scholarly journals Carbon and Tin-Based Polyacrylonitrile Hybrid Architecture Solid Phase Microextraction Fiber for the Detection and Quantification of Antibiotic Compounds in Aqueous Environmental Systems

Molecules ◽  
2019 ◽  
Vol 24 (9) ◽  
pp. 1670 ◽  
Author(s):  
Sandip Mondal ◽  
Jialing Jiang ◽  
Yin Li ◽  
Gangfeng Ouyang
Keyword(s):  
Solid Phase Microextraction ◽  
Tin Dioxide ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Tap Water ◽  
Coefficient Of Determination ◽  
Lower Amount ◽  
Custom Made ◽  
Relative Standard ◽  
Detection And Quantification

In this study, the detection and quantification of multiple classes of antibiotics in water matrices are proposed using a lab-made solid phase microextraction (SPME) fiber coupled with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). The lab-made fiber was prepared using a graphene oxide (G), carbon nanotubes (C), and tin dioxide (T) composite, namely GCT, with polyacrylonitrile (PAN) as supporting material. The detected antibiotics were enrofloxacin, sulfathiazole, erythromycin, and trimethoprim. The custom-made fiber was found to be superior compared with a commercial C18 fiber. The excellent reproducibility and lower intra-fiber relative standard deviations (RSDs 1.8% to 6.8%) and inter-fiber RSDs (4.5% to 8.8%) made it an ideal candidate for the detection of traces of antibiotics in real environmental samples. The proposed validated method provides a satisfactory limit of detection and good linear ranges with higher (>0.99) coefficient of determination in the aqueous system. Application of the method was made in different real water systems such as river, pond and tap water using the standard spiking method. Excellent sensitivity, reproducibility, lower amount of sample detection and higher recovery was found in a real water sample. Therefore, the extraction method was successfully applied to the detection and quantification of multiple classes of antibiotics in different aqueous systems with satisfactory results.

scholarly journals Determination of multi-class herbicides in soil by liquid-solid extraction coupled with headspace solid phase microextraction method

2016 ◽  
Vol 81 (8) ◽  
pp. 923-934 ◽  
Author(s):  
Rada Djurovic-Pejcev ◽  
Tijana Djordjevic ◽  
Vojislava Bursic
Keyword(s):  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Soil Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Optimum Number ◽  
Polydimethyl Siloxane ◽  
Headspace Solid Phase Microextraction ◽  
Relative Standard ◽  
Detection And Quantification

A method is described for simultaneous determination of five herbicides (metribuzin, acetochlor, clomazone, oxyfluorfen and dimethenamid) belonging to different pesticides groups in soil samples. Developed headspace solid phase microextraction method (HS-SPME) in combination with liquid-solid sample preparation (LS) was optimized and applied in the analysis of some agricultural samples. Optimization of microextraction conditions, such as temperature, extraction time and sodium chloride (NaCl) content was perfor-med using 100 ?m polydimethyl-siloxane (PDMS) fiber. The extraction effi-ciencies of methanol, methanol:acetone=1:1 and methanol:acetone:hexane= =2:2:1 and the optimum number of extraction steps during the sample prepa-ration, were tested, as well. Gas chromatography-mass spectrometry (GC-MS) was used for detection and quantification, obtaining relative standard deviation (RSD) below 13%, and recovery values higher than 83% for multiple analyses of soil samples fortified at 30 ?g kg-1 of each herbicide. Limits of detection (LOD) were less than 1.2 ?g kg-1 for all the studied herbicides.

scholarly journals Determination of Se4+ in Drinkable Water by Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry

2000 ◽  
Vol 83 (5) ◽  
pp. 1082-1086 ◽  
Author(s):  
Maurizio Guidotti
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Tap Water ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard ◽  
Drinkable Water

