Parameters optimization using experimental design for headspace solid phase micro-extraction analysis of short-chain chlorinated paraffins in waters under the European water framework directive

Gandolfi, F; Malleret, Laure; Sergent, Michelle; Doumenq, Pierre

doi:10.1016/j.chroma.2015.06.030

Cited by 27 publications

(23 citation statements)

References 40 publications

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“…A comparison with previous studies (Table ) revealed that the traditional LLE required at least 10 min, and SPE required more than 20 min for each sample (depending on the SPE flow rate, sample volume and SPE manifold setup) , and solvent consumption for LLE exceeded 450 mL . Moreover, comparing with the extraction time for the solvent‐free microextraction methods, SPME required at least 40 or 80 min , and SBSE required 24 h . The LOD or LOQ for this VALLME coupled GC–ECNI‐MS method is lower than those reported for SBSE and SPME methods , and the recoveries of the spiked samples are not significantly different.…”

Section: Resultsmentioning

confidence: 73%

“…Gandolfi et al. found SCCPs samples of surface water at concentration levels ranging from 0.2 to 1.4 μg/L, whereas SCCPs were detected in WWTP effluent with concentrations of 1.0 μg/L in France .…”

Section: Resultsmentioning

confidence: 99%

“…SPE is also time consuming, as the sample loading step requires a long wait time, and SPE cartridge blocking problems further discourage its use. Moreover, SPME and stir bar sorptive extraction (SBSE), two popular solvent‐free techniques, have also been employed to extract SCCPs from aqueous samples . The drawbacks of these techniques are that both are expensive, require the use of fragile coating layers, and that the fibers degrade with multiple usage.…”

Section: Introductionmentioning

confidence: 99%

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Vortex‐assisted liquid–liquid microextraction for the rapid screening of short‐chain chlorinated paraffins in water

Chang

Chung

Wang

2015

J of Separation Science

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The rapid screening of trace levels of short-chain chlorinated paraffins in various aqueous samples was performed by a simple and reliable procedure based on vortex-assisted liquid-liquid microextraction combined with gas chromatography and electron capture negative ionization mass spectrometry. The optimal vortex-assisted liquid-liquid microextraction conditions for 20 mL water sample were as follows: extractant 400 μL of dichloromethane; vortex extraction time of 1 min at 2500 × g; centrifugation of 3 min at 5000 × g; and no ionic strength adjustment. Under the optimum conditions, the limit of quantitation was 0.05 μg/L. Precision, as indicated by relative standard deviations, was less than 9% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was above 91%. The vortex-assisted liquid-liquid microextraction with gas chromatography and electron capture negative ionization mass spectrometry method was successfully applied to quantitatively extract short-chain chlorinated paraffins from samples of river water and the effluent of a wastewater treatment plant, and the concentrations ranged from 0.8 to 1.6 μg/L.

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Section: Resultsmentioning

confidence: 73%

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Vortex‐assisted liquid–liquid microextraction for the rapid screening of short‐chain chlorinated paraffins in water

Chang

Chung

Wang

2015

J of Separation Science

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“…Design of experiments consists of a set of mathematical and statistical techniques that can be used to quantify the relationship between output variables (responses) and the input variables [17] in other to determine the optimum operating variables. In this study, the Doehlert experimental design was performed [6].…”

Section: Experimental Designmentioning

confidence: 99%

Antibacterial properties of AgNO3-activated carbon composite on Escherichia coli: inhibition action

