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

Azzouz, Abdelmonaim; Souhail, Badredine; Ballesteros, Evaristo

doi:10.1016/j.chroma.2010.02.069

Cited by 64 publications

(44 citation statements)

References 31 publications

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“…In general terms, and due to the low concentrations of these chemicals and many other PCPs in environmental matrices, analytes need to be extracted and pre-concentrated before analysis. In this sense, solid phase extraction (SPE) is one of the most commonly used techniques, being also easily automated (Kuster et al, 2008;Cueva-Mestanza et al, 2008;Azzouz et al, 2010) and more environmentally friendly than conventional liquid liquid extraction (LLE) (Bester, 2005). The use of sorptive techniques such as solidphase microextraction (SPME) (Canosa et al, 2005) and stir bar sorptive extraction (SBSE) (Silva and Nogueira, 2008;Pedrouzo et al, 2010) for processing aqueous samples has increased over the last years.…”

Section: Introductionmentioning

confidence: 99%

Determining the distribution of triclosan and methyl triclosan in estuarine settings

2014

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h i g h l i g h t sSimultaneous extraction of TCS and MTCS by SBSE-LD and PLE-in-cell-clean up. Analysis of estuarine sediment and water samples and from photodegradation assays. Distribution of analytes in estuaries depends on wastewater sources and tides. TCS can be both photodegraded or converted to MTCS in estuaries. a r t i c l e i n f o a b s t r a c tWe have developed a method for the analysis of two sewage-derived contaminants: triclosan (TCS), an antibacterial agent, and methyl triclosan (MTCS), a TCS metabolite. For solid samples (4 g), extraction and cleanup were integrated into the same step using pressurized liquid extraction (PLE) with in-cellclean-up (1 g of florisil). The extraction was performed using dichloromethane at 100°C, 1500 psi and 3 static extraction cycles of 5 min each. For water samples (100 mL), stir bar sorptive extraction-liquid desorption (SBSE-LD) was used. Bars were stirred for 10 h and analytes were later desorbed using acetonitrile. Finally, MTCS and a silylated derivative of TCS were determined by gas chromatography-mass spectrometry (GC-MS). Recovery experiments in water and sediments were performed and the results ranged from 67% to 78%. Limits of detection (LODs) were 5 ng L À1 for TCS and 1 ng L À1 for MTCS, in water samples, and 0.1 ng g À1 for TCS and MTCS in solid samples. The method was applied then to determine the levels of these compounds in the estuary of Guadalete River (SW Spain). TCS and MTCS concentrations up to 9.6 ng g À1 in sediments and 310 ng L À1 in water were measured. Their distribution was strongly influenced by the presence of wastewater sources, treated and untreated, along the sampling area, where maximum concentrations were detected. Highest values were reached in the water column during low tides as the water volume in the estuary becomes lower.

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Section: Introductionmentioning

confidence: 99%

Determining the distribution of triclosan and methyl triclosan in estuarine settings

2014

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“…Furthermore, solvent removal and automation is rather easy to achieve. Various sorbents for SPE, such as silica-based C18 and polymeric-based Oasis HLB, have been used mainly for water and foodstuff samples [23,24]. Other techniques such as microwave-assisted extraction and pressurized liquid extraction (PLE) provide poor selectivity when dealing with complex samples.…”

Section: Introductionmentioning

confidence: 99%

Miniaturized extraction methods of triclosan from aqueous and fish roe samples. Bioconcentration studies in zebrafish larvae (Danio rerio)