Abstract A method was developed for the selective determination of Se4+ in drinkable water by solid-phase microextraction (SPME) and gas chromatography/mass spectrometry (GC/MS). Se4+ was selectively derivatized to ethane, 1,1′-selenobis by reaction with sodium tetraethylborate, extracted by the SPME fiber, and determined by GC/MS. Both headspace (HS)–SPME and direct SPME were studied. The method requires only a few milliliters of sample and 20 min for completion. At 2.0 μg/L concentration, the relative standard deviation was 10.1% for HS–SPME and 9.1% for direct SPME. For HS–SPME, the theoretical detection limit was 81 ng/L and 166 ng/L for direct SPME. The recovery rate was 95%. The method was used to determine Se4+ in 10 tap water samples.

scholarly journals Multiresidue Determination of Pesticides in Drinking and Related Waters by Solid-Phase Extraction and Liquid Chromatography with Ultraviolet Detection: Interlaboratory Study

2002 ◽  
Vol 85 (2) ◽  
pp. 375-383 ◽  
Author(s):  
François van Hoof ◽  
Peter van Wiele ◽  
Françoise Acobas ◽  
Jean-Luc Guinamant ◽  
Auguste Bruchet ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Standard Deviation ◽  
Solid Phase Extraction ◽  
Relative Standard Deviation ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Tap Water ◽  
Phase Extraction ◽  
Relative Standard ◽  
Styrene Divinylbenzene

Abstract As part of a project funded by the European Commission (EC) for the development and evaluation of multiresidue methods for analysis of drinking and related waters, 17 European laboratories evaluated a method using styrene–divinylbenzene copolymer solid-phase extraction followed by liquid chromatography with diode array detection. The main aim of the study was to evaluate whether the method meets the requirements of EC Drinking Water Directive 98/83 in terms of accuracy, precision, and detection limit for 21 pesticides according to the following requirements: limit of detection, ≤0.025 μg/L; accuracy expressed as recovery, between 75 and 125%; and precision expressed as repeatability relative standard deviation of the method, <12.5%, and as reproducibility relative standard deviation of the method, <25%. Analyses for unknown concentrations were performed with commercial bottled and tap waters. All laboratories were able to achieve detection limits of 0.01 μg/L for all pesticides except pirimicarb (0.02 μg/L). The criteria for repeatability were met for all compounds. Terbutryn in bottled water and carbendazim in tap water did not meet the criteria for reproducibility. In terms of accuracy, the method met the requirements for all pesticides in both matrixes, except for metamitron. However, several compounds (linuron, terbutryn, propazine, metobromuron, and isoproturon) showed recoveries slightly below 75%.

scholarly journals Preparation of a new coating of graphene oxide/nickel complex on a nickelized metal surface for direct immersion solid phase microextraction of some polycyclic aromatic hydrocarbons

BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Yalda Pasandideh ◽  
Habib Razmi
Keyword(s):  
Graphene Oxide ◽  
Solid Phase Microextraction ◽  
High Efficiency ◽  
Mechanical Stability ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Limit Of Quantification ◽  
Coating Materials ◽  
Relative Standard ◽  
Validation Parameters

Abstract Background Solid-phase microextraction (SPME) is a versatile sampling and sample preparation technology that possess a significant application in the extraction and pre-concentration of a broad range of micro-pollutants from different kind of matrices. Selection and preparation of an appropriate fiber substrate and coating materials have always been the main challenges of the SPME procedure. This paper introduces a high-efficiency metal-based SPME fiber with a new chemical coating of nickel/graphene oxide/nickel tetraazamacrocyclic complex (Ni/GO/NiTAM). Result The Ni/GO/NiTAM sorbent was electroless deposited onto the surface of an aluchrom (Alu) wire, and then the prepared fiber was employed for the extraction and pre-concentration of some PAHs before their HPLC–UV analysis. The prepared fiber characterization data were assessed using FE-SEM, EDX, XRD, FT-IR, and BET techniques. The method validation parameters, including the linearity range (LRs: 0.10 to 200.0 µg L−1), the limit of detection (LODs: 0.03‒0.30 µg L−1), and the limit of quantification (LOQs: 0.10–1.00 µg L−1), under optimal conditions. The relative standard deviations (RSDs) of intra-day, inter-day, and single fiber repeatability (for the samples spiked at 25 µg L‒1) were in the range of 0.32–2.94, 1.20–4.09, and 1.42‒4.39%, respectively. In addition, the technique recoveries (RR %) and enrichment factors (EF) were in the range of 83.10‒107.80% and 83–164, respectively. Conclusion The fiber fabrication was simple, and the applied materials were also economical and easily accessible. Alu metal has high physicochemical and mechanical stability and thus can be a good alternative for the substrate of the fragile commercial SPME fibers. High rigidity and durability, long service life, and high extraction capability are some of the other advantages of the offered fiber.

