Search results for "Detection limit"
showing 10 items of 810 documents
Matrix effects on solid-phase microextraction of organophosphorus pesticides from water
1997
Abstract This study develops a method for solid-phase microextraction (SPME) of eight organophosphorus pesticides, diazinon, fenthion, fenitrothion (sumithion), methyl-parathion, parathion, methyl-trithion, ethion and triazophos, from water. Determination is carried out by gas chromatography with nitrogen-phosphorus detection. To perform the SPME, poly(dimethylsiloxane) and polyacrylate fibers were initially compared on the basis of their absorption capacities for the selected pesticides, and polyacrylate was selected to accomplish the rest of assays. The main factors affecting the SPME process such as memory effect, stirring rate, extraction temperature and absorption-time profile were stu…
eta1-Allypalladium complexes with tridentate PNP’ ligand for the assembly of modified Screen Printed Electrodes: an electrochemical study.
2015
Specific Pd-based organometallic complex, in particular the [Pd(η1-CH2–CH=CH2)(P–N–P’)]BF4 was used for the assembly of chemically modified Screen Printed Electrodes (SPEs) and their electrochemical reactivity was also investigated. For this purpose potassium ferricyanide, hexaammineruthenium(III) chloride, sodium hexachloroiridate-(III) hydrate, ascorbic acid (AA), uric acid (UA), acetaminophen (Ac), guanine (G) and adenine (A) were used to study the electron-transfer processes, which occurred at modified SPEs, fabricated by using the [Pd(η1-CH2–CH=CH2)(P–N–P’)]BF4, applying the drop casting procedure. Interesting results were obtained in the case of the guanine (G) quantitative detection,…
Identification of unknown pesticides in fruits using ultra-performance liquid chromatography–quadrupole time-of-flight mass spectrometry
2007
Abstract Ultra-high-performance liquid chromatography–quadrupole time-of-flight mass spectrometry (UPLC-QqTOF-MS) is an emerging technique offering more rapid and efficient separation, as well as the possibility to obtain accurate mass measurement and tandem mass spectrometry (MS/MS). This paper deals with the use of UPLC-QqTOF-MS to identify the pesticide residues present in complex pear extracts. Carbendazim, imazalil, and ethoxyquin were successfully identified because of the accurate mass determination of their protonated molecule and their major fragments in the product ion mass spectra. A few plastic and latex additives were also found, most of them probably coming from the packaging …
Pressurised liquid extraction and capillary electrophoresis–mass spectrometry for the analysis of pesticide residues in fruits from Valencian markets…
2010
Abstract A procedure based in capillary electrophoresis–mass spectrometry (CE–MS) for the analysis of seven pesticides (flutolanil, simazine, haloxyfop, acifluorfen, dinoseb, picloram, and ioxynil) in four Mediterranean summer fruits with high water content (peaches, melon, watermelon, and apricot) is developed. Several conditions were studied for the optimisation of both, the separation and the electrospray (ESI) connection. The best results were obtained using 35 mM ammonium formiate (pH 9.7) as separation buffer, 20 °C as capillary temperature and 23 kV as applied voltage in an uncoated fused-silica capillary with 50 cm total length, 25 cm thermostated length, 25 cm at room temperature l…
Development of a pressurised liquid extraction and liquid chromatography with electrospray ionization-tandem mass spectrometry method for the determi…
2006
Amnesic shellfish poisoning (ASP) is a potentially lethal human toxic syndrome which is caused by domoic acid (DA) that originates in marine phytoplankton belonging to the Pseudonitzschia genus. A confirmatory and sensitive procedure has been developed and validated for the determination of DA in shellfish. The proposed method includes pressurised liquid extraction (PLE) with methanol/acetone (9:1), florisil ® cleanup purification inside the PLE extraction cell and detection by liquid chromatography (LC) coupled to electrospray ionization in positive mode tandem mass spectrometry (ESI-MS–MS). Comparison of ionization sources (ESI, atmospheric pressure ionization (APCI) atmospheric pressure …
