Determination of organochlorine and organophosphate pesticide residues in fruits, vegetables and sediments.

A method is described for the determination of organochlorine and organophosphate pesticide residues in fruits, vegetables and sediments. The concentrated solvent extract was sealed in a polymeric membrane tube, dialysed in cyclohexane and the solvent replaced with hexane. The organophosphates were analysed on a specific thermionic detector without further clean-up. For the organochlorine pesticides the extract was eluted through 3 g of alumina and analysed on GC/ECD. The clean-up for sediment extract was carried out on a 10 g alumina column with 100 mL hexane containing 5% acetone and the eluate was concentrated to 5 mL. The detection limit for organophosphates on a 40 g sample and a final volume of 10 mL was on the average 0.01 mg/kg. The detection limit for organochlorine pesticides, with the final volume of 25 mL, was 0.005 mg/kg for all pesticides except for p,p'-DDT and endosulfan sulphate, which was 0.01 mg/kg. The detection limit for organochlorine pesticides in sediment, with the final volume of 2 mL, was less than 1 microgram/kg and for organophosphate pesticides less than 10 micrograms/kg when the final volume was made to 0.5 mL. At the detection limits the method produced a very high coefficient of variation for both organochlorine and organophosphate pesticides.     

Determination of organochlorine and organophosphate pesticide residues in fruits,vegetables and sediments

Abstract

A method is described for the determination of organochlorine and organophosphate pesticide residues in fruits, vegetables and sediments. The concentrated solvent extract was sealed in a polymeric membrane tube, dialysed in cyclohexane and the solvent replaced with hexane. The organophosphates were analysed on a specific thermionic detector without further clean‐up. For the organochlorine pesticides the extract was eluted through 3 g of alumina and analysed on GC/ECD. The clean‐up for sediment extract was carried out on a10 g alumina column with 100 mL hexane containing 5% acetone and the eluate was concentrated to 5 mL.

The detection limit for organophosphates on a 40 g sample and a final volume of 10 mL was on the average 0.01 mg/kg. The detection limit for organochlorine pesticides, with the final volume of 25 mL, was 0.005 mg/kg for all pesticides except for p,p'‐DDT and endosulfan sulphate, which was 0.01 mg/kg.

The detection limit for oganochlorine pesticides in sediment, with the final volume of 2 mL, was less than 1 μg/kg and for organophosphate pesticides less than 10 μg/kg when the final volume was made to 0.5 mL. At the detection limits the method produced a very high coefficient of variation for both organochlorine and organophosphate pesticides.     

Validating a nondestructive optical method for apportioning colored particulate matter into black carbon and additional components

Exposure of black carbon (BC) is associated with a variety of adverse health outcomes. A number of optical methods for estimating BC on Teflon filters have been adopted but most assume all light absorption is due to BC while other sources of colored particulate matter exist. Recently, a four-wavelength-optical reflectance measurement for distinguishing second hand cigarette smoke (SHS) from soot-BC was developed (Brook et al., 2010; Lawless et al., 2004). However, the method has not been validated for soot-BC nor SHS and little work has been done to look at the methodological issues of the optical reflectance measurements for samples that could have SHS, BC, and other colored particles. We refined this method using a lab-modified integrating sphere with absorption measured continuously from 350 nm to 1000 nm. Furthermore, we characterized the absorption spectrum of additional components of particulate matter (PM) on PM(2.5) filters including ammonium sulfate, hematite, goethite, and magnetite. Finally, we validate this method for BC by comparison to other standard methods. Use of synthesized data indicates that it is important to optimize the choice of wavelengths to minimize computational errors as additional components (more than 2) are added to the apportionment model of colored components. We found that substantial errors are introduced when using 4 wavelengths suggested by Lawless et al. to quantify four substances, while an optimized choice of wavelengths can reduce model-derived error from over 10% to less than 2%. For environmental samples, the method was sensitive for estimating airborne levels of BC and SHS, but not mass loadings of iron oxides and sulfate. Duplicate samples collected in NYC show high reproducibility (points consistent with a 1:1 line, R(2) = 0.95). BC data measured by this method were consistent with those measured by other optical methods, including Aethalometer and Smoke-stain Reflectometer (SSR); although the SSR looses sensitivity at filter loadings above 90 ng/mm(2). Furthermore, positive correlations (R(2) = 0.7) were observed between EC measured by NIOSH Method 5040 on quartz filters and BC measured in co-located Teflon filter samples collected from both heating and non-heating seasons. Overall, the validation data demonstrates the usefulness of this method to evaluate BC from archived Teflon filters while potentially providing additional component information.     