Headspace Solid Phase Microextraction Procedure for the Detection of Polychlorinated Biphenyls in Seawater Sample

2013 ◽  
Vol 316-317 ◽  
pp. 383-386
Author(s):  
Xian Yin Ping ◽  
Yun Long Wang
Keyword(s):  
Polychlorinated Biphenyls ◽  
Film Thickness ◽  
Solid Phase Microextraction ◽  
Extraction Efficiency ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Headspace Solid Phase Microextraction ◽  
Relative Standard ◽  
Seawater Samples

Headspace solid phase microextraction combined with gas chromatography (HS-SPME–GC) method has been studied for determination of 7 polychlorinated biphenyls (PCBs) in seawater samples. To perform the HS-SPME polydimethylsiloxane (PDMS) (7, 30 and 100 µm film thickness) fibers were compared on the basis of their absorption capacities for the selected compounds, and PDMS 100 µm film thickness was selected. The influence of various parameters on PCBs extraction efficiency by HS-SPME was studied using GC-electron capture detector (ECD) compared with solid phase. The performance of proposed HS-SPME–GC methodology with respect to linearity, reproducibility and limit of detection (LOD) was evaluated by water spiked with target compounds. The linear range of most compounds was found to be between 0.1 and 100 µgL−1 and the limits of detection were between 15.2 and 63.8 ngL−1. The reproducibility of the method (n = 6), expressed as relative standard deviation (RSD), was between 4 and 10%. Finally, developed procedure was applied to determine selected PCBs in seawater samples.

Application of automated solid-phase microextraction to determine haloacetonitriles, haloketones, and chloropicrin in Canadian drinking water

2013 ◽  
Vol 48 (1) ◽  
pp. 85-98 ◽  
Author(s):  
Farhad Riazi Kermani ◽  
Anca-Maria Tugulea ◽  
Joan Hnatiw ◽  
Vadoud H. Niri ◽  
Janusz Pawliszyn
Keyword(s):  
Gas Chromatography ◽  
Drinking Water ◽  
Solid Phase Microextraction ◽  
Distribution Systems ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Electron Capture Detection ◽  
Experimental Conditions ◽  
Custom Made ◽  
Relative Standard

An automated headspace solid-phase microextraction gas chromatography mass spectrometry (HS-SPME-GC-MS) method was developed to monitor the occurrence of selected haloacetonitriles (HANs), haloketones (HKs), and chloropicrin (CP) in drinking water supplies. The method was rapid with analysis time of 30 min, including extraction and chromatographic run. Chemical ionization (CI) was used to increase the sensitivity of the method for the HKs. SPME fibers with seven different coatings including commercial polyacrylate (PA), carbowax/divinylbenzene (CW/DVB), polydimethylsiloxane (PDMS), polydimethylsiloxane/divinylbenzene (PDMS/DVB), carboxen/polydimethylsiloxane (CAR/PDMS), divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS), and a novel custom-made polydimethylsiloxane/divinylbenzene-N-vinylpyrrolidone (PDMS/DVB-NVP) were evaluated. The DVB/CAR/PDMS fiber was found more suitable for the range of the analytes and the novel PDMS/DVB-NVP fiber more efficient for the brominated acetonitriles under the experimental conditions. Method detection limits (MDLs) for the chlorinated acetonitriles and CP varied between 2 and 40 ng/L and for the brominated acetonitriles and HKs between 100 and 180 ng/L. Relative standard deviations (RSD %) of measurements were 4–7%. The method was applied in parallel with a liquid–liquid extraction gas chromatography electron capture detection (LLE-GC-ECD) method (EPA Method 551.1) to the analysis of drinking water samples from eight Canadian water treatment and distribution systems. The results generated by the two methods showed good agreement.

