Determination of multiclass pesticides in river sediments via matrix solid-phase dispersion extraction and gas chromatography–tandem mass spectrometry

A fast and environment-friendly analytical method was implemented to determine multiclass pesticides in river sediments. Twenty-three pesticides—organochlorine pesticides, organophosphorus pesticides, and triazines—were extracted via matrix solid-phase dispersion (MSPD) and analyzed by gas chromatography–tandem mass spectrometry (GC–MS/MS). Florisil demonstrated excellent analytes uptake capability as the extractant phase, with suitable selectivity for treating complex sediment samples. Under defined extraction conditions, the MSPD–GC–MS/MS method demonstrated robustness in the n inter-day analysis of sediments from different sources, providing limit of quantifications (LOQs) between 5 and 15 ng/g, linear responses in the range between LOQs and 150 ng/g, extraction recoveries of 71%–106%, and precision, assessed as relative standard deviation below 20%. The MSPD significantly reduced samples and solvents’ consumption, providing critical environmental gains compared to traditional extraction methods like Soxhlet. Finally, the method was applied to analyze sediment samples from three different collection areas of the Subachoque River (Cundinamarca, Colombia), demonstrating a fast, efficient, confident, and profitable analytical tool for pollution control and monitoring in environmental samples. The method allowed us to determine the current use in Colombia of banned pesticides under the 2001 Stockholm Convention.     

Determination of selected UV filters in indoor dust by matrix solid-phase dispersion and gas chromatography–tandem mass spectrometry

A simple, inexpensive sample preparation procedure, based on the matrix solid-phase dispersion (MSPD) technique, for the determination of six UV filters: 2-ethylhexyl salicylate (EHS), 3,3,5-trimethylcyclohexyl salicylate (Homosalate, HMS), 3-(4-methylbenzylidene) camphor (4-MBC), isoamyl-p-methoxycinnamate (IAMC), 2-ethylhexyl-p-methoxycinnamate (EHMC) and octocrylene (OCR), in dust from indoor environments is presented and the influence of several operational parameters on the extraction performance discussed. Under the final working conditions, sieved samples (0.5 g) were mixed with the same amount of anhydrous sodium sulphate and dispersed with 2 g of octadecyl bonded silica (C18) in a mortar with a pestle. This blend was transferred to a polypropylene solid-phase extraction cartridge containing 2 g of activated silica, as the clean-up co-sorbent. The cartridge was first rinsed with 5 mL of n-hexane and the analytes were then recovered with 4 mL of acetonitrile. This extract was adjusted to 1 mL, filtered and the compounds were determined by gas chromatography combined with tandem mass spectrometry (GC–MS/MS). Recoveries for samples spiked at two different concentrations ranged between 77% and 99%, and the limits of quantification (LOQs) of the method between 10 and 40 ng g⁻¹. Analysis of settled dust from different indoor areas, including private flats, public buildings and vehicle cabins, showed that EHMC and OCR were ubiquitous in this matrix, with maximum concentrations of 15 and 41 μg g⁻¹, respectively. Both UV filters were also quantified in dust reference material SRM 2585 for first time. EHS, 4-MBC and IAMC were detected in some of the analyzed samples, although at lower concentrations than EHMC and OCR.     

Determination of perfluorinated compounds in mollusks by matrix solid-phase dispersion and liquid chromatography–tandem mass spectrometry

Perfluorinated compounds (PFCs) have been used for over 40 years in different commercial and industrial applications mainly as surfactants and surface protectors and have become an important class of marine emerging pollutants. This study presents the development and validation of a new analytical method to determine the simultaneous presence of eight PFCs in different kinds of mollusks using matrix solid-phase dispersion (MSPD) followed by liquid chromatography–tandem mass spectrometry (LC-MS/MS). Simplicity of the analytical procedure, low volume of solvent and quantity of sample required, low global price, and integration of extraction and clean-up into a single step, are the most important advantages of the developed methodology. Solvent, solid support (dispersing agent), clean-up sorbent, and their amounts were optimized by means of an experimental design. In the final method, 0.5 g of sample are dispersed with 0.2 g of diatomaceous earth and transferred into a polypropylene syringe containing 4 g of silica as clean-up sorbent. Then, analytes are eluted with 20 mL of acetonitrile. The extract is finally concentrated to a final volume of 0.5 mL in methanol, avoiding extract dryness in order to prevent evaporation losses and injected in the LC-MS/MS. The combination of this MSPD protocol with LC-MS/MS afforded detection limits from 0.05 to 0.3 ng g⁻¹. Also, a good linearity was established for the eight PFCs in the range from limit of quantification (LOQ) to 500 ng mL⁻¹ with R ² > 0.9917. The recovery of the method was studied with three types of spiked mollusk and was in the 64–126% range. Moreover, a mussel sample was spiked and aged for more than 1 month and analyzed by the developed method and a reference method, ion-pair extraction, for comparison, producing both methods statistically equal concentration values. The method was finally applied to the determination of PFCs in different kinds of mollusks revealing concentrations up to 8.3 ng g⁻¹ for perfluoroundecanoic acid.     

