Inter-laboratory validation of solid-phase microextraction for the determination of triazine herbicides and their degradation products at ng/l level in water samples

Ferrari, R C; Nilsson, Torben; Arena, Rocco; Arlati, Patrizia; Bartolucci, Gianluca; Basla, Romilde; Cioni, Fabio; Carlo, Giuseppe Del; Dellavedova, Pierluisa; Fattore, Elena; Fungi, Martino; Grote, C.; Guidotti, Maurizio; Morgillo, Stefania; Müller, Laura; Volante, Marco

doi:10.1016/s0021-9673(97)00837-6

Cited by 61 publications

(26 citation statements)

References 13 publications

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“…If required, small sample volumes of 5 to 20 mL can be handled. The quantification of multiple analytes in water has been successfully applied for some years [10][11][12]. Validated and official standard protocols already exist; however, preliminary studies should always be carried out to assess extraction kinetics and time, as well as desorption temperature, to optimize extraction conditions for new analytes.…”

Section: Spme: Benefits and Drawbacks In Work Routinementioning

confidence: 99%

“…SPME has been applied in many different areas such as environmental analysis where precise quantification must be validated. This technique has been shown to be suitable and valid for a wide range of analytes from volatile to nonvolatile compounds including many HOCs [8][9][10][11] among others. As a consequence, a German DIN standard operational procedure for the analysis of 22 pesticides of different polarities from water samples was established in 2007 [12].…”

Section: Introductionmentioning

confidence: 99%

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Solid-phase microextraction for bioconcentration studies according to OECD TG 305

2012

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An important aim of the European Community Regulation on chemicals and their safe use is the identification of (very) persistent, (very) bioaccumulative, and toxic substances. In other regulatory chemical safety assessments (pharmaceuticals, biocides, pesticides), the identification of such (very) persistent, (very) bioaccumulative, and toxic substances is of increasing importance. Solid-phase microextraction is especially capable of extracting total water concentrations as well as the freely dissolved fraction of analytes in the water phase, which is available for bioconcentration in fish. However, although already well established in environmental analyses to determine and quantify analytes mainly in aqueous matrices, solid-phase microextraction is still a rather unusual method in regulatory ecotoxicological research. Here, the potential benefits and drawbacks of solid-phase microextraction are discussed as an analytical routine approach for aquatic bioconcentration studies according to OECD TG 305, with a special focus on the testing of hydrophobic organic compounds characterized by log K OW > 5.

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Section: Spme: Benefits and Drawbacks In Work Routinementioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Solid-phase microextraction for bioconcentration studies according to OECD TG 305

2012

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“…As already mentioned, an inter-laboratory validation of SPME for the determination of triazines and their metabolites at the ng/L in water samples was recently reported [13]. Optimised conditions for sensitivity were obtained using the CW-DVB fibre and an extraction time of 30 min.…”

Section: Quantitative Analysis and Validationmentioning

confidence: 99%

“…The two fibres containing divinylbenzene were shown to have the highest affinities for the more polar analytes. An interlaboratory study (including ten laboratories) about the analysis of triazine herbicides and their metabolites has been rep o rted [13]. The SPME conditions we re optimised in order to obtain maximum sensitivity.…”

Section: Selection Of the Nature And Thickness Of The Fibrementioning

confidence: 99%

Solid-phase microextraction and gas chromatography for rapid analysis of pesticides