A Novel Electrochemiluminescence Sensor for Sensitive Determination of Carbaryl Based on Solid Phase Microextraction at NH2–Graphene–Nafion Modified Electrode

2015 ◽  
Vol 68 (5) ◽  
pp. 793 ◽  
Author(s):  
Sui Wang ◽  
Shasha Lv ◽  
Wenwen Wu ◽  
Zhiyong Guo
Keyword(s):  
Solid Phase Microextraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Initial Response ◽  
X Ray Diffraction ◽  
Relative Standard ◽  
Sensitive Determination ◽  
Response Current

Sensitive electrochemiluminescence (ECL) detection and solid phase microextraction (SPME) using a NH2–graphene–Nafion modified glassy carbon electrode was developed for carbaryl. The NH2–graphene was synthesised and characterised by Fourier transform infrared spectroscopy, scanning electron microscopy, and X-ray diffraction. The main parameters that affect the extraction efficiencies, such as the buffer and sample pH, and extraction time were investigated and optimised. The introduction of NH2–graphene into Nafion improves the conductivity of the film because of its electrical conductivity. The electrode enables the determination of carbaryl in the range from 5 × 10–4 to 10 μg mL–1, and the limit of detection was 2 × 10–4 μg mL–1 at a signal-to-noise ratio of 3. The ECL intensity retained 97 % of its initial response current after storage for 10 days, indicating a good storage stability of the sensor. The relative standard deviations (RSDs) of intra-assay and inter-assay were found to be 3.5 and 5.3 %, respectively, indicating an acceptable reproducibility. Furthermore, the ECL sensor was successfully applied to the selective and sensitive quantitative determination of carbaryl in river samples, the recoveries of carbaryl ranged from 99.0 to 108.0 %, and the RSDs were less than 5.0 %, which shows good reproducibility and high precision of analysis.

scholarly journals Processing of Flavor-Enhanced Oils: Optimization and Validation of Multiple Headspace Solid-Phase Microextraction-Arrow to Quantify Pyrazines in the Oils

Life ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 390
Author(s):  
Ziyan Xu ◽  
Chuan Zhou ◽  
Haiming Shi ◽  
Hong Zhang ◽  
Yanlan Bi ◽  
...  
Keyword(s):  
Solid Phase Microextraction ◽  
Incubation Temperature ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Temperature ◽  
Headspace Solid Phase Microextraction ◽  
Flavor Analysis ◽  
Relative Standard ◽  
Limit Of Quantitation

An efficient and effective multiple headspace-solid phase microextraction-arrow-gas chromatography-mass spectrometry (MHS-SPME-arrow-GCMS) analytical protocol is established and used to quantify the flavor compounds in oils. SPME conditions, such as fiber coating, pre-incubation temperature, extraction temperature, and time were studied. The feasibility was compared between SPME-arrow and the traditional fiber by loading different sample amounts. It was found that the SPME-arrow was more suitable for the MHS-SPME. The limit of detection (LODs) and limit of quantitation (LOQs) of pyrazines were in the range of 2–60 ng and 6–180 ng/g oil, respectively. The relative standard deviation (RSD) of both intra- and inter-day were lower than 16%. The mean recoveries for spiked pyrazines in rapeseed oil were in the range of 91.6–109.2%. Furthermore, this newly established method of MHS-SPME-arrow was compared with stable isotopes dilution analysis (SIDA) by using [2H6]-2-methyl-pyrazine. The results are comparable and indicate this method can be used for edible oil flavor analysis.