Determination of fecal sterols by gas chromatography–mass spectrometry with solid-phase extraction and injection-port derivatization

Injection-port derivatization combined with solid-phase extraction (SPE) was developed and applied for the first time to determine five types of fecal sterols (coprostanol, cholestanol, epicholestanol, epicoprostanol and cholesterol) with gas chromatography–mass spectrometry (GC–MS). In this method, silylation of fecal sterols was performed with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) at GC injection-port. The factors influential to this technique such as injection-port temperature, purge-off time, derivatization reagent (BSTFA) volume, and the type of organic solvent were investigated. In addition, the conditions of SPE (including the type of SPE cartridge, the type of elution organic solvent) were also studied. After SPE followed by injection-port silylation by GC–MS, good linearity of analytes was achieved in the range of 0.02–10 ng/mL with coefficients of determination, R² > 0.995. Good reproducibility was obtained with relative standard deviation less than 19.6%. The limits of detection ranged from 1.3 ng/mL to 15 ng/mL (S/N = 3) in environmental water samples. Compared with traditional off-line silylation of fecal sterols performed with water bath (60 °C, 30 min), this injection-port silylation method is much simpler and convenient. The developed method has been successfully applied for the analysis of fecal sterols from real environmental water samples.     

Determination of microcystins in natural blooms and cyanobacterial strain cultures by matrix solid-phase dispersion and liquid chromatography–mass spectrometry

An analytical procedure based on matrix solid-phase dispersion (MSPD) and liquid chromatography–mass spectrometry (LC-MS) was developed for determining three microcystins (MCs) in natural water blooms and cyanobacteria strain cultures. The procedure involves sample homogenization with C₁₈, washed with dichloromethane to eliminate interfering compounds, and elution with acidic methanol. Results were compared to those achieved by using an organic solvent standard method. Mean recoveries of MCs with MSPD were 85–92% with intra-day relative standard deviation (RSDs) of 9–19%, whereas organic solvent extraction resulted in recovery rates of 92–105% with intra-day RSDs ranging from 8 to 18%. Limits of quantification (LOQs) were 1 g g^–1 dry weight for the MCs either by MSPD or organic solvent extraction. The two analytical methods tested were specific and sensitive to the extraction of MCs and were applied to the detection of MCs in water blooms and culture strains. The concentration of MCs varied from 7 to 3,330 g g^–1 of lyophilized cells with MC-LR always showing the highest concentration. MCs levels were higher in culture strains than in water blooms, except for MC-LR, whose concentration in blooms was slightly superior to that determined in culture strains.     

Trace analysis of benzophenone-derived compounds in surface waters and sediments using solid-phase extraction and microwave-assisted extraction followed by gas chromatography–mass spectrometry

This study describes a procedure for determining eight benzophenone-derived compounds in surface waters and sediments. These include the pharmaceutical ketoprofen, its phototransformation products 3-ethylbenzophenone and 3-acetylbenzophenone, and five benzophenone-type ultraviolet (UV) filters. The proposed analytical method involves the pre-concentration of water samples by solid-phase extraction (SPE) and microwave-assisted extraction (MAE) of sediment samples followed by derivatization and analysis by gas chromatography–mass spectrometry. Different parameters were investigated to achieve optimal method performance. Recoveries of 91 to 96 % from water samples were obtained using HLB Oasis SPE cartridges, whereas MAE of sediments (30 min at 150 °C) gave recoveries of 80 to 99 %. Limits of detection were between 0.1 and 1.9 ng L^?1 for water samples and from 0.1 to 1.4 ng g^?1 for sediment samples. The developed method was applied to environmental samples and revealed the presence of UV filters in the majority of the surface waters with up to 690 ng L^?1 of 2-hydroxy-4-methoxybenzophenone. By contrast, ketoprofen (≤2,900 ng L^?1) and its degradation products (≤320 ng L^?1) were found in only two rivers, both receiving wastewater treatment plant effluents. Sediment analysis revealed benzophenone to be present in concentrations up to 650 ng g^?1, whereas concentrations of other compounds were considerably lower (≤32 ng L^?1). For the first time, quantifiable amounts of two ketoprofen transformation products in the aqueous environment are reported.     

