Extraction polyaromatic hydrocarbon

This publication provides several examples of the use of solid-phase extractions for separating analytes from their matrices. Some of the examples included are caffeine from coffee, polyaromatic hydrocarbons from water, parabens from cosmetics, chlorinated pesticides from water, and steroids from hydrocortisone creams. Extracted analytes maybe determined quantitatively by gas (GC) or liquid chromatography (LG). 

Supercritical CO2 has also beea tested as a solveat for the removal of organic contaminants from sod. At 60°C and 41.4 MPa (6,000 psi), more than 95% of contaminants, such as diesel fuel and polychlotinated biphenyls (PCBs), may be removed from sod samples (77). Supercritical CO2 can also extract from sod the foUowiag hydrocarbons, polyaromatic hydrocarbons, chlotinated hydrocarbons, phenols, chlotinated phenols, and many pesticides (qv) and herbicides (qv). Sometimes a cosolvent is required for extracting the more polar contaminants (78). 

Petrick et al. [375] extracted up to 2000 dm3 of Atlantic Ocean waters using various solid resins. Down to 5 ng/dm were determined of chlorinated biphenyls, HCB, DDE, and polyaromatic hydrocarbons in samples taken at depths down to 4000 metres. 

Polyaromatic hydrocarbons, phenols Extraction with methylene dichloride GC-MS, HPLC [530]... 

Sometimes orthogonal offline SPE steps were used prior to online SPE LC/MS/MS. These preparation steps were used to remove interference and concentrate samples. In an application to measure urinary N7-(benzo[a]pyren-6-yl)guanine (BP-6-N7Gua), a biomarker for exposure to polyaromatic hydrocarbons (PAHs), a two-step offline SPE was first performed using Sep-Pak C8 (Waters, Milford, Massachusetts) and Strata SCX (Phenomenex, Torrance, California) cartridges to obtain high sensitivity (Chen et al. 2005). The extracts were applied to an online reversed phase SPE LC/MS system. The lower limit of detection was 2.5 fmol/mL when 10 mL of urine was used. 

The extraction procedure described by Karasek et al. [1] in section 2.1.1.1 has been applied to the determination of polyaromatic hydrocarbons in... 

Robbat et al. [42] carried out on-site detection of polyaromatic hydrocarbons in soils using thermal desorption gas chromatography-mass spectrometry on hexane extracts of soils. 

Analysis of variance was used to assess the effects on polyaromatic hydrocarbons extraction at the 99% confidence level for the four factors varied. The percentage of 14C in the extract and soil residue does not total 100% because of degradation and volatilization during incubation and due to losses during analysis. The data are presented in Table 2.3 and represent the average of the three replicates for the extract or soil residue. 

Significant differences at the 99% confidence level were observed for the extraction technique and for the polyaromatic hydrocarbons concentration in the soil. The average recovery by the Soxhlet technique was 74.5% whereas 62.8% was the average Polytron recovery. A much higher proportion was extracted with polyaromatic hydrocarbons at the 50pg/g level (72.6%) than at the 5pg/g level (64.6%) suggesting that the extraction efficiency is not constant with concentration. 

Fowlie and Bulman [43] have carried out a detailed study of the extraction of anthracene and benzo[tf]pyrene from soil. They carried out a replicated [24] factorial experiment using Soxhlet extraction and Polytron techniques. Soxhlet extraction followed by thin layer chromatography gave higher recoveries of the two polyaromatic hydrocarbons. 

Lagenfeld et al. [48] studied the effect of temperature and pressure on the supercritical fluid extraction efficiencies of polyaromatic hydrocarbons and polychlorobiphenyls in soils. At 50°C raising the pressure from 350 to 650atm had no effect on recoveries. 

Reindt and Hoffler [50] optimized parameters in the supercritical fluid extraction of polyaromatic hydrocarbons from soil. These workers used carbon dioxide -8% methanol for extraction and obtained 88-101% recovery of polyaromatic hydrocarbons in the final high-performance liquid chromatography. 

Barnabas et al. [51] have discussed an experimental design approach for the extraction of polyaromatic hydrocarbons from soil using supercritical carbon dioxide. They studied 16 different polyaromatic hydrocarbons using pure carbon dioxide and methanol modified carbon dioxide. The technique is capable of determining down to lOOmg kgy1 polyaromatic hydrocarbons in soils. 

Tena et al. [52] carried out a screening of polyaromatic hydrocarbon types in soil by on-line fibre optic interfaced supercritical fluid extraction spectrofluorimetry. 

The apparatus incorporates a fibre optic interface for the spectrofluorimetric measurement on the supercritical carbon dioxide emerging from the extraction cell of a supercritical fluid extractor, prior to depressurization from up to 350 bar. Recoveries of polyaromatic hydrocarbons are between 89 and 107%, and measurements can be carried on with a relative standard deviation of less than 5%. 

