In-field determination of nanomolar nitrite in seawater using a sequential injection technique combined with solid phase enrichment and colorimetric detection

A novel sequential injection method for the determination of nitrite at nanomolar level in seawater samples has been developed. The pink azo compound was formed based on the Griess reaction and quantitatively adsorbed onto a Sep-Pak C18 cartridge. The enriched azo compound was rinsed with water and ethanol (28%, v/v) in turn, and then eluted with an eluent containing 26.6% (v/v) ethanol and 0.108 mol L⁻¹ H₂SO₄. Finally the azo compound was measured using a spectrophotometer at 543 nm. Under the optimized conditions, the linear calibration ranges were 0.71–42.9 nmol L⁻¹ for a 150-mL sample and 35.7–429 nmol L⁻¹ for a 15-mL sample. The relative standard deviation of 8 measurements was 1.44% for 14.3 nmol L⁻¹ nitrite. For the 150 mL sample, the detection limit was estimated to be 0.1 nmol L⁻¹. The throughput of the method was about 4 samples per hour. The proposed method has been successfully applied to the in-field determination of nanomolar concentrations of nitrite in seawater.     

Single-drop microextraction and gas chromatography–mass spectrometry for the determination of volatile aldehydes in fresh cucumbers

Headspace single-drop microextraction (HS-SDME) was used as a rapid and reliable method for the isolation and preconcentration of volatile aldehydes from fresh cucumbers. The utility of this methodology is demonstrated in the determination of (E)-2-nonenal and (E,Z)-2,6-nonadienal. The limit of detection, linearity and repeatability have been determined for 2,6-nonadienal and (E)-2-nonenal. Limits of detection for nonenal and nonadienal were 0.05 and 0.04 mg kg ⁻¹, respectively. The repeatability of extraction was obtained with the RSD values lower than 13%. Concentrations of target aldehydes in fresh cucumbers obtained by means of the HS-SDME method were in the range 9.4–12.5 (nonadienal) and 2.6–3.8 mg kg ⁻¹ (nonenal). The results of the single-drop extraction in combination with gas chromatography show promising potential for the analysis of volatile aldehydes in vegetables. Presented at the 11th International Conference on Chemistry and the Environment, 9-12 September 2007, Torun, Poland.     

Spectrophotometric determination of triclosan in personal care products

A spectrophotometric method for the determination of triclosan in personal care products was proposed. It was based on the reaction of sodium nitrite with p-sulfanilic acid in an acidic medium to form diazonium ion, with which triclosan further formed an azo compound in an alkaline medium. The resulting yellow colored product has a maximum absorption at 452 nm. A good linear relationship (r = 0.9999) was obtained in the range of 0–30 mg L⁻¹ triclosan. A detection limit of 0.079 g L⁻¹ was achieved and the relative standard deviation was 0.24% (n = 11) at 14 mg L⁻¹ triclosan. The proposed method has been applied to the analyses of triclosan in several personal care products and the results were in good agreement with those obtained by high-performance liquid chromatography.     

Polarographic determination of nitrate in vegetables

A polarographic method for the determination of nitrate in vegetables is presented. The method is based on the reduction of nitrate to nitric oxide which reacts in solution with colbalt (II) and thiocyanate ions forming an electroactive complex that is reduced at the dropping mercury electrode at -0.5 V (vs. SCE). The nitric oxide is generated outside the polarographic cell by addition of ferrous ammonium sulfate and ammonium molybdate in hydrochloric acid to the previously triturated vegetable matrices. The calibration graph was linear in the range of 2-12x10(-6) mol nitrate. The recovery of nitrate in vegetable matrices (broccoli, kale, lettuce, radish, red beet, spinach, turnip and watercress) varied from 85.4 to 107.4 % and the nitrate content, expressed as sodium nitrate, varied from 751 to 10 806 mg kg(-1) of fresh vegetable. The relative standard deviation for the proposed method is lower than 7% and considering a sample of 5.0 g, the determination limit was 39 mg of nitrate per kg fresh vegetable weight. The precision and accuracy of the polarographic method were comparable to those of the reference spectrophotometric method (official AOAC reference method for the determination of nitrate in foodstuffs).     