Studies into the formation of dioxins in the sintering process used in the iron and steel industry. 1. Characterisation of isomer profiles in particulate and gaseous emissions

Dioxin analyses using a DB5MS chromatography column are presented for samples of dust from an electrostatic precipitator and emissions from the main stack of a UK sinter plant. The analyses have been repeated using the SP2331 column, for which the elution order has been determined for the whole range of tetra to octachlorodibenzo-p-dioxins and dibenzofurans, and which provides a larger degree of separation than the DB5MS column. Polychlorinated dibenzofurans are present in significantly larger amounts in both the dust and stack emissions, and are the main contributors to the I-TEQ. Analysis using the SP2331 column for dioxins show considerable similarity to those of Bacher et al. for soot from a wood-burning fire, but differ markedly from those of Addink et al. for simulation of waste incineration. The similarities to Bacher's results are less for the dibenzofurans. Comparison of absolute concentrations with reported vapour pressures shows the retention of significant dioxin in the dust to involve mechanisms other than pure condensation.     

Evaluation of the thermal/optical reflectance method for quantification of elemental carbon in sediments

The IMPROVE thermal/optical reflectance (TOR) method, commonly used for EC quantification in atmospheric aerosols, is applied to soils and sediments and compared with a thermochemical method commonly applied to these non-atmospheric samples. TOR determines elemental carbon (EC) by an optical method, but it also yields thermally defined EC fractions in a 2% O2/98% He oxidizing atmosphere at 550 degrees C (EC1), 700 degrees C (EC2), and 800 degrees C (EC3). Replicate TOR TC, OC, and EC values exhibited precisions of approximately +/-10% as determined from multiple analyses of the same samples. EC abundances relative to total mass concentrations were within the ranges reported by other methods for diesel exhaust soot, n-hexane soot, wood and rice chars, and coals, as well as for environmental matrices. A direct comparison with the chemothermal (CTO) method of Gustafson et al. for ten soil and sediment samples demonstrated that almost all of the OC and EC1 are eliminated, as is part of the EC2. The CTO soot carbon is bounded by the EC3 and EC2+EC3 fractions of the IMPROVE TOR analysis. It might be possible to adjust these fractions to obtain better agreement between atmospheric aerosol and soil/sediment analysis methods. Given its linking the EC measurement in the atmosphere to sediments, the TOR method will not only provide useful information on the explanation and comparison between different environmental matrices, but also can be used to derive information on global cycling of EC.     

Human health risk assessment of organochlorines associated with fish consumption in a coastal city in China

