Search results for "Limit of Detection"
showing 10 items of 146 documents
Implementing the contamination prevention programs in the pesticide industry by infrared spectroscopy.
2014
Abstract An infrared spectroscopy based methodology has been successfully developed to implement contamination prevention programs in the pesticide industry. Sensitivity of the IR procedure, traditionally considered the Achilles Hell of the technique, has been improved by using a transmission cell with an open upper side, an internal volume of 35 µL and an optical pathlength of 0.5 mm, providing detection limits of 32 mg L−1 for folpet and 48 mg L−1 for cymoxanil. The manufacturing of folpet and cymoxanil was employed as an example and the IR methodology was validated for the implementation of contamination prevention programs in the pesticide industry. The swab test and rinsate method were…
Optimization of sample preparation conditions for detecting trace amounts of β-tegafur in α- and β-tegafur mixture.
2012
We report a semiquantitative method for determining trace amounts (<1%) of thermodynamically stable forms in polymorphic mixtures, focusing on sample preparation ef- fects on solid phase transitions. Tegafur (5-fluoro-1-(oxolan-2-yl)-1,2,3,4-tetrahydropyrimidine- 2,4-dione) was used as a model material in this study. The amounts of the thermodynamically stable $ tegafur were increased to levels detectable by powder X-ray diffractometry by grind- ing the samples in a ball mill in the presence of water. The limit of detection for this method was as low as 0.0005% of $ tegafur in " and $ tegafur mixtures. The amount of $ tegafur after sample preparation was found to be proportional to the init…
Determination of total mercury in nuts at ultratrace level
2014
Abstract Total mercury, at μg kg−1 level, was determined in different types of nuts (cashew nut, Brazil nuts, almond, pistachio, peanut, walnut) using a direct mercury analyser after previous sample defatting and by cold vapour atomic fluorescence spectrometry. There is not enough sensitivity in the second approach to determine Hg in previously digested samples due to the strong matrix effect. Mercury levels in 25 edible nut samples from Brazil and Spain were found in the range from 0.6 to 2.7 μg kg−1 by using the pyrolysis of sample after the extraction of the nut fat. The accuracy of the proposed method was confirmed by analysing certified reference materials of Coal Fly Ash-NIST SRM 1633…
Optimization of Matrix Solid-Phase Dispersion method for simultaneous extraction of aflatoxins and OTA in cereals and its application to commercial s…
2010
Abstract A method based on Matrix Solid-Phase Dispersion (MSPD) has been developed for the determination of 5 mycotoxins (ochratoxin A and aflatoxins B and G) in different cereals. Several dispersants, eluents and ratios were tested during the optimization of the process in order to obtain the best results. Finally, samples were blended with C 18 and the mycotoxins were extracted with acetonitrile. Regarding to matrix effects, the results clearly demonstrated the necessity to use a matrix-matched calibration to validate the method. Analyses were performed by liquid chromatography–triple quadrupole-tandem mass spectrometry (LC–QqQ-MS/MS). The recoveries of the extraction process ranged from …
Simultaneous determinations of zirconium, hafnium, yttrium and lanthanides in seawater according to a co-precipitation technique onto iron-hydroxide.
2013
Very low concentrations (pg mL(-1) or sub-pg mL(-1) level) along with the high salinity are the main problems in determining trace metal contents in seawater. This problem is mainly considered for investigations of naturally occurring YLOID (Y and Lanthanides) and Zr and Hf in order to provide precise and accurate results. The inductively coupled plasma mass spectrometry (ICP-MS), both in high and low resolution, offers many advantages including simultaneous analyses of all elements and their quantitative determination with detection limits of the order of pg mL(-1). However in the analysis of YLOID in seawater, a better determination needs an efficient combination of ICP-MS measurement wit…
Selective and sentivive method based on capillary liquid chromatography with in-tube solid phase microextraction for determination of monochloramine …
2015
Abstract Due to the difficulties of working with chloramines, a critical examination of monochloramine standard preparation has been performed in order to select the best synthesis conditions. The analyte has been determined by in-tube solid phase extraction coupled to capillary liquid chromatography with UV detection (IT-SPME Capillary LC DAD). Potential factors affecting the response of monochloramine such as the pH of mobile phase and the volume of sample processed by IT-SPME Capillary LC DAD have been investigated and optimized. According to the results of the study, 0.1 mL or 4.0 mL of sample at neutral pH were loaded in the chromatographic system. A sensitive and selective method has …
Multimycotoxin LC-MS/MS Analysis in Tea Beverages after Dispersive Liquid-Liquid Microextraction (DLLME).
2017
The aim of the present study was to develop a multimycotoxin liquid chromatography tandem mass spectrometry (LC-MS/MS) method with a dispersive liquid-liquid microextraction procedure (DLLME) for the analysis of AFs, 3aDON, 15aDON, NIV, HT-2, T-2, ZEA, OTA, ENNs, and BEA in tea beverages and to evaluate their mycotoxin contents. The proposed method was characterized in terms of linearity, limits of detection (LODs), limits of quantification (LOQs), recoveries, repeatability (intraday precision), reproducibility (interday precision), and matrix effects to check suitability. The results show LODs in the range of 0.05-10 μg/L, LOQs in the range of 0.2-33 μg/L, and recoveries in the range of 65…
Determination of the new psychoactive substance dichloropane in saliva by microextraction by packed sorbent – Ion mobility spectrometry
2018
Abstract A simple procedure based on microextraction by packed sorbent (MEPS) has been proposed for the extraction of dichloropane in oral fluids and its determination by ion mobility spectrometry (IMS). Extraction conditions such as type of sorbent (octyl and octadecyl silica), sample pH, number of sample loadings, and elution volume were evaluated to obtain the most appropriate values. Dichloropane was extracted from saliva samples using C8 MEPS, loading with 100 μL sample (adjusted to pH 7) in 4 cycles, washing with 100 μL deionized water, and eluting with 50 μL 2-propanol in 10 cycles. The proposed MEPS procedure has been validated in terms of linearity, accuracy, and precision. A limit…
Selective solid-phase extraction of organophosphorus pesticides and their oxon-derivatives from water samples using molecularly imprinted polymer fol…
2020
Abstract A molecularly imprinted polymer was synthesized and characterized to be used as solid-phase extraction sorbent for simultaneous chlorpyrifos and diazinon and their oxon derivatives. Several imprinted polymers were prepared and evaluated in a retention study of these analytes compared with a non-printed polymer. Several parameters affecting the extraction of imprinted polymer such as washing solvent, composition and volume of the eluting solvent and sample volume, were also investigated. Under the optimum conditions, the developed method provided satisfactory limits of detection ranging between 0.07 µg L−1 to 0.12 µg L−1 and the material showed an excellent reusability (> 50 reuses)…
Determination of volatile organic compounds in contaminated air using semipermeable membrane devices
2009
Abstract Semipermeable membrane devices (SPMDs) were evaluated as passive samplers for the determination of 26 volatile organic compounds (VOCs) in contaminated air of occupational environments. A direct methodology based on the use of head-space-gas chromatography–mass spectrometry (HS-GC–MS) was developed for VOCs determinations in SPMDs, without any sample pre-treatment and avoiding the use of solvents. A desorption temperature of 150 °C for 10 min was sufficient for a sensitive VOCs determination providing limits of detection in the range of 15 ng SPMD−1 for 21 of 26 studied compounds. Linear and equilibrium uptake models were established for each VOC from compound isotherms. Highly vol…