Comparison of neutron activation analysis with conventional detection techniques for the evaluation of trace elemental contamination in Mallard (<Emphasis Type="Italic">Anas platyrhynchos</Emphasis>) feathers

Instrumental neutron activation analysis (INAA) was used to determine trace elemental contamination in bird feathers. Primary feathers from twelve mallard (Anas platyrhynchos) ducks, migrating through the Thousand Islands region of Ontario, Canada, were analyzed for selenium, mercury, chromium, arsenic and antimony. Certified reference materials were used to assess the quality of the analytical procedure. Quantification of chemical elements was performed using Ortec Gamma Vision software. Five chemical elements were quantified, with corresponding analytical uncertainties of less than 20%. Results indicated the presence of As (max = 0.13 mg kg⁻¹), Cr (max = 2.6 mg kg⁻¹), Hg (max = 7.7 mg kg⁻¹), Sb (max = 0.31 mg kg⁻¹) and Se (max = 1.31 mg kg⁻¹). To assess the validity of using INAA as a quantitative analytical technique for feather samples, two standard reference materials were examined and mercury results were compared to those obtained from both direct mercury analysis (DMA) and cold vapour atomic absorption spectroscopy (CVAAS). Several CVAAS results differed significantly from the INAA results; in many instances CVAAS appeared to under-report when compared to INAA, with relative percent difference values as high as 126%. Conversely, results obtained using DMA compared favourably with INAA. For all samples, RPD values were within 30%. This is the first study to use INAA to examine feather contamination in Canadian migratory waterfowl and the first to corroborate INAA feather results by comparing them to those obtained using CVAAS and DMA.     

Fast quantitation of 5-hydroxymethylfurfural in honey using planar chromatography

An approach for rapid quantitation of 5-hydroxymethylfurfural (HMF) in honey using planar chromatography is suggested for the first time. In high-performance thin-layer chromatography (HPTLC) the migration time is approximately 5 min. Detection is performed by absorbance measurement at 290 nm. Polynomial calibration in the matrix over a range of 1:80 showed correlation coefficients, r, of ≥ 0.9997 for peak areas and ≥ 0.9996 for peak heights. Repeatability in the matrix confirmed the suitability of HPTLC–UV for quantitation of HMF in honey. The relative standard deviation (RSD, %, n = 6) of HMF at 10 ng/band was 2.9% (peak height) and 5.2% (peak area); it was 0.6% and 1.0%, respectively, at 100 ng/band. Other possible detection modes, for example fluorescence measurement after post-chromatographic derivatization and mass spectrometric detection, were also evaluated and can coupling can be used as an additional tool when it is necessary to confirm the results of prior quantitation by HPTLC–UV. The confirmation is provided by monitoring the HMF sodium adduct [M + Na]⁺ at m/z 149 followed by quantitation in TIC or SIM mode. Detection limits for HPTLC–UV, HPTLC–MS (TIC), and HPTLC–MS (SIM) were 0.8 ng/band, 4 ng/band, and 0.9 ng/band, respectively. If 12 μL honey solution was applied to an HPTLC plate, the respective detection limits for HMF in honey corresponded to 0.6 mg kg⁻¹. Thus, the developed method was highly suitable for quantitation of HMF in honey at the strictest regulated level of 15 mg kg⁻¹. Comparison of HPTLC–UV detection with HPTLC–MS showed findings were comparable, with a mean deviation of 5.1 mg kg⁻¹ for quantitation in SIM mode and 6.1 mg kg⁻¹ for quantitation in TIC mode. The mean deviation of the HPTLC method compared with the HPLC method was 0.9 mg kg^-1 HMF in honey. Re-evaluation of the same HPTLC plate after one month showed a deviation of 0.5 mg kg⁻¹ HMF in honey. It was demonstrated that the proposed HPTLC method is an effective method for HMF quantitation in honey.      

Determination of residual monomers in latex by headspace hollow fiber protected liquid-phase microextraction combined with high-performance liquid chromatography

A simple and efficient method based on hollow fiber protected headspace liquid-phase in conjunction with high performance liquid chromatography has been introduced for extraction and determination of three residual monomers (2-ethylhexyl acrylate (EHA), vinyl acetate (VA), glycidyl methacrylate (GM)) in polymer latex. Using this methodology, the analytes of interest extracted from a sample are led into organic solvent located inside the porous hollow fiber membrane. Initially, several experimental parameters were controlled and optimized and the optimum conditions were reached with 8 cm neatly cut hollow fibers containing heptanol, which were exposed to the headspace of a 12 mL sample solution containing 20% (w/v) NaCl thermostated at 110 °C and stirred at 800 rpm for 20 min. Finally, 20 μL of the extraction solution was withdrawn into a syringe and injected into HPLC for analysis. The calibration curves were linear (r² ≥ 0.994) over the concentration range of 0.05-10 mg L⁻¹ for VA and 0.02-10 mg L⁻¹ for other analytes. The relative standard deviation (RSD%) for three-replicate extractions and measurements was below 8.6%. The limits of detection of this method for quantitative determination of the analytes were found within the range of 0.005 to 0.011 mg kg⁻¹ with the enrichment factors within the 5-164 range. The method was successfully applied for determination of residual monomers in polymer latex.     