scholarly journals Pre-Concentration and Determination of Tetracyclines Antibiotics Residues in Water Samples Using RGO/Fe3O4 Nanocomposite as Extraction Sorbent

2021 ◽  
Vol 21 (5) ◽  
pp. 1196
Author(s):  
Ungku Amirul Arif Ungku Abdullah ◽  
Nor Suhaila Mohamad Hanapi ◽  
Wan Nazihah Wan Ibrahim ◽  
Nursyamsyila Mat Hadzir ◽  
Nurzaimah Zaini ◽  
...  
Keyword(s):  
Water Samples ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Magnetic Solid Phase Extraction ◽  
Coefficient Of Determination ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Magnetic Solid

Existing methods used in tracing Tetracyclines' antibiotics (TCAs) residues which pose serious environmental problems, consume high amounts of organic solvents, are time-consuming, and are relatively expensive. A simple and effective magnetic solid-phase extraction (MSPE) based on reduced graphene oxide/magnetite (RGO/Fe3O4) nanocomposite sorbent was successfully developed for preconcentration and extraction of TCAs residues from water samples. The analytes were determined by high-performance liquid chromatography with a diode-array detector (HPLC-DAD). The synthesized nanocomposite was characterized using Fourier-transform infrared spectroscopy (FTIR), X-ray diffractometry (XRD), and field emission scanning electron microscopy (FESEM). Sample pH, amount of adsorbent, sample volume, extraction time, desorption time, and desorption solvent were evaluated and optimized. Under optimized conditions, the method demonstrated good linearity over the concentration range of 0.05–1.0 mg L–1 with the coefficient of determination (R2) ≥ 0.9978. Limit of detection (LOD) and limit of quantification (LOQ) were 0.006–0.011 mg L–1 and 0.019–0.036 mg L–1, respectively. The accuracy and precision of the developed method were proven by good analyte recovery (89.77–106.33%) and acceptable precision with relative standard deviation, RSD ≤ 5.54%. The results showed that magnetic solid RGO/Fe3O4 could be a suitable adsorbent in the preconcentration and extraction of TCAs in water samples.

A Simple Vortex-Assisted Magnetic Dispersive Solid Phase Microextraction System for Preconcentration and Separation of Triazine Herbicides from Environmental Water and Vegetable Samples Using Fe3O4@MIL-100(Fe) Sorbent

2018 ◽  
Vol 101 (5) ◽  
pp. 1639-1646 ◽  
Author(s):  
Atefe Nasrollahpour ◽  
Seyyed Ershad Moradi
Keyword(s):  
Solid Phase Microextraction ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Correlation Coefficients ◽  
Environmental Water ◽  
Triazine Herbicides ◽  
Vegetable Samples ◽  
Relative Standard

Abstract A vortex-assisted magnetic dispersive solid phase microextraction coupled with high-performance liquid chromatography has been developed for the extraction and determination of triazine herbicides by using magnetic metal organic frameworks [Fe3O4@MIL-100(Fe)] in environmental water and vegetable samples. The Fe3O4@MIL-100(Fe) composite has been characterized by using X-ray diffraction spectroscopy, tunneling electron microscopy, thermogravimetric measurement, and Brunauer-Emmett-Teller analysis. The method is based on the sorption of triazine herbicides on Fe3O4@MIL-100(Fe) because of the complex formation between iron oxide nanoparticles and triazine herbicides beside π-π interactions between organic parts of Fe3O4@MIL-100(Fe) and triazine herbicides. The experimental parameters for the preconcentration of triazine herbicides, such as the type and volume of the eluent, pH, time of the sorption and desorption, and the amount of the sorbent, were optimized. Under the optimized conditions, the method was linear over the concentration range of 0.0061 to 70 ng/mL for each triazine herbicide, and the correlation coefficients ranged from 0.9988 to 0.9997. The limit of detection of the method at a signal-to-noise ratio of 3 was 2.0 to 5.3 ng/mL. The relative standard deviations for inter- and intraday assays were in the range of 5.8 to 10.2% and 3.8 to 6.3%, respectively.

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