Huettenhain and Windrich [57] described a novel extraction method for polyaromatic hydrocarbons in soil in which the samples were first modified by grinding with silica gel to destroy the interaction between the analytes... 

Lopez-Avila et al. [59] used microwave assisted extraction to assist the extraction of polyaromatic hydrocarbons from soils. Another extraction method was described by Hartmann [60] for the recovery of polyaromatic hydrocarbons in forest soils. The method included saponification of samples in an ultrasonic bath, partitioning of polyaromatic hydrocarbons into hexane, extract cleanup by using solid-phase extraction, and gas chromatography-mass spectrometric analysis using deuterated internal standards. Polyaromatic hydrocarbons were thermally desorbed from soils and sediments without pretreatment in another investigation [61]. 

Readman et al. [70] used flame ionization capillary gas chromatography to determine polyaromatic hydrocarbons in extracts of rivers Mersey, Dee and Tamar estuary sediments. 

Tan [71] devised a rapid simple sample preparation technique for analysing polyaromatic hydrocarbons in sediments. Polyaromatic hydrocarbons are removed from the sediment by ultrasonic extraction and isolated by solvent partition and silica gel column chromatography. The sulphur removal step is combined into the ultrasonic extraction procedure. Identification of polyaromatic hydrocarbon is carried by gas chromatography alone and in conjunction with mass spectrometry. Quantitative determination is achieved by addition of known amounts of standard compounds using flame ionization and multiple ion detectors. 

Lee et al. [74] used UV spectroscopy to identify polyaromatic hydrocarbons in river sediments. The procedure involved the collection of sediments, air drying in the dark, sieving, and extraction for organic content. This was followed by column chromatography (silica gel with cyclohexane as eluent), followed by a second chromatographic step with Sephadex LH-20 and propan-2-ol as eluent. The eluate was then concentrated under vacuum and prepared for ultraviolet analysis. 

Saber et al. [75] reported on the quantitative determination of polyaromatic hydrocarbons in extracts of lacustrine sediments using high resolution Shpol skii Spectrofluorimetry at 10°K. 

Langenfeld et al. [48] also compared supercritical monochlorofluoromethane, nitrogen dioxide and carbon dioxide for the extraction of polyaromatic hydrocarbons from sediments. Monochlorodifluoromethane provided the highest recoveries. 

Dunn and Stich [78] and Dunn [79] have described a monitoring procedure for polyaromatic hydrocarbons, particularly benzo[a]pyrene in marine sediments. The procedures involve extraction and purification of hydrocarbon fractions from the sediments and determination of compounds by thin layer chromatography and fluorometry, or gas chromatography. In this procedure, the sediment was refluxed with ethanolic potassium hydroxide, then filtered and the filtrate extracted with isooctane. The isooctane extract was cleaned up on a florisil column, then the polyaromatic hydrocarbons were extracted from the isoactive extract with pure dimethyl sulphoxide. The latter phase was contacted with water, then extracted with isooctane to recover polyaromatic hydrocarbons. The overall recovery of polyaromatic hydrocarbons in this extract by fluorescence spectroscopy was 50-70%. 

Lopez-Avila et al. [25] studied the microwave assisted extraction of polyaromatic hydrocarbons, phenols and organochlorine insecticides from standard reference soils and sediments. 

The microwave assisted extraction for organic compounds including polyaromatic hydrocarbons, phenols and organochlorine insecticides, described in section 11.1.8 [25] has been applied to sediments. The application of supercritical fluid extraction to the determination of various insecticides in soils described in section 11.1.7 [23] has been applied to river sediments. 

Japenga et al. [56] determined polychlorinated biphenyls and chlorinated insecticides in River Elbe estuary sediments by a procedure in which the sediments were pretreated with acetic acid, mixed with silica and Soxhlet-extracted with benzene/hexane. Humic material and elemental sulphur were removed by passing the extract through a chromatographic column containing basic alumina, on which sodium sulphite and sodium hydroxide were adsorbed. Silica fractionation was followed by gas chromatography to analyse chlorinated pesticides, polychlorinated biphenyls and polyaromatic hydrocarbons. Recovery experiments with standard solutions gave recoveries of 90-102%. 

The Basic Extractive Sludge Treatment (B.E.S.T. ) process is an ex situ solvent extraction technology. The B.E.S.T. process uses one or more secondary or tertiary amines, such as diisopropylamine, to separate contaminants from soil, sediment, and sludge. This technology is applicable to most organics or oily contaminants, including polychlorinated biphenyls (PCBs), polyaromatic hydrocarbons (PAHs), pesticides, herbicides, dioxins, furans, and other organic compounds. 

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