Miège¹,

Dugay²

1998

Analusis

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DossierPesticide analysis M any pesticides can be analysed by gas chromatography but their detection and quantification in water samples at the 0.1 µg/L level require an extraction and enrichment step. This step is often carried out using liquid-liquid extraction (LLE) or solid-phase extraction (SPE). LLE requires large amount of organic solvent and has been largely replaced these recent years by SPE using a variety of different sorbents. Although the on-line coupling of SPE with GC is possible, it is not as easy as that involved with liquid chromatography (LC), for which several fully automated devices have been commercially available for several years. Anyway, SPE followed by GC analysis is commonly an off-line multi-step procedure proned to losses of analytes and still needed some organic solvent for analyte elution.Moreover, only an aliquot of the extract is injected into the gas chromatograph.Solid-phase microextraction (SPME) was introduced several years ago by Pawliszyn and co-workers [1] and represents a further advance as a complete solvent-free alternat ive technique wh i ch is well adapted to the ex t raction of pesticides from water samples. Organic compounds are simply extracted by dipping the solid phase coating of a silica fibre support into an aqueous solution. Extraction and concentration are then focused in a single step. Then the fibre is transferred into the heated injector of a gas chromatograph wh e re the ex t racted analytes are therm a l ly desorbed and a n a ly s e d. Contra ry to SPE, the total amount of ex t ra c t e d sample is used for the determination by GC. SPME requires small sample volumes (1 to 15 mL), and several fibres with different polarities are now available. Moreover, the technique is easy to automate by using a commercially available auto-sampler.A recent review [2] and the increasing number of papers devoted to this technique published these last two years, witnesses its increasing use especially in the env i ro n m e n t a l field [3][4][5][6][7][8][9][10][11]. The first pesticides applications concerned the m o re vo l atile orga n i ch l o ri n ated insecticides and used an e l e c t ro n -c ap t u re detector (ECD) [3]. Th e n , m a ny ap p l i c ations were devoted to nitrogen-and phosphorous-containing pesticides because of the selectivity of the nitrogen-phosp h o rus detector (NPD) [4][5][6]. Some recent publ i c at i o n s reported the use of mass spectrometric (MS) detector and are devoted to more numerous pesticides [7][8][9][10][11]. Solid-phase micro extraction (SPME) combined with gas ch ro m a t o g r a p hy (GC) is a fast and simple technique for the handling of aqueous samples using coated fused-silica fibres. F u l ly automated devices are commerc i a l ly ava i l a bl e. S everal applications have demonstrated the potential of the technique for both screening and quantification of pesticides in water samples with detection limits in the range from 5 to 100 ng/L using mass spectrometry detection.

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“…Various methods including the classical liquidliquid extraction (LLE) [8], solid-phase extraction (SPE) [9][10][11], supercritical fluid extraction (SFE) [12,13], liquid-phase microextraction (LPME) [14,15], solid-phase microextraction (SPME) [16][17][18], and coupled extraction techniques [19,20] were applied for extraction and preconcentration of atrazines from various samples. However, most of these methods were not applicable for simultaneous extracting triazines and their metabolites as the metabolites are usually much more polar than the parent compounds.…”

mentioning

confidence: 99%

Determination of atrazine, desethyl atrazine and desisopropyl atrazine in environmental water samples using hollow fiber-protected liquid-phase microextraction and high performance liquid chromatography

Peng

Lü

et al. 2007

Microchim Acta

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Abstract.A new method based on hollow fiberprotected liquid-phase microextraction (LPME) was developed for the simultaneous determination of atrazine, desethyl atrazine and desisopropyl atrazine in environmental water samples. In LPME, analytes were extracted into 1-octanol immobilized in the micropores of a poly(vinylidene fluoride) porous hollow fiber membrane, and back extracted into the acceptor (4 M HCl) filled in the lumen of the hollow fiber. After LPME, the analytes trapped in the acceptor were analyzed with high-performance liquid chromatography after neutralization. The effect of extraction factors such as sample pH, acceptor pH, salinity, extraction time, stirring rate, and humic acid were studied. Under the optimized conditions, the limits of detection and relative standard deviations were respectively in the range of 0.5-1.0 mg L À1 and 3.9-4.7% (n ¼ 5). The proposed method was applied to determine atrazine, desethyl atrazine and desisopropyl atrazine in wastewater and groundwater samples. The three analytes were below the limits of detection, but good relative spiked recoveries over 90.1 AE 5.9% at 5 mg L À1 spiked level were obtained.

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Inter-laboratory validation of solid-phase microextraction for the determination of triazine herbicides and their degradation products at ng/l level in water samples

Cited by 61 publications

References 13 publications

Solid-phase microextraction for bioconcentration studies according to OECD TG 305

Solid-phase microextraction for bioconcentration studies according to OECD TG 305

Solid-phase microextraction and gas chromatography for rapid analysis of pesticides

Determination of atrazine, desethyl atrazine and desisopropyl atrazine in environmental water samples using hollow fiber-protected liquid-phase microextraction and high performance liquid chromatography

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