Validation of Powder X-Ray Diffraction Following EN ISO/IEC 17025
2012
: Powder X-ray diffraction (PXRD) is used widely in forensic science laboratories with the main focus of qualitative phase identification. Little is found in literature referring to the topic of validation of PXRD in the field of forensic sciences. According to EN ISO/IEC 17025, the method has to be tested for several parameters. Trueness, specificity, and selectivity of PXRD were tested using certified reference materials or a combination thereof. All three tested parameters showed the secure performance of the method. Sample preparation errors were simulated to evaluate the robustness of the method. These errors were either easily detected by the operator or nonsignificant for phase iden…
Minimizing the impact of sample preparation on analytical results: In-tube solid-phase microextraction coupled on-line to nano-liquid chromatography …
2020
The degradation kinetics and residual levels of the sulfonylurea herbicide tribenuron-methyl (TBM) in different environmental waters were studied using in tube-solid phase microextraction (IT-SPME) coupled on-line to nano-liquid chromatography (nanoLC) and UV diode array detection (DAD). This approach combines the high extraction efficiency of IT-SPME using polymeric coatings reinforced with metal oxide nanoparticles and the high sensitivity attainable by nanoLC, making possible the determination of TBM at low ppb levels (limit of detection, 0.25 ppb) without altering the sample matrix. The present study demonstrated that the preservation of the sample properties is essential to ensure accu…
Chlorinated acetic and propionic acids in pine needles from industrial areas
1998
Abstract Concentrations of chlorinated acetic and propionic acids in pine needles from the surroundings of a pulp and paper mill and a metal reclamation plant were measured. Different ways of extraction and chromatographic separation were tried. Ultrasonic extraction with water of the powdered needles was found to be efficient. The acids were analysed as their pentafluorobenzyl esters with GC-ECD. The ECD sensitivity of the pentafluorobenzyl derivatives was good. The detection limit was below 1 ng/g for the chlorinated acetic and propionic acids. The concentrations of dichloroacetic acid and 2,2-dichloropropionic acid in fresh needles were on the 0–4 ng/g level. Monochloroacetic acid, 2-chl…
Analysis of Polycyclic Aromatic Hydrocarbons and Their Oxygen-Containing Derivatives and Metabolites in Soils
2010
Although polycyclic aromatic hydrocarbons (PAHs) have been extensively studied, the knowledge of their oxygen-containing derivatives and metabolites (OPAHs) in soils is limited. We modified and tested an existing analytical protocol involving pressurized liquid extraction of soil followed by fractionation of target compounds into PAHs and OPAHs on a silica gel column and gas chromatography/ mass spectrometry-based separation and quantification. Polycyclic aromatic hydrocarbons and carbonyl-OPAHs were quantified directly after separation on silica gel columns, and hydroxyl/carboxyl-OPAHs were quantified after silylation with N,O-bis(trimethylsilyl)trifluoroacetamide. Recoveries between 78 an…
Determination of n-alkanes, PAHs and hopanes in atmospheric aerosol: evaluation and comparison of thermal desorption GC-MS and solvent extraction GC-…
2019
Organic aerosol (OA) constitutes a large fraction of fine particulate matter (PM) in the urban air. However, the chemical nature and sources of OA are not well constrained. Quantitative analysis of OA is essential for understanding the sources and atmospheric evolution of fine PM, which requires accurate quantification of some organic compounds (e.g., markers). In this study, two analytical approaches, i.e., thermal desorption (TD) gas chromatography-mass spectrometry (GC-MS) and solvent extract (SE) GC-MS were evaluated for the determination of n-alkanes, polycyclic aromatic hydrocarbons (PAHs), and hopanes in ambient aerosol. For the SE approach, the recovery obtained is 89.3–101.5&…