Sequential injection system for on-line analysis of total nitrogen with UV-mineralization

An automatic method for the determination of total nitrogen in wastewater by sequential injection analysis and mineralization with UV radiation has been developed. The method is based on the mineralization of the samples with sodium persulphate in basic medium under UV radiation. Small volumes of sample and reagents are firstly aspirated into a single channel and then propelled by flow reversal to the UV reactor and then to the detector. The organic and inorganic nitrogen compounds are oxidized to nitrate that is then measured at 226 nm. The sequential injection procedure has been optimized and the factors affecting the efficiency of the oxidation have been studied with a number of test substances with different chemical structures and properties. Solutions in the concentration range 1-56 g l⁻¹ of nitrogen can be analyzed with the described procedure. The sample rate is of 30-40 samples h⁻¹. The LOD is 0.6 mg l⁻¹ N and the reproducibility is 1.8% (28 mg l⁻¹ N). Organic carbon in the form of glucose was added to a number of test solutions to study the potential interference of organic matter.The method was compared with the Kjeldahl digestion method by analyzing 15 wastewater samples with both methods. The nitrate and nitrite content of the non-oxidized samples were subtracted from the corresponding nitrogen content determined after photo-oxidation and the value compared with the Kjeldahl nitrogen content.     

Residue Analysis of Propionylbrassinolide in Fruit and Vegetables by GC–MS

A rapid and simple method for the determination of propionylbrassinolide residues in tomatoes, apples and grapes using GC–MS is reported. Samples were extracted with acetonitrile, and the extracts were analyzed without any further clean-up. The results showed good linearity (r ² > 0.99) with standard solutions over the concentration range of 0.5–50 mg L⁻¹. The LODs and LOQs of propionylbrassinolide were 0.15 and 0.5 mg kg⁻¹ in all samples. Recoveries were in the range of 81.9–111.2%, with corresponding RSDs of 4.6–12.9% for three fortified levels. Intra- and inter-day RSDs were in the ranges of 1.5–14.2% and 5.3–15.6%. It was demonstrated that the proposed method is simple and efficient, and particularly suitable for detecting propionylbrassinolide residues in fruit and vegetables.     

Development of a photochemically induced fluorescence-based optosensor for the determination of imidacloprid in peppers and environmental waters

A novel flow-through solid phase spectroscopic assembly implemented with photochemically induced fluorescence (PIF) has been developed for the rapid, sensitive and selective determination of imidacloprid. The pesticide is derivatized on-line by irradiation with ultraviolet light providing an intensively fluorescent compound. The determination is carried out by measuring the fluorescence intensity of the photoproduct once retained on C₁₈ silica gel filling the flow-cell. The method proposed has been applied to the determination of imidacloprid in natural waters and peppers. The quantification limit (QL) (0.015 mg kg⁻¹) in peppers was lower than the maximum residue limit (MRL) established by Spanish Legislation (0.5 mg kg⁻¹). The method also seems to be suitable for environmental water analysis providing satisfactory recoveries (94.0-108.6%). The results obtained in the analysis of real samples are in good agreement with those provided by a reference liquid chromatography (HPLC) method.     