Determination of tetrabromobisphenol-A,tetrachlorobisphenol-A and bisphenol-A in soil by ultrasonic assisted extraction and gas chromatography–mass spectrometry

In this work, an isotope dilution method for the determination, in agricultural and industrial soil samples, of tetrabromobisphenol-A, tetrachlorobisphenol-A and bisphenol-A by gas chromatography–mass spectrometry was developed. The compounds were extracted from soil by sonication assisted extraction in small columns (SAESC) with a low volume of ethyl acetate as extraction solvent. For dirty soil samples, such as industrial soils, a simultaneous clean-up on an acidified Florisil–anhydrous sodium sulfate mixture was carried out to remove interferences. After extraction, solvent was evaporated and analytes were derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and determined by isotope dilution gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode (GC–MS–SIM), using ¹³C₁₂ labeled compounds as internal standards. Recoveries from spiked samples were between 88% and 108% and the estimated limits of detection (S/N = 3) varied from 30 pg g⁻¹ to 90 pg g⁻¹. The response obtained with this method was linear over the range assayed, 5–300 ng ml⁻¹, with correlation coefficients equal or higher than 0.999. The validated method was used to investigate the levels of these phenolic compounds in soil samples collected from different locations in Spain. Bisphenol-A was detected in all samples at concentrations from 0.7 ng g⁻¹ to 4.6 ng g⁻¹ in agricultural soils and from 1.1 ng g⁻¹ to 44.5 ng g⁻¹ in industrial soils. Tetrabromobisphenol-A was found in various soil samples at levels in the range of 3.4–32.2 ng g⁻¹ in industrial soils and at 0.3 ng g⁻¹ in one agricultural soil, whereas tetrachlorobisphenol-A was not detected.     

Determination of five nitrobenzoic acids in groundwater by solid-phase extraction and liquid chromatography–mass spectrometry

A method involving solid-phase extraction (SPE) and reversed-phase liquid chromatography–mass spectrometry (LC–MS) has been developed for determination, in groundwater, of nitrobenzoic acids associated with 2,4,6-trinitrotoluene production. Pre-concentration on a co-polymer-based SPE cartridge enabled quantitative extraction of the analytes from water. Investigation of negative ion electrospray and atmospheric-pressure chemical ionization mass spectrometry indicated the sensitivity of APCI was more than twice that of ESI. An ¹⁵N-labeled internal standard was used to achieve more accurate quantitation and mass assignment. Recovery was better than 80% when 10 mL water was extracted with the SPE cartridge. Combination of SPE with LC–MS analysis resulted in method detection limits of less than 5 μg L⁻¹. The method has been used for analysis of groundwater samples collected from a site of a former ammunition plant. Contamination with nitrobenzoic acids was determined at μg L⁻¹ levels.     

Determination of drugs of abuse in water by solid-phase extraction,derivatisation and gas chromatography–ion trap-tandem mass spectrometry

An alternative method for the sensitive determination of several drugs of abuse and some of their metabolites in surface and sewage water samples is proposed. Analytes are concentrated using a solid-phase extraction (SPE) sorbent, converted into the corresponding trimethylsilyl derivatives and selectively determined by gas chromatography (GC) with tandem mass spectrometry (MS/MS) detection. Parameters affecting the performance of extraction, derivatisation and determination steps are systematically investigated. Moreover, the stability of target analytes in sewage water samples is discussed. Under final working conditions, water samples were adjusted at pH 8.5 and concentrated using a 200 mg OASIS HLB SPE cartridge. Analytes were sequentially eluted with ethyl acetate followed by acetone and silylated using N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA). The reaction was completed in 60 min at 80 °C and the mixture injected directly in the GC–MS/MS system without further purification. In most cases, analytes presented a poor stability in sewage water samples; however, once they are submitted to the SPE process, cartridges can be stored at −20 °C for at least 3 months without significant degradation and/or inter-conversion reactions of illicit drugs. The proposed method provided recoveries over 74% and LODs between 0.8 and 15 ng/L for river and treated wastewater samples. In the case of raw wastewater slightly worse recoveries, between 63 and 137%, and similar LODs were attained. Analysis of a limited number of waste and surface water samples confirmed the presence of several illicit drugs in the aquatic environment, with the highest levels and frequency corresponding to benzoylecgonine, the main metabolite of cocaine.     