Food consumption is an important route of human exposure to organochlorines (OCs). In order to assess the potential health risks associated with these contaminants due to fish consumption, five species of fish were collected from a local market in Zhoushan City, an island in the East China Sea. Dioxin-like compounds, such as polychlorinated dibenzo-p-dioxins/ dibenzofurans, in the fish samples were screened by H4IIE-luc cell bioassay, and the concentrations of specific organochlorines were measured by gas chromatograph-electron capture detector (GC-ECD). The bioassay results indicated that concentrations of dioxin-like compounds in the fish samples were below detection limit (0.64 pg/mL). The concentrations of OC pesticides and PCBs ranged from 0.67 to 13 and 0.24 to 1.4 ng/g wet wt., respectively. Significantly, concentrations of p,p'-DDE in fish meat were comparatively high (average 3.9 ng/g wet wt.) compared with the other OC pesticides. The daily fish consumption, based on a dietary survey conducted among 160 local healthy residents, was determined to be 105 g/person. The relevant cancer benchmark concentrations of HCB, dieldrin, chlordane, DDTs and PCBs were 0.36, 0.04, 1.6, 1.7, and 0.29 ng/kg per day, respectively, based on the local diet. The hazard ratios (HRs), based on non-cancer endpoints were all less than 1.0, while the HRs based on cancer were greater than 1.0 for certain contaminants based on the 95th centile concentration in fish tissue.     

Residual levels of DDTs and PAHs in freshwater and marine fish from Hong Kong markets and their health risk assessment

Axial and ventral muscle from 10 each species of freshwater and marine fish purchased from markets in Hong Kong were analyzed for dichlorodiphenyltrichloroethane (total DDTs including DDE, DDD and DDT) and polycyclic aromatic hydrocarbons (PAHs). Among the 10 freshwater fish species, rice field eel (Monopterus albus) showed significantly higher levels of DDTs in both ventral (125 ng/g wet wt) and axial muscle (127 ng/g wet wt) than the other species. The highest concentration of PAHs was detected in catfish (Clarias fuscus), with 24.8 ng/g in ventral muscle and 9.1 ng/g in axial muscle. As to marine fish, snubnose pompano (Trachinotus blochii) showed significantly higher levels of DDT and its metabolites (1018 ng/g in ventral and 409 ng/g wet wt in axial tissues) than all other marine fish species. The overall concentrations of PAHs in marine fish species were 15.5-57.0 ng/g (axial muscle) and 18.1-118 ng/g wet wt (ventral muscle) where yellow seafin (Acanthopeyrus latus) and golden threadfin bream (Nemipterus virgatus) exhibited the highest concentrations of PAHs in the axial and ventral muscles, respectively. In general, results showed that levels of PAHs in Hong Kong market fish was low and do not expect to cause any concern for human consumption. However, the levels of DDTs in fish samples ranged from 1.10 to 1018 ng/g wet wt, and based on a fish consumption rate of 142.2g/day to calculate the screening value of 14.4 ng/g wet wt for human consumption (USEPA, 2000. Guidance for assessing chemical contaminant, data for use in fish advisories, vol. 1: fish sampling and analysis, third ed. EPA 823-R-95-007. Office of Water, Washington, DC), there were 9 out of 20 (45%) muscle samples of freshwater fish species and 14 out of 20 (70%) muscle samples of marine fish species had elevated levels of DDTs exceeded the screening value. It was also suggested to use ventral muscle for detecting concentrations of persistent organic pollutants in fish.     

Optimized method for dissolved hydrogen sampling in groundwater

Dissolved hydrogen concentrations are used to characterize redox conditions of contaminated aquifers. The currently accepted and recommended bubble strip method for hydrogen sampling (Wiedemeier et al., 1998) requires relatively long sampling times and immediate field analysis. In this study we present methods for optimized sampling and for sample storage. The bubble strip sampling method was examined for various flow rates, bubble sizes (headspace volume in the sampling bulb) and two different H2 concentrations. The results were compared to a theoretical equilibration model. Turbulent flow in the sampling bulb was optimized for gas transfer by reducing the inlet diameter. Extraction with a 5 mL headspace volume and flow rates higher than 100 mL/min resulted in 95-100% equilibrium within 10-15 min. In order to investigate the storage of samples from the gas sampling bulb gas samples were kept in headspace vials for varying periods. Hydrogen samples (4.5 ppmv, corresponding to 3.5 nM in liquid phase) could be stored up to 48 h and 72 h with a recovery rate of 100.1+/-2.6% and 94.6+/-3.2%, respectively. These results are promising and prove the possibility of storage for 2-3 days before laboratory analysis. The optimized method was tested at a field site contaminated with chlorinated solvents. Duplicate gas samples were stored in headspace vials and analyzed after 24 h. Concentrations were measured in the range of 2.5-8.0 nM corresponding to known concentrations in reduced aquifers.     

