Selective pressurized liquid extraction of polychlorinated biphenyls in sediment.

A selective pressurized liquid extraction procedure (SPLE) was developed for a fast determination of polychlorinated biphenyls in sediment. The final method was performed at 100 degrees C with heptane/dichloromethane (90:10, v/v) as extraction solvent for 2x5 min. Sulfuric acid impregnated silica was placed downstream of the sample in the extraction cell to remove interfering components. This simultaneous extraction/clean-up was performed in 20 min, with an average congener recovery of 92% compared to a classical 24 h Soxhlet methodology and 2 h of external manual clean-up.     

Direct ultrasonic agitation for rapid extraction of organic matter from airborne particulate

Direct ultrasonic extraction (DUE) is proposed as simple and rapid sample pretreatment method. This new approach is applied to the extraction of particulate organic matter (POM) from airborne particulate by using dichloromethane (DCM) or DCM/methanol (90/10, v/v) as extractant. The analytical determination was carried out by weighing the extractable POM on an electrobalance. Total recovery for POM could be obtained when the sample was extracted three times with 25–50 mL extractant each for about 5 min at 50 W ultrasonic power. In comparison with conventional Soxhlet extraction, less extraction time (total 15 min only) and solvent consumption(100 mL) were required by DUE. The efficiency of the DUE was similar or even higher than the routine Soxhlet method. Additionally, the new extractor is very simple and easy to use and can accelerate the extraction procedures of organic components from various solid samples.     

Direct ultrasonic agitation for rapid extraction of organic matter from airborne particulate

Direct ultrasonic extraction (DUE) is proposed as simple and rapid sample pretreatment method. This new approach is applied to the extraction of particulate organic matter (POM) from airborne particulate by using dichloromethane (DCM) or DCM/methanol (90/10, v/v) as extractant. The analytical determination was carried out by weighing the extractable POM on an electrobalance. Total recovery for POM could be obtained when the sample was extracted three times with 25-50 mL extractant each for about 5 min at 50 W ultrasonic power. In comparison with conventional Soxhlet extraction, less extraction time (total 15 min only) and solvent consumption (100 mL) were required by DUE. The efficiency of the DUE was similar or even higher than the routine Soxhlet method. Additionally, the new extractor is very simple and easy to use and can accelerate the extraction procedures of organic components from various solid samples.     

Microwave-assisted extraction of phenolics from Canarium album L. and identification of the main phenolic compound

Microwave-assisted extraction (MAE) was applied in the extraction of phenolics from Canarium album L. Effects of various conditions including the solvent, solvent to material ratio, microwave power and irradiation time on extraction yield of phenolics were investigated. In terms of the optimal conditions of MAE, it was concluded that 70% (v/v) of ethanol was the proper extraction solvent, the solvent to material ratio was 10 : 1 (mL : g), and the microwave power and irradiation time were 600 W and 15 s, respectively. Compared with normal stirring extraction and ultrasound-assisted extraction, the MAE of phenolics from C. album L. was more time efficient and gave a high extraction rate. More than 1.2% extraction yield was achieved with MAE, and the purity of the phenolics in the extract product was up to 25%. In addition, by ultraviolet-visible (UV) spectrometry and electrospray ionised mass spectrometry (ESI/MS), the main phenolic compound in the extract product was identified as gallic acid.     

Determination of the oil content of seeds by focused microwave-assisted soxhlet extraction

Sumamry Soybean, rape and sunflower lipids have been extracted with a focused microwave-assisted Saxhlet extractor. The main factors affecting extraction efficiency, namely microwave irradiation power, number of cycles and microwave irradiation time were optimised by means of a power, number of cycles and microwave irradiation time were optimised by means of a central composite design based on a two-level-three-factor factorial design. A study of the influence of particle size on the extraction procedure was also performed. The results obtained were compared with those obtained by use of an ISO method using a conventional Soxhlet extractor. Quantitative results for lipid content based on gravimetric determinations and qualitative results based on analysis of fatty acid methyl esters and polymeric compounds were similar to those obtained by Soxhlet extraction with hexane. Substantial reduction of sample manipulation. analysis time and solvent wastage is achieved by use of the proposed method.     

