complete remediation system consisting of extraction and solar detoxification reactors. This paper investigates extraction efficiencies under different conditions, outlines solvent recovery technique and compares extraction efficiency of the developed ultrasonication technique with a commercially available laboratory-scale sonication bath. The spiked soil sample with fluoranthene (19.4 microg g(-1)) and organic solvent was ultrasonicated at 40 degrees C for 20 min. The sonicated mixture was allowed to settle for 10 min before the extract gravitated into the modified solar reactor for fluoranthene detoxification. The added solvents were removed from the remedied soil before it was released to site. The mixture of cyclohexane and ethanol (CH:ETOH) (3:1) was the favorable solvent from among 10 organic solvents because of its high extraction efficiency, safety and low cost. Preliminary results indicated that the developed extraction technique recovered more than 93% of fluoranthene from soil samples.     

Matrix effects in applying mono- and polyclonal ELISA systems to the analysis of weathered oils in contaminated soil

Commercial mono- and polyclonal enzyme-linked immunosorbent assay (ELISA) systems were applied to the on-site analysis of weathered hydrocarbon-contaminated soils at a former integrated steelworks. Comparisons were made between concentrations of solvent extractable matter (SEM) determined gravimetrically by Soxhlet (dichloromethane) extraction and those estimated immunologically by ELISA determination over a concentration range of 2000-330,000 mg SEM/kg soil dry weight. Both ELISA systems tinder-reported for the more weathered soil samples. Results suggest this is due to matrix effects in the sample rather than any inherent bias in the ELISA systems and it is concluded that, for weathered hydrocarbons typical of steelworks and coke production sites, the use of ELISA requires careful consideration as a field technique. Consideration of the target analyte relative to the composition of the hydrocarbon waste encountered appears critical.     

Characterization of polycyclic aromatic hydrocarbons (PAHs) on lime spray dryer (LSD) ash using different extraction methods

In this study, traditional Soxhlet, automatic Soxhlet and ultrasonic extraction techniques were employed to determine the speciation and concentration of polycyclic aromatic hydrocarbons (PAHs) on lime spray dryer (LSD) ash samples collected from the baghouse of a spreader stoker boiler. To test the efficiencies of different extraction methods, LSD ash samples were doped with a mixture of 16 US EPA specified PAHs to measure the matrix spike recoveries. The results showed that the spike recoveries of PAHs were different using these three extraction methods with dichloromethane (DCM) as the solvent. Traditional Soxhlet extraction achieved slightly higher recoveries than automatic Soxhlet and ultrasonic extraction. Different solvents including toluene, DCM:acetone (1:1 V/V) and hexane:acetone (1:1 V/V) were further examined to optimize the recovery using ultrasonic extraction. Toluene achieved the highest spike recoveries of PAHs at a spike level of 10 microg kg(-1). When the spike level was increased to 50 microg kg(-1), the spike recoveries of PAHs also correspondingly increased. Although the type and concentration of PAHs detected on LSD ash samples by different extraction methods varied, the concentration of each detected PAH was consistently low, at microg kg(-1) levels.     

Addition of surrogate standards in the routine analysis of investigating polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/F)

Conclusion  Independent losses of internal standard by evaporation and/or sorption will increase both absolute and random errors for the native analyte. Thus, the internal standard should only be used for compensation of losses, variations and irregularities in the clean-up, dilution, transfer and instrument. This is achieved by addition of internal standard to the eluent after extraction, or avoiding direct contact between internal standards and suspected active matrices. The analytical results will then not guarantee a correct quantification of the true analyte concentration on the matrix, only maximise the precision of measurement of extracted analyte. In Soxhlet extraction, the internal standard can be added to the solvent reservoir. In supercritical fluid extraction (SFE), the internal standard might be added to an aliquot of reversed phase silica (C-8, C-18) located after the sample in the fluid direction.     

含油污泥中油水含量的3种测定方法比较

利用索氏提取一减量法、减量法和自行开发的高效抽提法,对一系列已知组成的含油污泥进行了油、水含量的测定。测定结果表明,高效抽提法在油、水含量的测定精度方面优于其他2种方法,对于不同组成的含油污泥,由其测定的油含量与含油污泥样品实际油含量的相对偏差均小于5％,由其测定的水含量与含油污泥样品实际水含量的相对偏差均小于7％。在测定效率方面,高效抽提法也优于其他2种方法,40min即可完成10g油一水一固质量比为3：2：5含油污泥中油、水含量的测定。     

Comparison between solid-phase extraction methods for the chromatographic determination of organophosphorus pesticides in water

A solid-phase microextraction (SPME) procedure has been developed to extract eight organophosphorus pesticides (OPs) in water and the method was compared with a conventional solid phase extraction (SPE) technique. The extracted OPs were analyzed by gas chromatography using thermionic specific detection. Both extraction methods presented linear calibration at least over the concentration range investigated (100 to 1000 ng x mL(-1) for SPE and 1 to 100 ng x mL(-1) for SPME). SPME method presented higher sensitivity than SPE. The quantitation limits were between 0.1 to 1.0 ng x mL(-1) for SPME depending upon the analyte, and 100 ng x mL(-1) for SPE. The precision, as measured by the standard deviations (RSD), were in the range 3.6% to 5.8% for SPME and 2.4% to 9.2% for SPE. Along with the feature of being a solvent - free sampling technique, SPME offers additional benefits due to its high sensitivity, simplicity, and small size sample required (typically: SPE - 500 mL, SPME - 5 mL).     