Insights into low fish mercury bioaccumulation in a mercury-contaminated reservoir, Guizhou, China

We examined Hg biogeochemistry in Baihua Reservoir, a system affected by industrial wastewater containing mercury (Hg). As expected, we found high levels of total Hg (THg, 664-7421 ng g(-1)) and monomethylmercury (MMHg, 3-21 ng g(-1)) in the surface sediments (0-10 cm). In the water column, both THg and MMHg showed strong vertical variations with higher concentrations in the anoxic layer (>4m) than in the oxic layer (0-4 m), which was most pronounced for the dissolved MMHg (p < 0.001). However, mercury levels in biota samples (mostly cyprinid fish) were one order of magnitude lower than common regulatory values (i.e. 0.3-0.5 mg kg(-1)) for human consumption. We identified three main reasons to explain the low fish Hg bioaccumulation: disconnection of the aquatic food web from the high MMHg zone, simple food web structures, and biodilution effect at the base of the food chain in this eutrophic reservoir.     

Method for the determination of organophosphate insecticides in water, sediment and biota

A procedure for the determination of 13 organophosphate insecticides (OPs) in water, sediment and biota at low ppb levels is described. Samples were extracted with dichloromethane or acetone/hexane and cleaned up with micro-column silica gel chromatography. Measurements were made by dual capillary column gas chromatography using both nitrogen-phosphorus (NPD) and electron capture (ECD) detection. Recoveries from fortified water samples ranged from 76% to 102% for all sample types. Practical detection limits ranged between 0.003 and 0.029 microg/l in natural water samples, 0.0004-0.005 microg/g w.w. for sediments, and 0.001-0.005 microg/g w.w for biota using the NPD and ECD method. Losses in sediments were experienced when sulphur was removed. Precision and accuracy were not affected in sediment samples where sulphur was not removed.     

Determination of pesticide residues in IPM and non-IPM samples of mango (Mangifera indica)

Studies were conducted to analyze the residue of commonly used pesticides viz. methyl parathion, chloropyrifos, endosulfan, cypermethrin, fenvalerate, carbendazim, imidacloprid and carbaryl in mango, Dashehari variety, integrated pest management (IPM) and non-IPM samples were collected from the IPM and non-IPM orchards, Lucknow, India. We also present a method for the simultaneous determination of these pesticides in mango samples. Residues of methyl parathion, chloropyriphos, endosulfan, cypermethrin, fenvalerate were extracted from the samples with acetone: cyclohexane: ethyl acetate in the ratio 2:1:1 followed by cleanup using neutral alumina. Analysis was performed by gas chromatography-electron capture detector (GC-ECD) with a megabore column (OV-1). Residues of carbendazim, imidacloprid and carbaryl were extracted with acetone and after cleanup, analysis was performed by high performance liquid chromatography (HPLC) using photo diode array (PDA) detector. Recoveries of all the pesticides ranged between 72.7-110.6%, at 0.1 and 1.0 microg g(-1) level of fortification. The residues detected in non-IPM samples of mango were found to be below the prescribed limits of maximum residue limit (MRL) while IPM samples were free from pesticide residues.     

