Search results for "LIMIT"
showing 10 items of 2826 documents
Matrix solid-phase dispersion extraction procedure for multiresidue pesticide analysis in oranges.
1996
A multiresidue extraction method based on matrix solid-phase dispersion (MSPD) is optimized for the extraction and gas chromatographic screening of eighteen insecticides (aldrin, carbophenothion, captafol, chlorpyriphos, chlorfenvinphos, diazinon, dicofol, alpha-endosulfan, beta-endosulfan, ethion, fenitrothion, folpet, methidathion, malathion, methyl-azinphos, methyl-parathion, phosmet, and tetradifon) from oranges. After optimization of different parameters, such as type of solid phase used and the amount of solid phase or eluent, recoveries ranged from 67 to 102% with relative standard deviations ranging from 2 to 10%. The limits of detection, calculated as 3 times the baseline noise ran…
Improving detection limits for organotin compounds in several matrix water samples by derivatization-headspace-solid-phase microextraction and GC-MS.
2010
Triethyltin, tributyltin, diphenyltin and triphenyltin were selected as model compounds. The method is based on in situ ethylation and simultaneous headspace-solid-phase microextraction (HS-SPME) and gas chromatographic-mass spectrometry analysis (GC-MS). The extraction procedure was optimized studying some variables such as reaction time, salinity, sample volume and headspace volume. SPME-GC-MS and SPME-GC-FID techniques were compared; quality assurance parameters such as sensitivity, selectivity and precision were established. The proposed procedure showed limits of detection between 0.025 and 1 ng/L. The linearity was in the 0.025-5000 ng/L range. The precision expressed as relative stan…
Direct analysis in real-time high-resolution mass spectrometry as a valuable tool for polyphenols profiling in olive oil
2018
A fast and reliable method to characterize the polyphenolic compound profiles in extra virgin olive oil (EVOO) has been developed using direct analysis in real time (DART) and linear ion-trap Orbitrap mass spectrometry (LTQ-Orbitrap-MS). Hydroalcoholic extraction increased speed and reduced matrix effects, and DART-MS/MS ensured accurate analysis. Characterization of polyphenol fingerprinting in EVOO samples takes 2 min. This method exhibited proper linearity (R2 ≥ 0.99) in the range of 5–2500 μg g−1, limit of detection (LOD) of 1.5 μg g−1 (signal-to noise S/N = 3), and limits of quantitation (LOQs) of 5 μg g−1 (S/N = 10) for resveratrol (a polyphenol not detected in olive oil). Six spiked …
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…