Routine analysis of hydrocarbons, PCB and PAH in marine sediments using supercritical CO2 extraction

Automated Supercritical Fluid Extraction (SFE), using CO2, was tested and optimised for routine analysis of hydrocarbons (THC), polychlorinated biphenyls (PCB) and polycyclic aromatic hydrocarbons (PAH) in marine sediments. The aim of the exercise was to reduce the amount of solvents used and to reduce the manual handling time for each sample. The sediments contained elemental sulphur, which was removed during the extraction step using activated Cu. Similar recoveries and reproducibility where found for THC when conventional solvent extractions and SFE where compared. Modifying the CO2 with methanol was necessary to obtain extraction recoveries similar to conventional extraction methods for PCB and PAH.     

Comparison of supercritical fluid extraction and Soxhlet extraction for the determination of PCBs in seaweed samples

The efficiency of supercritical fluid extraction for the determination of 12 polychlorinated biphenyls from algae samples is compared to Soxhlet extraction. Analytical detection limits for the individual congeners ranged from 0.62 microgl(-1) to 19 microgl(-1). Recovery was tested for both methods using standard addition procedure. At maximum spike level of concentration, the mean recoveries were not significantly different (P>0.05) of all PCBs studied, with the exception of PCBs 28, 52, 77 and 169. Method precision for Soxhlet extraction (< or =3.9%) was slightly better than for SFE (< or =9.2%). Although both methods yield comparable results, SFE offers the advantage of detecting all PCBs studied at lower concentrations, reducing extraction time, and reducing the amount of solvents needed. The optimized methods were applied to the analysis of three real seaweed samples, except for PCB101 the concentrations of all PCBs were low or below the detection limits. The levels of PCB101 found in sample 1 were 6.6+/-0.54 ng g(-1) d.w., in sample 2 the levels were 8.2+/-0.86 ng g(-1) d.w. and in sample 3 they were 7.7+/-0.08 ng g(-1) d.w.     

Evaluation of pressurized liquid extraction for determination of organophosphorus and pyrethroid pesticides in soybean

The purpose of this study was to develop an analytical method for the determination of organophosphorus and pyrethroid pesticides in soybean by pressurized liquid extraction (PLE). Two organic solvents, acetone and acetonitrile, were evaluated as extraction solvents. In both cases, the amount of extract was enhanced with increasing extraction temperature. The extracts obtained using acetonitrile were measured by gas chromatography/mass spectrometry after a cleanup process based on the analytical method for the Japanese Positive List System for Agricultural Chemicals Remaining in Foods. The effect of extraction temperature (range: 40– 130°C) on extraction efficiency was evaluated by a recovery study using 21 organophosphorus pesticides and 10 pyrethroid pesticides as target analytes and acetonitrile as the solvent. The results indicated that at 130°C, some organophosphorus pesticides might be degraded, whereas extraction temperatures between 70°C and 100°C were optimal. Next, a prepared sample containing fenitrothion and permethrin was analyzed. Although the sample was not soaked in water prior to analysis, PLE provided analytical results comparable to those obtained by solvent extraction with homogenization. Therefore, PLE is considered a simple and alternative technique for the extraction of organophosphorus and pyrethroid pesticides in soybean.     

Evaluation of pressurized liquid extraction for determination of organophosphorus and pyrethroid pesticides in soybean

The purpose of this study was to develop an analytical method for the determination of organophosphorus and pyrethroid pesticides in soybean by pressurized liquid extraction (PLE). Two organic solvents, acetone and acetonitrile, were evaluated as extraction solvents. In both cases, the amount of extract was enhanced with increasing extraction temperature. The extracts obtained using acetonitrile were measured by gas chromatography/mass spectrometry after a cleanup process based on the analytical method for the Japanese Positive List System for Agricultural Chemicals Remaining in Foods. The effect of extraction temperature (range: 40- 130°C) on extraction efficiency was evaluated by a recovery study using 21 organophosphorus pesticides and 10 pyrethroid pesticides as target analytes and acetonitrile as the solvent. The results indicated that at 130°C, some organophosphorus pesticides might be degraded, whereas extraction temperatures between 70°C and 100°C were optimal. Next, a prepared sample containing fenitrothion and permethrin was analyzed. Although the sample was not soaked in water prior to analysis, PLE provided analytical results comparable to those obtained by solvent extraction with homogenization. Therefore, PLE is considered a simple and alternative technique for the extraction of organophosphorus and pyrethroid pesticides in soybean.