Residue analysis of four diacylhydrazine insecticides in fruits and vegetables by Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method using ultra-performance liquid chromatography coupled to tandem mass spectrometry

The new analytical method using Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) procedure for simultaneous determination of diacylhydrazine insecticide residues in fruits and vegetables was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS). The four insecticides (tebufenozide, methoxfenozide, chromafenozide, and halofenozide) were extracted from six fruit and vegetable matrices using acetonitrile and subsequently cleaned up using primary secondary amine (PSA) or octadecylsilane (C18) as sorbent prior to UPLC-MS/MS analysis. The determination of the target compounds was achieved in less than 3.0 min using an electrospray ionization source in positive mode (ESI+) for tebufenozide, methoxfenozide, and halofenozide and in negative mode (ESI−) for chromafenozide. The limits of detection were below 0.6 μg kg⁻¹, while the limit of quantification did not exceed 2 μg kg⁻¹ in different matrices. The QuEChERS procedure by using two sorbents (PSA and C18) and the matrix-matched standards gave satisfactory recoveries and relative standard deviation (RSD) values in different matrices at four spiked levels (0.01, 0.05, 0.1, and 1 mg kg⁻¹). The overall average recoveries for this method in apple, grape, cucumber, tomato, cabbage, and spinach at four levels ranged from 74.2% to 112.5% with RSDs in the range of 1.4–13.8% (n = 5) for all analytes. This study provides a theoretical basis for China to draw up maximum residue limits and analytical method for diacylhydrazine insecticide in vegetables and fruits.     

Determination of arsenic (III) and arsenic (V) in freshwater biological samples from Thailand by solvent extraction and neutron activation

Neutron activation analysis (NAA) methods were employed for the determination of total arsenic, and water soluble As(III) and As(V) compounds in freshwater fish/shellfish and plant samples from Southern Thailand. Total arsenic concentrations varied from 0.05 to 425 mg kg⁻¹. Water soluble arsenic species were separated by solvent extraction using ammonium pyrrolidinedithiocarbamate (APDC)/methylisobutylketone (MIBK) followed by NAA. The water soluble As(III) and As(V) levels varied from 0.07 to 26.4 and 0.03 to 22.9 mg kg⁻¹, respectively. The As(III) and As(V) detection limits were 0.007 for fish/shellfish, 0.005 for As(III) and 0.006 mg kg⁻¹ for As(V) in plants. This separation method allows for the determination of water soluble As(III) and As(V) using commonly available and inexpensive laboratory equipment and chemicals, which can be coupled to a variety of quantification techniques.     

Interfacial reaction using particle-immobilized reagents in a fluidized reactor. Determination of glycerol in biodiesel

A novel fluidized beads strategy for utilization of particle-immobilized reagents in flow analysis was developed in this study. The performance of the suggested strategy was demonstrated by the determination of glycerol in biodiesel. This analytical task was used as a proof-of-concept example. The method is based on on-line extraction of glycerol from biodiesel into aqueous stationary phase of extraction-chromatographic column, followed by elution and spectrophotometric determination in the form of copper glycerate formed in a fluidized reactor of stepwise injection system. The floating of cation exchange resin Dowex^® 50WX4, saturated with Cu(II) ions in liquid phase, was accomplished by air-bubbling. The linear range was from 100 to 1000 mg kg⁻¹, and the limit of detection, calculated as 3s of a blank test (n = 5), was found to be 30 mg kg⁻¹. The method was successfully applied to the analysis of biodiesel and biodiesel-blend (B 20) samples.     

Application of manganese(IV) dioxide microcolumn for determination and speciation of nitrite and nitrate using a flow injection analysis-flame atomic absorption spectrometry system

A flow injection (FI) method with flame atomic absorption spectrometry (FAAS) detection was developed for the determination and speciation of nitrite and nitrate in foodstuffs and wastewaters. The method is based on the oxidation of nitrite to nitrate using a manganese(IV) dioxide oxidant microcolumn where the flow of the sample through the microcolumn reduces the MnO₂ solid phase reagent to Mn(II), which is measured by FAAS. The absorbance of Mn(II) are proportional to the concentration of nitrite in the samples. The injected sample volume was 400 μL with a sampling rate of analyses was 90 h⁻¹ with a relative standard deviation better than 1.0% in a repeatability study. Nitrate is reduced to nitrite in proposed FI-FAAS system using a copperized cadmium microcolumn and analyzed as nitrite. The calibration curves were linear up to 20 mg L⁻¹ and 30 mg L⁻¹ with a detection limit of 0.07 mg L⁻¹ and 0.14 mg L⁻¹ for nitrite and nitrate, respectively. The results exhibit no interference from the presence of large amounts of ions. The method was successfully applied to the speciation of nitrite and nitrate in spiked natural water, wastewater and foodstuff samples. The precision and accuracy of the proposed method were comparable to those of the reference spectrophotometric method.     