Gonzalo-Lumbreras

Sanz‐Landaluze

Guinea³

et al. 2012

Anal Bioanal Chem

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Triclosan, an antibacterial and antifungal agent, is widely used in household and personal care products, processed foods and food packaging, etc., and thus also released into the environment. Triclosan is acutely and chronically toxic to aquatic organisms and bioaccumulates in fish tissue. Here, we propose a new miniaturized triclosan extraction method for aqueous and fish roe samples, based on the use of a vortex mixer and an ultrasonic probe, respectively, and useful for triclosan determination by gas chromatography coupled to a micro electron capture detector. Different solvents for extraction and sorbents for clean-up purposes were tested. Multivariate optimization of the variables affecting ultrasonic extraction (ultrasound radiation amplitude, sonication time, sample temperature, and the ratio of sample amount and extracting volume) was carried out. Solvent extraction using ethyl acetate and further clean-up with mixed bed cartridges with two layers of Florisil® and Florisil® impregnated with 10% sulfuric acid only for fish roe samples was finally selected. Extraction efficiencies of up to 95% and 90%, and detection limits of 0.165 ng ml(-1) and 2.7 ng g(-1) for aqueous and fish roe samples were obtained, respectively. The optimized method was used in bioconcentration studies with zebrafish larvae (Danio rerio), as an alternative method to the Organization for Economic Cooperation and Development technical guideline 305. Bioconcentration values, BCF = 2,630 and 2,018 at exposure concentrations of 30 and 3 μg L(-1), respectively, were assessed. These results are in agreement with those reported in the literature, showing the feasibility of the method for estimation of toxicokinetic parameters and bioconcentration factors using zebrafish larvae instead of adult fishes, reducing considerable animal testing, as suggested by the European legislation.

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“…This group includes pharmaceutically active compounds such as analgesics, antiinflammatories, psychiatric drugs, lipid regulators, antibiotics, antiseptics, anticonvulsants…, and personal care products such as fragrances, plasticizers, UV filters, and insect repellents.... Concentrations of these substances in aqueous samples have been measured within a range from less than 10 ng/L (in river water) to more than 100 μg/L (in raw wastewater) [5]. Although less frequently analyzed, PPCPs have been also detected in soil and sediment samples, at concentrations typically between 0.5 and 10 ng/g [6].…”

Section: Introductionmentioning

confidence: 99%

Environmentally friendly analysis of emerging contaminants by pressurized hot water extraction–stir bar sorptive extraction–derivatization and gas chromatography–mass spectrometry

2012

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This work describes the development, optimization, and validation of a new method for the simultaneous determination of a wide range of pharmaceuticals (betablockers, lipid regulators…) and personal care products (fragrances, UV filters, phthalates…) in both aqueous and solid environmental matrices. Target compounds were extracted from sediments using pressurized hot water extraction followed by stir bar sorptive extraction. The first stage was performed at 1,500 psi during three static extraction cycles of 5 min each after optimizing the extraction temperature (50-150°C) and addition of organic modifiers (% methanol) to water, the extraction solvent. Next, aqueous extracts and water samples were processed using polydimethylsiloxane bars. Several parameters were optimized for this technique, including extraction and desorption time, ionic strength, presence of organic modifiers, and pH. Finally, analytes were extracted from the bars by ultrasonic irradiation using a reduced amount of solvent (0.2 mL) prior to derivatization and gas chromatography-mass spectrometry analysis. The optimized protocol uses minimal amounts of organic solvents (<10 mL/sample) and time (≈8 h/sample) compared to previous existing methodologies. Low standard deviation (usually below 10 %) and limits of detection (sub-ppb) vouch for the applicability of the methodology for the analysis of target compounds at trace levels. Once developed, the method was applied to determine concentrations of these compounds in several types of sample (wastewater, seawater, pore water, and sediment) from Cadiz Bay (SW Spain). To our knowledge, these findings represent the first information available on the presence of some of the target compounds in the marine environment.

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

Cited by 64 publications

References 31 publications

Determining the distribution of triclosan and methyl triclosan in estuarine settings

Determining the distribution of triclosan and methyl triclosan in estuarine settings

Miniaturized extraction methods of triclosan from aqueous and fish roe samples. Bioconcentration studies in zebrafish larvae (Danio rerio)

Environmentally friendly analysis of emerging contaminants by pressurized hot water extraction–stir bar sorptive extraction–derivatization and gas chromatography–mass spectrometry

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