Membrane-assisted solvent extraction of triazines and other semi-volatile contaminants directly coupled to large-volume injection–gas chromatography–mass spectrometric detection

Hauser, Barbara; Popp, Peter; Kleine-Benne, Eike

doi:10.1016/s0021-9673(02)00135-8

Cited by 72 publications

(17 citation statements)

References 17 publications

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“…Dispersive solid phase extraction proposed as a multicomponent method for the determination of numerous pesticides in wine achieved LOQ levels of low parts per billion, too [37]. However, this type of sample preparation is difficult to automate, whereas the MASE technique has already been verified as a fully automated method operating at line to the GC-MS as reported previously [26][27][28]. Automation and online coupling of the MASE technique with HPLC-MS/MS is possible, too, but within our investigations, no appropriate autosampler was available.…”

Section: Methods Validationmentioning

confidence: 93%

“…The membrane extraction devices developed by Hauser et al [26] were purchased from Gerstel (Muelheim an der Ruhr, Germany) and consist of a non-porous polyethylene polymer bag mounted to a metal holder which guides the syringe needle into the bag volume filled with an organic acceptor solvent. Five different wine sorts were bought from supermarkets and shops specializing on organic products.…”

Section: Chemicals and Materialsmentioning

confidence: 99%

“…The design of the membrane extraction device has been reported previously together with the respective extraction methods developed [25][26][27][28][29][30]. Briefly, the extraction vial contains 10 mL wine in which the membrane bag filled with 100 μL toluene as organic extraction solvent is immersed.…”

Section: Membrane-assisted Solvent Extraction Proceduresmentioning

confidence: 99%

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Determination of pesticide residues in wine by membrane-assisted solvent extraction and high-performance liquid chromatography–tandem mass spectrometry

et al. 2012

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The determination of pesticides in food products is an essential issue to guarantee food safety and minimise health risks of consumers. A protocol based on membrane-assisted solvent extraction and liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) that allows the determination of 18 pesticides in red wine at minimum labour effort for sample preparation was developed and validated. Ten millilitres of wine were extracted using 100 μL of toluene filled in a non-porous polyethylene membrane bag which is immersed in the wine sample. After 150 min extraction under stirring, an aliquot of the extraction solution is analysed using HPLC-MS/MS. The limits of quantification ranged from 3 ng/L for Pirimicarb to 1.33 μg/L for Imidacloprid. Quantification by matrix-matched calibration provided relative standard deviations ≤16 % for most of the target pesticides. The linearity of calibration was given over three to four orders of magnitude, which enables the reliable measurement of a broad range of pesticide concentrations, and for each target pesticide, the sensitivity of the protocol meets the maximum residue levels set by legislations at least for wine grapes. Good agreement of results was found when the new method was compared with a standard liquid-liquid extraction protocol. In five wine samples analysed, Carbendazim and Metalaxyl were determined at micrograms per litre concentrations, even in some of the organic wines. Tebuconazol and Cyprodinitril were determined at lower abundance and concentration, followed by Spiroxamin and Diuron.

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Section: Methods Validationmentioning

confidence: 93%

Section: Chemicals and Materialsmentioning

confidence: 99%

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Determination of pesticide residues in wine by membrane-assisted solvent extraction and high-performance liquid chromatography–tandem mass spectrometry

et al. 2012

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“…Lehotay and coworkers [12][13][14] introduced solvent in silicone tube extraction as an approach to be combined with the QuEChERS (quick, easy, cheap, effective, rugged and safe) method to reduce the detection limit of 26 pesticides analysed at the ppb level, using acetonitrile as inner solvent in PDMS tubing, in combination with GC-MS. Sandra and coworkers [15][16][17] introduced silicon membrane sorptive extraction (SMSE), and used ethyl acetate as solvent to concentrate and then quantify atrazine and its three metabolites in water samples in the 1-10 ppt range by GC-SIM-MS and LC-MS. Van Hoeck also investigated the influence of ethyl acetate as inner PDMS solvent on recovery of EDCs (endocrine disrupters) and pharmaceuticals of different polarity (K O/W between 0 and 4) from a salted-out standard solution at the ppt level and found that SMSE was more effective than SBSE only for very polar compounds (K O/W o2) [18]. Hauser et al [19,20] and Schellin et al [21][22][23] applied the same approach (membrane-assisted solvent extraction) in a fully automatic analysis system using a tubing of dense polypropylene as ''sorptive'' membrane medium, filled with 500-800 mL of hexane or cyclohexane as acceptor solvent, and triazines, 2,4-dichloroanilines, a-HCH and phenanthrene as model compounds; the resulting solution was then online analysed by large-volume injection GC-MS [19]. They also applied this technique to determine polychlorinated biphenyls [20], organophosphorus pesticides as such [21] or together with triazines and organochlorine compounds [22] in several real-world water samples and other matrices.…”