Determination of acidic pharmaceutical products and carbamazepine in roughly primary-treated wastewater by solid-phase extraction and gas chromatography–tandem mass spectrometry

A gas chromatography–tandem mass spectrometry (GC–MS/MS) method has been developed for the determination of selected pharmaceutical residues (carbamazepine, salicylic acid, clofibric acid, ibuprofen, 2-hydroxy-ibuprofen, fenoprofen, naproxen, ketoprofen, diclofenac, and triclosan) in sewage influent and roughly primary-treated effluent. The method involved solid-phase extraction (SPE) with polymeric sorbents, and two SPE cartridges were compared for the extraction and elution of the targeted compounds in complex matrices. A successful chemical derivatization of carbamazepine and acidic compounds using N,O-bis(trimethylsilyl) trifluoroacetamide +10% trimethylchlorosilane is also described. The quantification limits of the analytical procedure ranged from 30 to 60?ng?L^?1 for 500?mL of wastewater. The best recovery rates (72–102%) in spiked effluent samples were obtained with Phenomenex Strata-X? cartridges. Detection limits (S/N?=?3) were estimated at between 1 and 18?ng?L^?1. The reported GC–MS/MS method significantly reduces the strong matrix effects encountered with more expensive LC-MS/MS techniques. Application of the developed method showed that most selected analytes were detected at concentrations ranging from low µg?L^?1 to trace level ng?L^?1 in Montreal's wastewater treatment plant effluent and influent, as well as in the receiving waters at more than 8?km downstream of the effluent outfall. The rugged alternative analytical method is suitable for the simultaneous analysis of carbamazepine and pharmaceutical acidic residues in wastewater samples from influents and effluents that have undergone rough primary treatment.     

Determination of endocrine-disrupting chemicals in the liquid and solid phases of activated sludge by solid phase extraction and gas chromatography–mass spectrometry

The highly complex matrix of activated sludge in sewage treatment plants (STPs) makes it difficult to detect endocrine-disrupting chemicals (EDCs) which are usually present at low concentration levels. To date, no literature has reported the concentrations of steroid estrogens in activated sludge in China and very limited data are available worldwide. In this work, a highly selective and sensitive analytical method was developed for simultaneous determination of two classes of EDCs, including estrone (E1), 17β-estradiol (E2), estriol (E3), 17α-ethynylestradiol (EE2), 4-nonylphenol (NP) and bisphenol A (BPA), in the liquid and solid phases of activated sludge. The procedures for sample preparation, extracts derivatization, and gas chromatography–mass spectrometry (GC–MS) quantification were all optimized to effectively determine target EDCs while minimizing matrix interference. The developed method showed good calibration linearity, recovery, precision, and a low limit of quantification (LOQ) for all selected EDCs in both liquid and solid phases of activated sludge. It was successfully applied to determine the concentrations of EDCs in activated sludge samples from two STPs located in Beijing and Shanghai of China, respectively.     

Determination of organophosphate flame retardants in sediments by microwave-assisted extraction and gas chromatography–mass spectrometry with electron impact and chemical ionization

An efficient microwave-assisted extraction (MAE) procedure coupled to gas chromatography–mass spectrometry (GC–MS) with electron impact (EI) and chemical ionization (CI) has been developed to determine five organophosphate flame retardants (OPFRs) in marine and river sediments. The effects of various operating parameters on the quantitative extraction of the OPFRs through MAE were systematically investigated. Selected OPFRs were extracted from the sediments through MAE using 40 mL of acetone at 120 °C for 20 min. The limits of quantitation ranged from 0.1 to 0.4 ng/g (dry weight) in 2 g of the sediment samples. Moreover, as the chlorinated alkyl phosphates present no molecular ions in EI, GC–MS with furan-CI (furan-CI) was applied to confirm their determination in complex environmental samples. The recoveries of the selected OPFRs in spiked sediment samples ranged from 62% to 106% (relative standard derivation, 1−11%). The total concentrations of the selected OPFR residues in marine and river sediments ranged from 1.0 to 12.6 ng/g.     