Dietary uptake of polybrominated diphenyl ethers (PBDEs), occurrence and profiles, in aquacultured turbots (Psetta maxima) from Galicia, Spain

Polybromodiphenyl ethers (PBDEs) are one of the many toxic chemicals present in the environment and in the food we eat every day, being fish one of the main sources of persistent organic pollutants in our diet; like other lipid-related contaminants, they are of concern since they can bioaccumulate and biomagnify through the trophic chain. We published a study focused on the dietary uptake of dioxins and furans (PCDD/Fs) and dioxin-like polychlorobiphenyls (dl-PCBs) in a set of samples of Spanish farmed turbot (Blanco et al., 2007). In the present paper, we extend the study to PBDEs to provide more information about the uptake and transfer from feed to fish of halogenated contaminants. PBDEs in the feeds (2.35-4.76 ng g(-1)) were reflected in turbot fillets (0.54-2.05 ng g(-1)): predominant congeners were tetra-BDE 47, penta-BDEs 99 and 100. It is remarkable that tetra-BDE 49, accounting for only 2% in the feed, contributed to 15% of total PBDEs in turbot fillets. Dietary net accumulation values, 30-45%, showed that tri-, tetra-, penta- and hexa-BDEs were as efficiently transferred into turbot as dl-PCBs and tetra- and penta-chlorinated PCDD/Fs. Lipid-normalized biomagnification factors relating concentration in fish and in feed, BMFs>1 were obtained, except for BDE 209. BDE 49 accumulation, 90%, was possibly contributed by metabolism of higher brominated BDEs. Implication in aquaculture management is a need for uncontaminated fish feed to offer safe products.     

Determination of pesticide residues in IPM and non-IPM samples of mango (Mangifera indica)

Studies were conducted to analyze the residue of commonly used pesticides viz. methyl parathion, chloropyrifos, endosulfan, cypermethrin, fenvalerate, carbendazim, imidacloprid and carbaryl in mango, Dashehari variety, integrated pest management (IPM) and non-IPM samples were collected from the IPM and non-IPM orchards, Lucknow, India. We also present a method for the simultaneous determination of these pesticides in mango samples. Residues of methyl parathion, chloropyriphos, endosulfan, cypermethrin, fenvalerate were extracted from the samples with acetone: cyclohexane: ethyl acetate in the ratio 2:1:1 followed by cleanup using neutral alumina. Analysis was performed by gas chromatography-electron capture detector (GC-ECD) with a megabore column (OV-1). Residues of carbendazim, imidacloprid and carbaryl were extracted with acetone and after cleanup, analysis was performed by high performance liquid chromatography (HPLC) using photo diode array (PDA) detector. Recoveries of all the pesticides ranged between 72.7 – 110.6%, at 0.1 and 1.0 μg g^{? 1} level of fortification. The residues detected in non-IPM samples of mango were found to be below the prescribed limits of maximum residue limit (MRL) while IPM samples were free from pesticide residues.     

Determination of sixteen pesticides in peppers using high-performance liquid chromatography/mass spectrometry

A method for the detection and quantification of 16 pesticides: flufenoxuron, fenoxycarb, dimethomorph, acetamiprid, imidacloprid, lufenuron, thiacloprid, thiabendazole, thiophanate-methyl, spinosad, fenbutatin oxide, methoxyfenozide, oxamyl, clothianidin, thiamethoxam and carbendazim has been developed based on high-performance liquid chromatography-mass spectrometry. Pesticide residues were extracted from the samples according to the QuEChERS method which stands for quick, essay, cheap, effective, rugged and safe. Homogenised analytical portions (10 g ± 0.1) of samples of peppers were spiked at two levels (10 and 100 μg kg?1) with a small volume of an appropriate standard mixture solution containing each pesticide. Analyses were performed using electrospray ionization (ESI) and a MSD trap system. Chromatography separation was achieved using a ZORBAX SB-C18 3.5 μm particle size analytical column, 2.1 × 50 mm from Agilent, with gradient elution at a flow-rate of 0.4 mL/min with mobile phases: waters-0.1 % HCOOH-5 mM HCOONH? and MeOH-5 mM HCOONH?. The method has been validated based on the SANCO European Guidelines. Under the optimized conditions the recoveries (n = 7) were in the range 70-110 % with satisfactory precision (CV ≤ 20 %). A linear dynamic range was obtained over a range of concentrations from 10 to 100 μg kg?1 for each of the analytes, with correlation coefficients >0.997.     