微波萃取土壤中PAHs的研究

研究了MK-1型光纤压力自控微波溶样系统用于微波萃取的可行性.以合成土样为对象,比较系统地研究了微波萃取PAHs的条件、萃取效率以及溶剂、水分、土壤基体物质等因素的影响.在微波作用下丙酮-正已烷(体积比为1:1)和二氯甲烷对PAHs的萃取能力相近;试样中小于20%的水分使丙酮-正己烷(体积比为1:1)的萃取能力提高,而水分高于5%则使二氯甲烷的萃取能力略有降低.在选定条件下,萘、苊烯、芴、菲、蒽、(出)、苯并(a)芘的回收率在82.2%～94.1%之间.     

Comparison of techniques for the extraction of the anti-cancer drug camptothecin from Nothapodytes foetida

Extraction methods using stirring extraction, Soxhlet extraction, ultrasonic extraction and microwave-assisted extraction (MAE) were evaluated for the percentage extraction of camptothecin (CPT) and 9-methoxycamptothecin (9-Me-CPT) from Nothapodytes foetida. The extracts were analyzed by high performance liquid chromatography (HPLC). Methanol (90%, v/v) extracted high percentage extraction of CPT and 9-Me-CPT compared to ethanol (90%, v/v). The results shows that the percentage extraction of CPT and 9-Me-CPT from N. foetida by MAE was more efficient in short time followed by Soxhlet extraction, ultrasonic and stirring extraction methods. Maximum percentage extraction of CPT (2.67%, w/w) was obtained by MAE technique. MAE has need of 3 min, whereas ultrasonic extraction, Soxhlet extraction and stirring extraction techniques require 30, 120 and 30 min, respectively to leach higher percentage extraction of CPT and 9-Me-CPT. The times taken by the microwave extraction process was 40 times less than the Soxhlet extraction for percentage extraction of alkaloids. The present results show that the extraction efficiency and considerable saving of time by MAE was more competent than the other extraction techniques.     

Microwave-assisted extraction of oxymatrine from Sophora flavescens

In this paper, microwave-assisted extraction (MAE) of oxymatrine from Sophora flavescens were studied by HPLC-photodiode array detection. Effects of several experimental parameters, such as concentration of extraction solvent, ratio of liquid to material, microwave power, extraction temperature, and extraction time on the extraction efficiencies of oxymatrine were evaluated. The optimal extraction conditions were 60% ethanol, a 20:1 (v/v) ratio of liquid to material and extraction for 10 min at 50 °C under 500 W microwave irradiation. Under the optimum conditions, the yield of oxymatrine was 14.37 mg/g. The crude extract obtained could be used as either a component of some complex traditional medicines or for further isolation and purification of bioactive compounds. The results, which indicated that MAE is a very useful tool for the extraction of important phytochemicals from plant materials, should prove helpful for the full utilization of Sophora flavescens.     

Optimization of microwave-assisted extraction of hydrocarbons in marine sediments: comparison with the Soxhlet extraction method

Microwave energy was applied to extract polycyclic aromatic hydrocarbons (PAHs) and linear aliphatic hydrocarbons (LAHs) from marine sediments. The influence of experimental conditions, such as different extracting solvents and mixtures, microwave power, irradiation time and number of samples extracted per run has been tested using real marine sediment samples; volume of the solvent, sample quantity and matrix effects were also evaluated. The yield of extracted compounds obtained by microwave irradiation was compared with that obtained using the traditional Soxhlet extraction. The best results were achieved with a mixture of acetone and hexane (1:1), and recoveries ranged from 92 to 106%. The extraction time is dependent on the irradiation power and the number of samples extracted per run, so when the irradiation power was set to 500 W, the extraction times varied from 6 min for 1 sample to 18 min for 8 samples. Analytical determinations were carried out by high-performance liquid chromatography (HPLC) with an ultraviolet-visible photodiode-array detector for PAHs and gas chromatography (GC) using a FID detector for LAHs. To test the accuracy of the microwave-assisted extraction (MAE) technique, optimized methodology was applied to the analysis of standard reference material (SRM 1941), obtaining acceptable results.     