Determination of ethylphenols in wine by in situ derivatisation and headspace solid-phase microextraction–gas chromatography–mass spectrometry

Contamination by Brettanomyces is a frequent problem in many wineries that has a dramatic effect on wine aroma and hence its quality. The yeast Brettanomyces/Dekkera is involved in the formation of three important volatile ethylphenols—4-ethylphenol, 4-ethylguaiacol and 4-ethylcatechol—that transmit an unpleasant aroma to wine that has often been described as ‘medicinal’, ‘stable’ or ‘leather’. This study proposes an in situ derivatisation and headspace solid-phase microextraction– gas chromatography coupled to mass spectrometry method to determine the three ethylphenols in red Brettanomyces-tainted wines. The most important variables involved in the derivatisation (acetic anhydride and base concentration) and the extraction (extraction temperature and salt addition) processes were optimised by experimental design. The optimal conditions using 4 mL of wine in 20-mL sealed vials were 35 μL of acetic anhydride per millilitre of wine, 1 mL of 5.5% potassium carbonate solution and 0.9 g of sodium chloride and the extraction was performed with a divinylbenzene–carboxen–poly(dimethylsiloxane) fibre at 70 °C for 70 min. Then, the performance characteristics were established using wine samples spiked with the ethylphenols. For all compounds, the detection limits were below the odour threshold reported in the literature and they were between 2 and 17 μg L⁻¹ for 4-ethylguaiacol and 4-ethylphenol, respectively. Intermediate precision (as relative standard deviation) was acceptable, with values ranging from 0.3 to 12.1%. Finally, the method was applied in the analysis of aged Brettanomyces-tainted wines.     

Identification of dissolved organic species in non-drinking tap water by solid-phase extraction and gas chromatography–mass spectrometry

A method is presented for qualitative identification of dissolved volatile organic compounds (VOCs) in non-drinking tap water samples based on applications of both solid-phase extraction (SPE) and gas chromatography–mass spectrometric (GC–MS) techniques. Water samples were collected and passed over a micro-column packed with acid treated active silica gel phase (pH = 2.6) for adsorption of dissolved organic species under this pH-condition. Silica-bound-organics were then divided into equal portions followed by suspension into organic solvents of different polarities such as methanol, ethanol, butan-1-ol, ethyl acetate, diethyl ether and chloroform. These suspensions were then automatically shaken for 1 h at room temperature. The organic extracts were subjected to GC–MS analysis under temperature programming conditions. The mass spectrum of each eluted chromatographic peak was library searched or manually interpreted to identify the correct name and structure. Blank solvent and silica samples were also subjected to the same GC–MS analysis for comparison.     

Determination of cannabinoids in hemp food products by use of headspace solid-phase microextraction and gas chromatography–mass spectrometry

A fully automated procedure using alkaline hydrolysis and headspace solid-phase microextraction (HS-SPME), followed by on-fiber derivatization and gas chromatographic–mass spectrometric (GC–MS) detection has been developed for determination of cannabinoids in hemp food samples. After addition of a deuterated internal standard, the sample was hydrolyzed with sodium hydroxide and submitted to direct HS-SPME. After absorption of analytes for on-fiber derivatization, the fiber was placed directly into the headspace of a second vial containing N-methyl-N-trimethylsilyltrifluoroacetamide (MSTFA), before GC–MS analysis. Linearity was good for ⁹-tetrahydrocannabinol (THC), cannabidiol, and cannabinol; regression coefficients were greater than 0.99. Depending on the characteristics of the matrix the detection limits obtained ranged between 0.01 and 0.17 mg kg^–1 and the precision between 0.4 and 11.8%. In comparison with conventional liquid–liquid extraction this automated HS-SPME–GC–MS procedure is substantially faster. It is easy to perform, solvent-free, and sample quantities are minimal, yet it maintains the same sensitivity and reproducibility. The applicability was demonstrated by analysis of 30 hemp food samples. Cannabinoids were detected in all of the samples and it was possible to differentiate between drug-type and fiber-type Cannabis sativa L. In comparison with other studies relatively low THC concentrations between 0.01 and 15.53 mg kg^–1 were determined.     

