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.

Analysis of Polychlorinated Biphenyls in Biological Samples by Headspace Solid Phase Microextraction Coupled with Gas Chromatography

2015 ◽  
Vol 1092-1093 ◽  
pp. 770-773
Author(s):  
Yong Li Liu ◽  
Xian Yin Ping
Keyword(s):  
Gas Chromatography ◽  
Polychlorinated Biphenyls ◽  
Biological Samples ◽  
Solid Phase Microextraction ◽  
Extraction Efficiency ◽  
Solid Phase ◽  
Headspace Solid Phase Microextraction ◽  
Relative Standard ◽  
Divinyl Benzene

Based on headspace solid phase microextraction (HS-SPME) procedure coupled with gas chromatography, a method for determination of polychlorinated biphenyls (PCBs) in biological samples was developed. The optimization of factors influencing the performances of SPME was studied in detail. To perform the HS-SPME polydimethylsiloxane (PDMS), polydimethylsiloxane-divinyl benzene (PDMS-DVB) and polyacrylate (PA) fibers were compared on the basis of their absorption capacities for the selected compounds, and PDMS-DVB fiber was selected. The influence of various parameters on PCBs extraction efficiency by HS-SPME was studied using GC-electron capture detector (ECD). The linear range of most compounds was found to be between 1 and 100 μgL−1 and the limits of detection were between 20.1 and 42.3 ngL−1. The reproducibility of the method (n = 6), expressed as relative standard deviation (RSD), was between 4.63 and 9.71%. Finally, the optimization of method was applied to determine selected PCBs in biological samples.

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 Simultaneous Determination of Some Phenothiazine Derivatives in Human Blood by Headspace Solid-Phase Microextraction and Gas Chromatography with Nitrogen-Phosphorus Detection

2008 ◽  
Vol 91 (6) ◽  
pp. 1354-1362 ◽  
Author(s):  
Natsuko Shinmen ◽  
Xiao-Pen Lee ◽  
Takeshi Kumazawa ◽  
Chika Hasegawa ◽  
Yasuhiro Ishiwata ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Whole Blood ◽  
Solid Phase Microextraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Regression Equations ◽  
Phenothiazine Derivatives ◽  
Headspace Solid Phase Microextraction ◽  
Coefficients Of Variation

Abstract Chlorpromazine, levomepromazine, promazine, triflupromazine, and trimeprazine were simultaneously determined in human whole blood and plasma by combining headspace solid-phase microextraction and gas chromatography with nitrogenphosphorus detection. Extraction efficiency for the phenothiazine derivatives was 0.0130.117 for both sample types. Regression equations were linear [correlation coefficient (r) 0.99510.9999] within the range 2.5200 ng/0.5 mL for triflupromazine and trimeprazine, and 6.3200 ng/0.5 mL for chlorpromazine, levomepromazine, and promazine. The limit of detection for each compound was 0.23.9 ng/0.5 mL whole blood and plasma. Intraday and interday coefficients of variation for all phenothiazines in both human samples were commonly <15 and 20, respectively. We also report the determination of levomepromazine in human plasma after oral administration.

scholarly journals Optimization of Headspace Solid-Phase Microextraction Conditions for the Identification of Phytophthora cinnamomi Rands

Plant Disease ◽  
2014 ◽  
Vol 98 (8) ◽  
pp. 1088-1098 ◽  
Author(s):  
Rui Qiu ◽  
Dong Qu ◽  
Giles E. St. J. Hardy ◽  
Robert Trengove ◽  
Manjree Agarwal ◽  
...  
Keyword(s):  
Solid Phase Microextraction ◽  
Extraction Efficiency ◽  
Phytophthora Cinnamomi ◽  
Solid Phase ◽  
Colony Development ◽  
Fiber Types ◽  
Headspace Solid Phase Microextraction ◽  
Morphological Studies ◽  
Relative Standard

A robust technique was developed to identify Phytophthora cinnamomi using headspace solid-phase microextraction (HS-SPME) combined with gas chromatography (GC) coupled to a flame ionization detector (FID) for analyzing volatile organic compounds (VOCs). Six fiber types were evaluated and results indicated that the three-phase fiber 50/30 μm divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) had the highest extraction efficiency for both polar and nonpolar GC columns. The maximum extraction efficiency (equilibrium absorption) was achieved 16 h after fiber exposure in the HS. Absorbed compounds on the fiber were completely desorbed in the GC injector after 5 min at 250°C. Compared with the nonpolar column, the polar column showed optimum separation of VOCs released from P. cinnamomi. Under the optimized HS-SPME and GC/FID conditions, lower detection limits for the four external standards was found to be between 1.57 to 27.36 ng/liter. Relative standard deviations <9.010% showed that the method is precise and reliable. The method also showed good linearity for the concentration range that was analyzed using four standards, with regression coefficients between 0.989 and 0.995, and the sensitivity of the method was 104 times greater than that of the conventional HS method. In this study, the VOC profiles of six Phytophthora spp. and one Pythium sp. were characterized by the optimized HS-SPME-GC method. The combination of the VOCs creates a unique pattern for each pathogen; the chromatograms of different isolates of P. cinnamomi were the same and the specific VOC pattern of P. cinnamomi remained consistently independent of the growth medium used. The chromatograms and morphological studies showed that P. cinnamomi released specific VOCs at different stages of colony development. Using the optimized HS-SPME GC method, identification of P. cinnamomi from 15 in vivo diseased soil samples was as high as 100%. Results from this study demonstrate the feasibility of this method for identifying P. cinnamomi and the potential use of this method for physiological studies on P. cinnamomi.

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.

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