Microwave-assisted solvent extraction and gas chromatography ion trap mass spectrometry procedure for the determination of persistent organochlorine pesticides (POPs) in marine sediment

Microwave-assisted solvent extraction of persistent organochlorine pesticides (POPs) in marine sediment was developed and optimized by means of two-level factorial designs. Six variables (microwave power, extraction time and temperature, amount of sample, solvent volume, and sample moisture) were considered as factors in the optimization process. The results show that the amount of sample to be extracted and solvent volume are statistically significant for the overall recovery of the studied pesticides, although compromise conditions have to be established with the object of avoiding overpressure in closed vessels. After extraction, a clean up step including the use of a silica cartridge was performed prior to chromatographic determination in order to remove interferences. The optimized procedure was compared to conventional Soxhlet extraction. The MS-MS ion preparation mode was applied to improve the sensitivity and selectivity of the chromatographic technique.     

Pressurized liquid extraction in determination of polychlorinated biphenyls and organochlorine pesticides in fish samples

Pressurized liquid extraction (PLE) is a relatively new technique applicable for the extraction of persistent organic pollutants from various matrices. The main advantages of this method are short time and low consumption of extraction solvent. The effects of various operational parameters (i.e. temperature of extraction, number of static cycles and extraction solvent mixtures) on the PLE efficiency were investigated in this study. Fish muscle tissue containing 3.2% (w/w) lipids and native polychlorinated biphenyls (PCBs), organochlorine pesticides (OCPs) and other related compounds was used for testing. Purification of crude extracts was carried out by gel permeation chromatography employing Bio-Beads S-X3. Identification and quantitation of target indicator PCBs and OCPs was performed by high-resolution gas chromatography (HRGC) with two parallel electron-capture detectors (ECDs). Results obtained by the optimized PLE procedure were compared with conventional Soxhlet extraction (the same extraction solvent mixtures hexane–dichloromethane (1:1 v/v) and hexane–acetone (4:1 v/v) were used). The recoveries obtained by PLE operated at 90–120 °C were either comparable to “classic” Soxhlet extraction (for higher-chlorinated PCB congeners and DDT group) or even better (for lower chlorinated analytes). The highest recoveries were obtained for three static 5 min extraction cycles.     

Optimization of microwave-assisted extraction of hydrocarbons in marine sediments: comparison with the Soxhlet extraction method

Microwave energy was applied to extract polycyclic aromatic hydrocarbons (PAHs) and linear aliphatic hydrocarbons (LAHs) from marine sediments. The influence of experimental conditions, such as different extracting solvents and mixtures, microwave power, irradiation time and number of samples extracted per run has been tested using real marine sediment samples; volume of the solvent, sample quantity and matrix effects were also evaluated. The yield of extracted compounds obtained by microwave irradiation was compared with that obtained using the traditional Soxhlet extraction. The best results were achieved with a mixture of acetone and hexane ¶(1?:?1), and recoveries ranged from 92 to 106%. The extraction time is dependent on the irradiation power and the number of samples extracted per run, so when the irradiation power was set to 500 W, the extraction times varied from 6 min for 1 sample to 18 min for 8 samples. Analytical determinations were carried out by high-performance liquid chromatography (HPLC) with an ultraviolet-visible photodiode-array detector for PAHs and gas chromatography (GC) using a FID detector for LAHs. To test the accuracy of the microwave-assisted extraction (MAE) technique, optimized methodology was applied to the analysis of standard reference material (SRM 1941), obtaining acceptable results.     