Homogeneous liquid-liquid extraction combined with gas chromatography-electron capture detector for the determination of three pesticide residues in soils

In this study, a new method was developed for analyzing malathion, cypermethrin and lambda-cyhalothrin from soil samples by using homogeneous liquid–liquid extraction (HLLE) and gas chromatography with electron capture detector (GC–ECD). Acetone was used as extraction solvent for the extraction of target pesticides from soil samples. When the extraction process was finished, the target analytes in the extraction solvent were rapidly transferred from the acetone extract to carbon tetrachloride, using HLLE. Under the optimum conditions, linearity was obtained in the range of 0.05–40 μg kg⁻¹ for malathion, 0.04–10 μg kg⁻¹ for lambda-cyhalothrin and 0.05–50 μg kg⁻¹ for cypermethrin, respectively. Coefficients of correlation (r²) ranged from 0.9993 to 0.9998. The repeatability was carried out by spiking soil samples at concentration levels of 2.5 μg kg⁻¹ for lambda-cyhalothrin, and 10 μg kg⁻¹ for malathion and cypermethrin, respectively. The relative standard deviations (RSDs) varied between 2.3 and 9.6% (n = 3). The limits of detection (LODs), based on signal-to-noise ratio (S/N) of 3, varied between 0.01 and 0.04 μg kg⁻¹. The relative recoveries of three pesticides from soil A1, A2 and A3 at spiking levels of 2.5, 5 and 10 μg kg⁻¹ were in the range of 82.20–91.60%, 88.90–110.5% and 77.10–98.50%, respectively. In conclusion, the proposed method can be successfully applied for the determination of target pesticide residues in real soil samples.     

A green analytical procedure for flow-injection determination of nitrate in natural waters

Nitrate determination in waters is generally carried out with cadmium filings and carcinogenic reagents or by reaction with phenolic compounds in highly concentrated sulfuric acid medium. In this work, it was developed a green analytical procedure for nitrate determination in natural waters based on direct spectrophotometric measurements in ultraviolet, using a flow-injection system with an anion-exchange column for separation of nitrate from interfering species. The proposed method employs only one reagent (HClO₄) in a minimum amount (equivalent to 18 μL concentrated acid per determination), and allowed nitrate determination within 0.50-25.0 mg L⁻¹, without interference of up to 200.0 mg L⁻¹ humic acid; 1.0 mg L⁻¹ NO₂⁻; 200.0 mg L⁻¹ PO₄³⁻; 75.0 mg L⁻¹ Cl⁻; 50.0 mg L⁻¹ SO₄²⁻ and 15.0 mg L⁻¹ Fe³⁺. The detection limit (99.7% confidence level) and the coefficient of variation (n = 20) were estimated as 0.1 mg L⁻¹ and 0.7%, respectively. The results obtained for natural water samples were in agreement with those achieved by the reference method based on nitrate reduction with copperized cadmium at the 95% confidence level.     

Determination of photoirradiated high polar benzoylureas in tomato by HPLC with luminol chemiluminescence detection

This study reports the first analytical application of luminol chemiluminescence reaction for the sensitive detection of two benzoylurea insecticides (diflubenzuron and triflumuron). Off-line experiments demonstrated that previously irradiated traces of these benzoylurea insecticides largely enhanced the chemiluminescence emission yielded from the oxidation of luminol in methanol:water mixtures, by potassium permanganate in alkaline medium, the enhancement being proportional to the concentration of both pesticides. The two benzoylureas were determined in tomato samples by coupling liquid chromatography with post-column photoderivatization and detection based on this chemiluminescence reaction. Tomato samples were extracted using the QuEChERS method based on extraction with acetonitrile and dispersive solid-phase clean-up using primary and secondary amine (PSA). Interferences due to matrix effect were overcome by using matrix-matched standards. The optimised method was validated with respect to linearity, limits of detection and quantification, precision and accuracy. Under the optimised conditions, calibrations graphs were linear between 0.05 and 0.50 μg mL⁻¹ for diflubenzuron and between 0.10 and 1.00 μg mL⁻¹ for triflumuron. Method detection limits were 0.0025 and 0.0131 μg mL⁻¹ (equivalent to 0.0005 and 0.0026 mg kg⁻¹) and quantification limits were 0.05 and 0.10 μg mL⁻¹ (equivalent to 0.01 and 0.02 mg kg⁻¹) for diflubenzuron and triflumuron, respectively. In both cases, quantification limits were lower than the maximum residue levels (MRLs) established by the European legislation. The relative standard deviation of intra-day precision was below 10% and recoveries were between 79.7% and 94.2% for both pesticides.     