Determination of dioxin concentrations in fish and seafood samples using a highly sensitive reporter cell line, DR-EcoScreen cells

There is a strong need for the development of relatively rapid and low-cost bioassays for the determination of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs), and dioxin-like polychlorinated biphenyls (dl-PCBs) in environmental and food samples. In this study, we applied a reporter gene assay using DR-EcoScreen cells (DR-cell assay), which is highly sensitive to dioxins, to the determination of PCDD/Fs and dl-PCBs in fish and seafood samples. The PCDD/Fs and dl-PCBs were extracted from homogenated samples (10 g) of 30 fish and shellfish, purified by clean-up procedure using a multilayered silica gel column and an alumina column, and applied to DR-cell assay. Interestingly, the bioanalytical equivalent (BEQ) values obtained from the DR-cell assay [<0.1 ∼ 5.4 pg BEQ g⁻¹ wet weight (ww)] were closely correlated with the toxicity equivalent (TEQ) values from conventional high-resolution gas chromatography/high-resolution mass spectrometry (HRGC-HRMS) analysis (r² = 0.912), and the slope of regression line was 0.913. Therefore, we multiplied the BEQ values from the DR-cell assay by a conversion coefficient (1.095, the reciprocal of 0.913) to approximate the TEQ values from the HRGC-HRMS analysis. Furthermore, we used this DR-cell assay to perform a prescreening test of PCDD/Fs and dl-PCBs in 16 fish and seafood samples purchased from a supermarket, revealing that a sample from the fatty flesh of a bluefin tuna exceeded 8 pg TEQ g⁻¹ ww (the European Union-tolerance limit). Taken together, these results suggest that the DR-cell assay might be applicable as a rapid and low-cost prescreening method to determine dioxin levels in fish and seafood samples.     

Perfluorinated compounds in whole fish homogenates from the Ohio, Missouri, and Upper Mississippi Rivers, USA

A method for the analysis of 10 perfluorinated compounds (PFCs) in whole fish homogenate is presented and applied to 60 fish samples collected from the Ohio, Missouri, and upper Mississippi Rivers in 2005. Method accuracy ranged between 86 and 125% with limits of quantitation between 0.2 and 10 ng/g wet weight. Intra- and inter-batch precision was generally ±20%. Perfluorooctane sulfonate (PFOS) was the predominant compound identified in these samples, contributing over 80% of total PFC composition in the fish from these rivers, with median PFOS concentrations of 24.4, 31.8, and 53.9 ng/g wet wt in the Missouri, Ohio, and Mississippi Rivers, respectively. Median PFOS levels were significantly (p = 0.01) elevated in piscivorous fish (88.0 ng/g) when compared with non-piscivorous fish (15.9 ng/g). The 10 samples with PFOS concentrations above 200 ng/g were broadly scattered across all three rivers, providing evidence of the widespread presence of this compound in these US waterways.     

Exposure to polybrominated diphenyl ethers associated with consumption of marine and freshwater fish in Hong Kong

Concentrations of polybrominated diphenyl ethers (PBDEs) in market fish have not previously been reported in Hong Kong. Axial and ventral muscles from 10 each common species of freshwater and marine fish purchased from markets in Hong Kong were analyzed for 22 PBDEs. Among the 10 freshwater fish species, spotted snakehead (Channa maculate) contained the highest level of PBDEs in ventral muscle (130 ng g(-1) wet wt.). For marine fish, bigeye (Priacanthus macracanthus) showed significantly higher levels of PBDEs (60.7 ng g(-1)wet wt. in ventral tissue) than all other marine species. The levels of PBDEs in fish samples ranged from 0.53 to 130 ng g(-1)wetwt. The tetrabrominated congener BDE-47 and pentabrominated BDE-99 were the predominant congeners, which accounted for 27% and 30%, respectively, of the total PBDEs. Daily PBDE intake was calculated according to the different fish consumption rate for Hong Kong consumers, and the results ranged from 222 to 1198 ng day(-1) for marine fish and 403-2170 ng day(-1) for freshwater fish. The daily PBDE intake from fish reported here were higher than those reported from the United States (8.94-15.7 ng day(-1)) and Europe (14-23.1 ng day(-1)).     