Optimisation and comparison of microwave-assisted extraction and Soxhlet extraction for the determination of polychlorinated biphenyls in soil samples using an experimental design approach

Optimisation of microwave-assisted extraction (MAE) for the extraction of polychlorinated biphenyls (PCBs) from soil samples has been accomplished using an experimental design approach. Variables studied have been: percentage of acetone (v/v) in an acetone:n-hexane mixture, solvent volume, extraction time, microwave power and pressure inside the extraction vessel. Five samples of a certified soil (CRM 481) have been extracted under the optimum conditions of the developed method and the results have been compared to those obtained by Soxhlet extraction. Good recoveries (>95%) have been obtained for all the PCBs studied. All extracts have been analysed by gas chromatography/mass spectrometry (GC/MS) and an optimum determination method for the electron impact mass spectrometric (EIMS) has also been developed.     

Statistical mixture design optimization of extraction media and mobile phase compositions for the characterization of green tea

The influence of different solvents on the extraction medium and the RP-HPLC mobile phase composition were investigated by statistical mixture designs to optimize solvent proportions to prepare the fingerprint of a medicinal herbal extract. For modeling, the number of peaks was used as a measure of fingerprint information. The optimum compositions of solvent to extract chemical substances from green tea and for mobile phase chromatographic analysis were ethyl acetate/ ethanol/dichloromethane (20:5:75 v/v/v) and MeOH/ACN/water (7.5:57.5:35 v/v/v), respectively. This system results in 26 peaks in the chromatographic fingerprint. These results show that an incorrect choice of modifiers for mobile phase composition and solvent extraction hampers the detection of a maximum number of peaks and produces a poor chromatographic fingerprint.     

Green approach to the extraction of major capsaicinoids from habanero pepper using near-infrared,microwave, ultrasound and Soxhlet methods,a comparative study

A simple method for the extraction of two major capsaicinoids from habanero peppers, using near-infrared irradiation, microwave irradiation or ultrasound as the energy source and ethanol as the solvent, was compared with Soxhlet extraction. The extraction processes were monitored by gas chromatography/mass spectrometry. The new processes offer better overall yields and a higher ratio of capsaicin to dihydrocapsaicin than Soxhlet extraction. The physical effect of the different energy sources on the peppers was determined using scanning electron microscopy. Extraction of capsaicin and dihydrocapsaicin using near-infrared irradiation, which has not been previously reported, was shown to be a simple and efficient alternative extraction procedure.     

A cost effective,sensitive, and environmentally friendly sample preparation method for determination of polycyclic aromatic hydrocarbons in solid samples

A simple, cost effective, and yet sensitive sample preparation technique was investigated for determining Polycyclic Aromatic Hydrocarbons (PAHs) in solid samples. The method comprises ultrasonic extraction, Stir Bar Sorptive Extraction (SBSE), and thermal desorption–gas chromatography–mass spectrometry to increase analytical capacity in laboratories. This method required no clean-up, satisfied PAHs recovery, and significantly advances cost performance over conventional extraction methods, such as Soxhlet and Microwave Assisted Extraction (MAE). This study evaluated three operational parameters for ultrasonic extraction: solvent composition, extraction time, and sample load. A standard material, SRM 1649 a (urban dust), was used as the solid sample matrix, and 12 priority PAHs on the US Environmental Protection Agency (US EPA) list were analyzed. Combination of non-polar and polar solvents ameliorated extraction efficiency. Acetone/hexane mixtures of 2:3 and 1:1 (v/v) gave the most satisfactory results: recoveries ranged from 63.3% to 122%. Single composition solvents (methanol, hexane, and dichloromethane) showed fewer recoveries. Comparing 20 min with 60 min sonication, longer sonication diminished extraction efficiencies in general. Furthermore, sample load became a critical factor in certain solvent systems, particularly MeOH. MAE was also compared to the ultrasonic extraction, and results determined that the 20-min ultrasonic extraction using acetone/hexane (2:3, v/v) was as potent as MAE. The SBSE method using 20 mL of 30% alcohol-fortified solution rendered a limit of detection ranging from 1.7 to 32 ng L⁻¹ and a limit of quantitation ranging from 5.8 to 110 ng L⁻¹ for the 16 US EPA PAHs.     