Mercury speciation analysis in seafood by species-specific isotope dilution: method validation and occurrence data

Methylmercury (MeHg) and total mercury (THg) in seafood were determined using species-specific isotope dilution analysis and gas chromatography combined with inductively coupled plasma mass spectrometry. Sample preparation methods (extraction and derivation step) were evaluated on certified reference materials using isotopically enriched Hg species. Solid–liquid extraction, derivation by propylation and automated agitation gave excellent accuracy and precision results. Satisfactory figures of merit for the selected method were obtained in terms of limit of quantification (1.2 μg Hg kg⁻¹ for MeHg and 1.4 μg Hg kg⁻¹ for THg), repeatability (1.3–1.7%), intermediate precision reproducibility (1.5% for MeHg and 2.2% for THg) and trueness (bias error less than 7%). By means of a recent strategy based on accuracy profiles (β-expectation tolerance intervals), the selected method was successfully validated in the range of approximately 0.15–5.1 mg kg⁻¹ for MeHg and 0.27–5.2 mg kg⁻¹ for THg. Probability β was set to 95% and the acceptability limits to ±15%. The method was then applied to 62 seafood samples representative of consumption in the French population. The MeHg concentrations were generally low (1.9–588 μg kg⁻¹), and the percentage of MeHg varied from 28% to 98% in shellfish and from 84% to 97% in fish. For all real samples tested, methylation and demethylation reactions were not significant, except in one oyster sample. The method presented here could be used for monitoring food contamination by MeHg and inorganic Hg in the future to more accurately assess human exposure.     

A simple; efficient and environmentally friendly method for the extraction of pesticides from onion by matrix solid-phase dispersion with liquid chromatography-tandem mass spectrometric detection

An evaluation of the extraction of pesticides from onion by matrix solid-phase dispersion (MSPD) with the determination by liquid chromatography tandem mass spectrometry using electrospray as the ionization source (LC-ESI-MS/MS) was carried out. The performance of different sorbents, including reused C18 bonded silica, was evaluated. Different parameters affecting the extraction efficiency were evaluated, such as the type and amount of sorbent, the time of interaction after the fortification step, the time of sample dispersion and the elution solvent. The matrix effect regarding the recovery of the pesticides by MSPD was also investigated. The best results were obtained using 0.5 g of sample, 1.0 g reused C18, interaction time of 1 h, dispersion time of 5 min, and acetonitrile as the elution solvent. The method was validated by the fortification of the onion sample, free of pesticides, at different concentration levels (0.01, 0.1 and 1.0 mg kg⁻¹). Average recoveries ranged from 78.3 to 120.4% and relative standard deviation below 20% was obtained. Detection and quantification limits ranged from 0.003 to 0.03 mg kg⁻¹ and from 0.01 to 0.1 mg kg⁻¹, respectively.     

Simultaneous determination of 186 fungal and bacterial metabolites in indoor matrices by liquid chromatography/tandem mass spectrometry

This paper describes the application of a previously published multi-mycotoxin method for food and feed matrices based on liquid chromatography/electrospray ionization-tandem mass spectrometry (HPLC/ESI-MS/MS) to the analysis of microbial metabolites in indoor matrices. The range of investigated analytes has been extended by 99 fungal and bacterial metabolites to cover now 186 compounds overall. The method is based on a single extraction step using an acidified acetonitrile/water mixture (which has been determined to be preferable to methanol and ethyl acetate) followed by analysis of the diluted crude extract. The analytical signal of one third of the investigated analytes was reduced by more than 50% due to matrix effects in a spiked extract of house dust, whereas the other investigated materials were less critical in that aspect. For determination of method performance characteristics, a spiked reference material for house dust was chosen as a model sample for an extremely complex matrix. With few exceptions, coefficients of variation of the whole procedure of <10% and limits of detection of <50 μg kg⁻¹ were obtained. The apparent recoveries were below 50% for half of the investigated analytes due to incomplete extraction and/or detection-related matrix effects. The application of the method to 14 samples from damp buildings revealed the presence of 20 different analytes at concentrations of up to 130 mg kg⁻¹. Most of these compounds have never been identified before in real-world samples, although they are known to be produced by indoor-relevant fungi. This underlines the great value of the described method for the on-site determination of microbial metabolites.