Rachel

Abdelaziz²,

Nsami³

et al. 2018

IJAC

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AgNO3- activated carbon composite based palm kernel shell was prepared by hydrothermal carbonization. The concentration of AgNO3, activation temperature and impregnation time were investigated on five responses (iodine number, methylene blue number, BET surface area, micropore volume and total pore volume). The most influential parameters of the preparation process were optimized using the Doehlert optimal design. From the ANOVA, the following optimal conditions of preparation were retained: 0.068 mol/L, 210°C and 3.7 h for AgNO3 concentration, activation temperature and impregnation time respectively. The activated carbon (AC) and the composite (AC-AgNO3) were characterized using Fourier Transform infrared spectroscopy, X-Ray diffraction, Scanning Electron Microscopy coupled to Energy Dispersive X-ray spectroscopy and measurements of the surface area. The XRD pattern and SEM-EDX clearly confirmed the presence of silver in the composite. The experimental parameters of AC- AgNO3 composite were as followed: 708.44 mg/g; 293.09 mg/g; 713.0 m2/g; 0.49 cm3/g and 0.76 cm3/g, for iodine number, methylene blue number, BET surface area, micropore volume and total pore volume of AC- AgNO3 respectively. The antibacterial test carried on Escherichia Coli showed that AC-AgNO3 composite has a high-improved antibacterial property of 99.99% fixation with a dosage of 1500 ppm for 5 hours of contact time.

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“…The GC coupled to ECD (electronic capture detector) has also been used in CPs determination, but this detector is little selective in organochorine-rich extracts. However, the GC coupled to mass spectrometry with electron capture negative ionization (GC-ECNI-MS) is today the more frequently used approach (Tomy et al 1997;Reth and Oehme 2004;Gandolfi et al 2015). Nowadays, the GC coupled to triple quadrupole mass spectrometry in mode Mass/Mass (GC-QqQ-MS/MS) is beginning to be used for analysis of CCPs in environmental samples using fragments of low m/z Tölgyessy et al 2017).…”

Section: Introductionmentioning

confidence: 99%

Development of a method for the determination of SCCPs (short-chain chlorinated paraffins) in bivalve mollusk using Soxtec device followed by gas chromatography-triple quadrupole tandem mass spectrometry

et al. 2018

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Background: Organochlorinated compounds are major environmental concern due to their persistence, long-range transportability and bio-accumulation. Chlorinated paraffin (CP) mixtures, especially short-chain CPs (SCCPs), are found in environmental samples at very high levels. However, information about their levels is still insufficient, mainly in marine biota. Methods: This study aimed to optimize and validate a method for the determination of SCCPs (short-chain chlorinated paraffins) in bivalve mollusk using a Soxtec extractor and Gas Chromatography coupled with Mass Spectrometry in tandem GC-QqQ-MS/MS (EI). A Plackett-Burman (2^7*3/16) type III resolution factorial design was used to optimize the extraction and purification procedures, sample amount, extractant volume, boiling and rinsing times as extraction variables and alumina, acid silica gel amounts and elution volume as purification variables. Results: The most influent factors were sample amount, rinsing time, extractant volume and acid silica gel amount. Further experiments were performed in order to attain the optimal values of these factors (4 g sample amount, 50 mL n-hexane-dichloromethane as extractant volume, 2 and 1.5 h boiling and rinsing times, 8 g alumina, 4 g acid silica gel (15%) and 50 mL n-hexane-dichloromethane as elution solvent). Validation of the optimized method presented recoveries higher than 90% with RSD below 10%, showing good accuracy and precision. The whole method limits of detection and quantification were 46.13 mg Kg -1 and 153.75 mg Kg

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Parameters optimization using experimental design for headspace solid phase micro-extraction analysis of short-chain chlorinated paraffins in waters under the European water framework directive

Cited by 27 publications

References 40 publications

Vortex‐assisted liquid–liquid microextraction for the rapid screening of short‐chain chlorinated paraffins in water

Vortex‐assisted liquid–liquid microextraction for the rapid screening of short‐chain chlorinated paraffins in water

Antibacterial properties of AgNO3-activated carbon composite on Escherichia coli: inhibition action

Development of a method for the determination of SCCPs (short-chain chlorinated paraffins) in bivalve mollusk using Soxtec device followed by gas chromatography-triple quadrupole tandem mass spectrometry

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