Sediment Matrix Induced Response Enhancement in the Gas Chromatographic–Mass Spectrometric Quantification of Insecticides in Four Different Solvent Extracts from Ultrasonic and Soxhlet Extraction

The performance of ultrasonic and Soxhlet extraction using hexane, dichloromethane, ethylacetate/methyl-tert-butylether (1/3, v/v) and hexane/acetone (1/1, v/v) for the analysis of seventeen insecticides in sediments was evaluated. The contents of the extracts differed severely. The extracts obtained with ethylacetate/methyl-tert-butylether (1/3, v/v) and hexane/acetone (1/1, v/v) were dark yellow to green, whereas the extracts obtained with dichloromethane and hexane were light yellow and clear respectively. This is due to higher solubility of matrix compounds in ethylacetate/methyl-tert-butylether (1/3, v/v) and hexane/acetone (1/1, v/v). High loads of coextracted matrix compounds lead to matrix effects in the evaporation step of GC–MS measurements. This is known as matrix induced response enhancement effect. Matrix effects and recoveries were checked by analysis of spiked sediments. The suitable choice of extraction method in connection with an appropriate solvent separates the analytes from matrix compounds. Matrix effects are reduced and recoveries of spiked samples are improved.Revised: 6 January and 2 May 2005     

Microwave-assisted extraction of polycyclic aromatic compounds from coal

Microwave-assisted extraction (MAE) of polycyclic aromatic compounds (PACs) from coal is shown to give the same pattern of compounds as Soxhlet extraction. MAE requires only 10 mL solvent and 10 min extraction time whereas Soxhlet uses 200 mL and takes 24 h. Although the yields were lower, dichloromethane (DCM) was preferred to pyridine, N-methyl-2-pyrrolidone (NMP), and NMP with CS2 because the pattern of the PACs is shown to be independent of solvent and DCM is a much more convenient solvent to work with.     

Optimization and comparison of MAE, ASE and Soxhlet extraction for the determination of HCH isomers in soil samples

The microwave-assisted extraction (MAE), accelerated solvent extraction (ASE) and Soxhlet extraction of two isomers of hexachlorocyclohexane, alpha-HCH and gamma-HCH, from a polluted landfill soil have been optimized following different experimental designs. In the case of microwave-assisted extraction, the following variables were considered: pressure, extraction time, microwave power, percentage of acetone in n-hexane mixture and solvent volume. When ASE extraction was studied the variables were pressure, temperature and extraction time. Finally, the percentage of acetone in n-hexane mixture and the extraction time were the only variables studied for Soxhlet extraction. The concentrations obtained by the three extraction techniques were, within their experimental uncertainties, in good agreement. This fact assures the possibility of using both ASE and MAE techniques in the routine determination of lindane in polluted soils and sediments.     

Optimization and comparison of MAE, ASE and Soxhlet extraction for the determination of HCH isomers in soil samples

The microwave-assisted extraction (MAE), accelerated solvent extraction (ASE) and Soxhlet extraction of two isomers of hexachlorocyclohexane, α-HCH and γ-HCH, from a polluted landfill soil have been optimized following different experimental designs. In the case of microwave-assisted extraction, the following variables were considered: pressure, extraction time, microwave power, percentage of acetone in n-hexane mixture and solvent volume. When ASE extraction was studied the variables were pressure, temperature and extraction time. Finally, the percentage of acetone in n-hexane mixture and the extraction time were the only variables studied for Soxhlet extraction. The concentrations obtained by the three extraction techniques were, within their experimental uncertainties, in good agreement. This fact assures the possibility of using both ASE and MAE techniques in the routine determination of lindane in polluted soils and sediments. Received: 28 January 2000 / Revised: 28 March 2000 / Accepted: 31 March 2000