Continuous solid-phase extraction and gas chromatography–mass spectrometry determination of pharmaceuticals and hormones in water samples

A semi-automatic flow-based method for the simultaneous determination of 9 pharmaceuticals and 3 hormones in water samples in a single analytical run is proposed. The analytes were retained on a solid-phase extraction sorbent column and 1 μL of the eluate analysed by gas chromatography in combination with electron impact ionization mass spectrometry in the SIM mode. The sorbent used, Oasis-HLB, provided near-quantitative recovery of all analytes. The proposed method was validated with quite good analytical results including low limits of detection (0.01–0.06 ng L⁻¹ for 100 mL of water) and good linearity (r² > 0.993) throughout the studied concentration ranges. The method provided good accuracy (recoveries of 85–103%) and precision (between- and within-day RSD values less than 7%) in the determination of the pharmaceuticals and hormones in tap, river, pond, well, swimming pool and wastewater.     

Determination of synthetic phenolic antioxidants and their metabolites in water samples by downscaled solid-phase extraction,silylation and gas chromatography–mass spectrometry

The development and performance evaluation of an analytical method dedicated to the comprehensive determination of the most relevant antioxidants and their metabolites in aqueous environmental samples is presented. This was achieved by a miniaturised solid-phase extraction (SPE) with 10 mg Oasis HLB cartridges, which allow to achieve a concentration factor of 200, reducing organic solvent wastes (1 mL of ethyl acetate suffices for complete elution) and SPE costs and eliminating the need for solvent evaporation that otherwise compromises the recoveries of butylated hydroxytoluene (BHT) and 2,6-di-tert-butylcyclohexa-2,5-diene-1,4-dione (BHT-Q). Analytes were then determined by gas chromatography–mass spectrometry (GC–MS) after derivatisation with N-methyl-N-(tert-butyldimethylsilyl)-trifluoroacetamide (MTBSTFA) in a single run. BHT-d₇ and n-propyl-paraben-d₄ (PrP-d₄) were used as surrogate internal standards. These surrogates allowed obtaining relative recoveries in the 80–110% range for all analytes even with complex wastewater samples and LODs at the 2–44 ng L⁻¹ level taking into account blank issues often associated to antioxidants analysis. The method was applied to sewage and river waters, showing that the seven analytes could be detected in raw wastewater. BHT and BHT-Q were the most concentrated species in that type of sample (in the 275–871 ng L⁻¹ range). On the other hand two metabolites of BHT, 3,5-di-tert-butyl-4-hydroxybenzaldehyde (BHT-CHO) and 3,5-di-tert-butyl-4-hydroxybenzoic acid (BHT-COOH) appeared to be the most ubiquitous species, being found in all samples in the 10–150 ng L⁻¹ concentration range.     

Determination of gamma-hydroxybutyric acid in serum and urine by headspace solid-phase dynamic extraction combined with gas chromatography–positive chemical ionization mass spectrometry

Gamma-hydroxybutyric acid is an emerging drug of abuse. Beside relaxation and euphoria it causes hypnosis and unconsciousness. Therefore the substance is misused as recreational drug and at drug-facilitated sexual assaults. An automated and effortless method for quantitation of gamma-hydroxybutyric acid in serum and urine was optimized and validated. Five hundred microliters sample volume are used for both matrices. The acid catalyzed conversion of gamma-hydroxybutyric acid to the corresponding gamma-butyrolactone is applied. Furthermore the method is based on headspace solid-phase dynamic extraction coupled with gas chromatography–mass spectrometry. The extraction process is performed by repeated aspiration and ejection of the headspace through a steel cannula which is coated on the inside with a polydimethylsiloxane sorbent. Thus absorption of analyte molecules by the sorbent is achieved. The influence of parameters as sorbent type, incubation temperature, number of extraction strokes, injection port temperature and injection flow speed on extraction recovery was investigated. The validation revealed good accuracy with a bias less than ±5%. Intra- and interday precision determined at 10, 50 and 150 μg/ml for each matrix were in following ranges: 1.96–3.49% (intraday, serum), 2.38–4.31% (intraday, urine), 2.33–5.13% (interday, serum) and 2.53–5.64% (interday, urine). The method provided good linearity between 2 and 200 μg/ml yielding coefficients of determination R² ≥ 0.9985. Limit of detection were determined at 0.16 μg/ml for serum and 0.17 μg/ml for urine, respectively. This method exhibits a fast, solvent-free and widely automated extraction process. It has been applied to toxicological routine analysis and therapeutic drug monitoring successfully.