Section: Introductionmentioning

confidence: 99%

Solvent‐enhanced headspace sorptive extraction in the analysis of the volatile fraction of matrices of vegetable origin

Sgorbini

Budziak

Cordero

et al. 2010

J of Separation Science

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The solvent-enhanced headspace sorptive extraction technique aims at modifying PDMS polarity using a solvent to increase its concentration capability. In solvent-enhanced headspace sorptive extraction, a PDMS tubing closed at both ends by small glass stoppers and filled with an organic solvent is suspended in the sample headspace for a fixed time. After sampling, the sampled analytes are recovered from the PDMS tubing by thermal desorption and online transferred to a GC-flame ionization detector or GC-MS system for analysis. Cyclohexane, iso-octane, ethyl acetate, acetone, acetonitrile and methanol were tested as PDMS modifiers to sample the volatile fractions of sage (Salvia lavandulifolia Vahl.), thyme (Thymus vulgaris L.) and roasted coffee. Ethyl acetate was found to be the most effective PDMS modifier for all matrices investigated; although to a lesser extent, cyclohexane also increased component recoveries with sage and thyme. Acetone, acetonitrile and methanol did not increase PDMS recovery, while isooctane was excluded because of its interaction with the polymer. The results show that solvent-modified PDMS extends the range of sampled headspace components with different polarities, increases the recovery of many of them, improves sensitivity in trace analysis, speeds up recovery and gives repeatability comparable with that of unmodified PDMS.

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“…Methods for triazine determination in water include separation by HPLC [4][5][6] and GC 7,8 after solid-phase extraction (SPE), [9][10][11] capillary electrophoresis, 12 micellar electrokinetic capillary chromatography, 13 triazine multianalyte immunoassays, 14,15 CL/ ECL immunoassays, 16,17 ELISA, 18,19 ECL, 20 fluorometric methods with dansyl chloride 21 and photochemically-induced fluorometric method with o-phthalaldehyde-2-mercaptoethanol derivitazation. 22 These methods are sensitive and accurate; however, many of these involve expensive methods, and toxic solvents, are slow and require the development of extremely complex gradients for the separation.…”

Section: Introductionmentioning

confidence: 99%

Photodegradation and Flow-Injection Determination of Simetryn Herbicide by Luminol Chemiluminescence Detection

2008

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A novel and simple flow injection chemiluminescence method is reported for the determination of simetryn, a common herbicide. The method is based on the direct oxidation of luminol by the photoproducts of the simetryn in alkaline medium in the absence of catalyst/oxidant. The linear concentration range was 0.01 -2 mg mL -1 simetryn with a correlation coefficient (r 2 ) of 0.9997 and relative standard deviations (RSD; n = 4) in the range of 0.9 -2.3%. The limit of detection (S/N = 3) was 7.5 ng mL -1 with a sample throughput of 100 h -1 . The proposed method has been applied to determine simetryn in natural waters using Sep-Pak C18 cartridges for solid phase extraction (SPE) procedure. The recoveries were in the range of 97 ± 1 to 104 ± 2%. The mechanism of chemiluminescence reaction has also been discussed briefly.

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Membrane-assisted solvent extraction of triazines and other semi-volatile contaminants directly coupled to large-volume injection–gas chromatography–mass spectrometric detection

Cited by 72 publications

References 17 publications

Determination of pesticide residues in wine by membrane-assisted solvent extraction and high-performance liquid chromatography–tandem mass spectrometry

Determination of pesticide residues in wine by membrane-assisted solvent extraction and high-performance liquid chromatography–tandem mass spectrometry

Solvent‐enhanced headspace sorptive extraction in the analysis of the volatile fraction of matrices of vegetable origin

Photodegradation and Flow-Injection Determination of Simetryn Herbicide by Luminol Chemiluminescence Detection

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