Search results for "sample preparation"
showing 10 items of 343 documents
Routine application using single quadrupole liquid chromatography-mass spectrometry to pesticides analysis in citrus fruits.
2005
Abstract A rapid and sensitive liquid chromatography–electrospray ionization–mass spectrometry method has been developed for the routine analysis of buprofezin, bupirimate, hexaflumuron, tebufenpyrad, fluvalinate and pyriproxyfen in citrus fruits. Extracts were obtained by matrix solid-phase dispersion (MSPD) using C 18 as dispersant and dichloromethane-methanol (80:20, v/v) as eluent. Matrix effects were tested for all matrices by addition of standard to sample blank extracts (samples containing no detectable residues). Mean recoveries obtained at fortification levels between 0.01 and 5 mg kg −1 were 57–97% with relative standard deviations (RSDs) from 5 to 19%. The limits of quantificatio…
Determination of macrolide antibiotics in meat and fish using pressurized liquid extraction and liquid chromatography–mass spectrometry
2008
We developed a method for determining the quantities of seven macrolide antibiotics in meat and fish by using pressurized liquid extraction (PLE) and liquid chromatography-mass spectrometry with electrospray ionization (LC-(ESI)MS). The PLE was optimized with regard to solvents, temperature, pressure, extraction time and number of cycles. The optimum conditions were: methanol as the extraction solvent; a temperature of 80 degrees C; a pressure of 1500psi; an extraction time of 15min; 2 cycles; a flush volume of 150% and a purge time of 300s. All recoveries for macrolide antibiotics were over 77% at 200mug/kg, except for erythromycin, which was 58%. The repeatability and reproducibility on d…
Direct infusion mass spectrometry as a fingerprint of protein-binding media used in works of art
2005
A direct infusion mass spectrometry method for the characterization of proteinaceous glues from binding media used in pictorial works of art prior to conservation or restoration treatment is proposed. Amino acids are released by acid hydrolysis and dissolved in a mixture of acidic water and ethanol. This mixture is directly infused into a mass spectrometer without any derivatization. The mass spectrometer is operated in positive ion electrospray mode (ESI-MS) to yield [M+H]+ ions for the amino acids. Relative amounts of each amino acid are calculated for each protein (beef and porcine gelatines, albumin, casein and egg). The analyzed proteins were satisfactorily distinguished. The method is…
Effects of Weak Links in the Nonlinear Microwave Response of MgB2 Superconductor
2006
We report experimental results of second-harmonic (SH) response at microwave frequency in several ceramic MgB2 samples, prepared by different methods. The SH signal has been investigated as a function of the temperature and DC magnetic field. The investigation has been carried out at low magnetic fields, where nonlinear processes arising from motion of Abrikosov fluxons are ineffective. We show that the low-temperature SH emission is ascribable to processes involving weak links. Comparison among the peculiarities of the SH signal radiated by the different samples shows that the presence of weak links strongly depends on the sample preparation method, as well as the purity and morphology of …
Standardisation, Reference Materials and Comparative Measurements for Surface Area and Pore Characterisation
1991
Summary This paper reviews current activities to standardise measuring procedures for surface area and pore size determination. Comparative measurements at different laboratories using candidate reference materials revealed that surfaces of highly dispersed materials can be affected remarkably during storing and sample preparation. On account of the fractal nature of these materials, the results depend on the measuring methods. Reference materials of dispersed materials are offered by national and international standardisation administrations and by industrial distributers. The standardisation of measuring methods becomes more and more international (ISO, IUPAC). The survey includes tables …
Combined use of liquid chromatography triple quadrupole mass spectrometry and liquid chromatography quadrupole time-of-flight mass spectrometry in sy…
2012
As a suitable way for routine screening of pesticides and control of other organic contaminants in water, the combination of liquid chromatography triple quadrupole tandem mass spectrometry (LC-QqQ-MS/MS) and liquid chromatography-hybrid quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) has been applied to the analysis of 63 surface and waste water samples after conventional solid-phase extraction (SPE). The extracts were screened for 43 pesticides or degradation products by LC-QqQ-MS/MS achieving limits of detection (LOD) ranged from 0.04 to 2 ng L(-1). Of the 43 selected pesticides, 33 were detected in water samples. The ESI-QTOF MS instrument was run using two simultaneous acquisi…
Multivariate Assessment of Procedures for Molecularly Imprinted Polymer Synthesis for Pesticides Determination in Environmental and Agricultural Samp…
2021
In the case of quantitative and qualitative analysis of pesticides in environmental and food samples, it is required to perform a sample pre-treatment process. It allows to minimalize the impact of interferences on the final results, as well as increase the recovery rate. Nowadays, apart from routinely employed sample preparation techniques such as solid-phase extraction (SPE) or solid-phase microextraction (SPME), the application of molecularly imprinted polymers (MIPs) is gaining greater popularity. It is mainly related to their physicochemical properties, sorption capacity and selectivity, thermo-mechanical resistance, as well as a wide range of polymerization techniques allowing to obta…
Influence of sample pan on the thermal behaviour of KSCN measured with TG
2003
Abstract In this study, the influence of the sample pan on the thermal behaviour of potassium thiocyanate (KSCN) was investigated. The measurements were performed with thermogravimetry (TG) and the two sample pans used were a platinum pan and a ceramic crucible. The samples were heated to 400–950 °C and the thermal products were identified by powder diffraction. The thermal behaviour of KSCN was found to be dependent on the sample pan used. With the platinum sample pan KSCN reacted in the first step into a mixture of K 2 SO 4 and potassium tetracyanoplatinate (K 2 Pt(CN) 4 ). In the second step, the mixture reacted further to pure K 2 SO 4 . In the ceramic sample crucible, however, the reac…
Optimization of a matrix solid-phase dispersion method for the analysis of pesticide residues in vegetables
1996
A multiresidue method based on matrix solid-phase dispersion (MSPD) is studied to determine chlorfenvinfos, chlorpyrifos, fenarimol, iprodione, procimydone, propiconazole, tetradifon, triadimefon and vinclozolin in artichokes, green beans, lettuces and tomatoes. Alumina, silica and Florisil were assessed as extracting phases, and the extracts from Florisil were the cleanest. To facilitate manual extraction, sand was added to the sample together with the dispersing phase. Three eluting systems were then studied, and dichloromethane proved to be the best. Further purification can be performed using solid-phase cleanup after diluting extracts with aqueous solutions. Octyl- and octadecyl-silica…
Determination of the cultivar and aging of Sicilian olive oils using HPLC-MS and linear discriminant analysis
2010
A large number of certified samples (84) of Sicilian olive oils arising from the eight cultivars most represented in Sicily (Biancolilla, Cerasuola, Moresca, Nocellara del Belice, Nocellara Etnea, Oglialora Messinese, Brandofino and Tonda Iblea) have been collected and analyzed by HPLC/MS using an atmospheric pressure chemical ionization (APCI) source. The sample preparation is very simple; in fact, the oil samples are diluted without any chemical derivatization. A following statistical data treatment by general discriminant analysis (GDA) allows the determination of the olive oil cultivar. Furthermore, changes in the composition of glyceridic components of the olive oils lead to easy discr…