A novel pretreatment approach for fast determination of organochlorine pesticides in biotic samples

Recent studies have focused on enantiomeric behaviors of chiral organochlorine pesticides (OCPs) in biotic matrix because they provide insights into the biotransformation processes of chiral OCPs. In the present paper, a double in-line column chromatographic method was developed to effectively remove the lipid impurity in different biotic samples for clean-up of OCPs. After an initial Soxhlet extraction of OCPs from the biotic samples by a mixture of acetone and dichloromethane (DCM), dimethyl sulfoxide (DMSO) was directly added to the extract, and low boiling point solvents (acetone and DCM) were then evaporated. OCPs remained in DMSO were eluted via column 1 filled with silicon gel, and subsequently passed through column 2 packed with 15% deactivated florisil. This novel method was characterized by significant time and solvent savings. The recovery rates of alpha-HCH (hexachlorocyclohexane), beta-HCH, gamma-HCH and delta-HCH were 78.5+/-3.1%, 72.4+/-7.7%, 72+/-4.0% and 70.0+/-8.7%, respectively, and 92.5+/-3.8%, 79.7+/-6.7% and 83.4+/-6.5% for 1,1-dichloro-2-(2-chlorophenyl)-2-(4- chlorophenyl) ethylene (o,p'-DDE), 1,1-dichloro-2-(2-chlorophenyl)-2-(4-chloro phenyl)ethane (o,p'-DDD) and 1,1,1-trichloro-2-(2-chlorophenyl)-2-(4-chlorophenyl) ethane (o,p'-DDT), separately. In addition, the separation efficiencies of the target compounds by both achiral and chiral gas chromatographic columns were satisfactory using the established method. Therefore, the double in-line column chromatography was a useful alternative method for pretreatment of OCPs in different biotic samples.     

Detection of indoor PCB contamination by thermal desorption of dust. A rapid screening method?

Although PCB in caulking materials has been forbidden for many years in most of Europe, including Denmark, there has been continued interest to measure PCB levels in the air of contaminated buildings and blood of the occupants (Mengon and Schlatter 1993, Fromme et al. 1996, Ewers et al. 1998, Currado and Harrad 1998, Gabrio et al. 2000). The relatively low priority for investigations of this contamination is probably due to the small quantities inhaled compared to exposure via food, and the rapid metabolism of the most volatile congeners demonstrated by low concentrations of all congeners in the blood of exposed persons (Ewers et al. 1998, Gabrio et al. 2000). There is, however, evidence that PCB containing caulking materials have been used even during the '90s (Fromme et al. 1996). In Denmark, it is estimated that 75 t PCB is still in buildings (Organization of Sealant Branch's Manufacturers and Distributors 2000). During an investigation of dust from buildings with excessive microbial growth (including 35 rooms from 9 buildings), the analysis of semivolatile compounds by thermal desorption-GC/MS of samples from a single building surprisingly revealed large amounts of PCBs containing 3, 4 and 5 chlorine atoms, 10-20 times the amounts found in samples from other buildings. Extraction of the dust by SFE followed by GC/ECD analysis for 12 PCB congeners showed that there was approximately 20 times the total PCB concentrations in dust from the polluted building compared to the levels in the other buildings. Subsequent headspace analysis of caulking material from the polluted building revealed this to be the source. Shelf dust functions as a passive sampling medium and, thus, can be used as a screening method to detect PCB and other semivolatile pollution indoors.