Search results for "Preparation method"
showing 10 items of 31 documents
Use of the modified quick easy cheap effective rugged and safe sample preparation approach for the simultaneous analysis of type A- and B-trichothece…
2010
A suitable extraction and purification method for the simultaneous liquid chromatography-mass spectrometry (LC-MS) determination of five mycotoxins, three type A, diacetoxyscirpenol (DAS), T-2 toxin (T-2) and HT-2 toxin (HT-2), and two type B-trichothecenes, deoxynivalenol (DON) and nivalenol (NIV), has been optimised using a modified "Quick Easy Cheap Effective Rugged and Safe" (QuEChERS) method. Different solvents were studied in the extraction procedure to obtain better recoveries, which ranged from 86 to 108%, using a 85/15 (v/v) mixture of methanol/acetonitrile. The values obtained for recovery, repeatability and reproducibility of the optimized method are in agreement with Commission …
Drop-on-demand sample introduction system coupled with the flowing atmospheric-pressure afterglow for direct molecular analysis of complex liquid mic…
2012
One of the fastest developing fields in analytical spectrochemistry in recent years is ambient desorption/ionization mass spectrometry (ADI-MS). This burgeoning interest has been due to the demonstrated advantages of the method: simple mass spectra, little or no sample preparation, and applicability to samples in the solid, liquid, or gaseous state. One such ADI-MS source, the flowing atmospheric-pressure afterglow (FAPA), is capable of direct analysis of solids just by aiming the source at the solid surface and sampling the produced ions into a mass spectrometer. However, direct introduction of significant volumes of liquid samples into this source has not been possible, as solvent loads c…
Occurrence and risk assessment of mycotoxins, acrylamide, and furan in Latvian beer.
2018
This work reports data on the occurrence of nine mycotoxins and two food processing contaminants - acrylamide and furan - in a total of 100 beers produced in Latvia. Mycotoxins were detected by high-performance liquid chromatography (HPLC) coupled with time-of-flight mass spectrometry, acrylamide by HPLC coupled with quadrupole-Orbitrap mass spectrometry, and furan by headspace gas chromatography-mass spectrometry. The most frequently occurring mycotoxins were HT-2 and deoxynivalenol (DON), which were detected in 52% and 51% of the analysed samples. The highest content was observed for DON, reaching the maximum of 248 µg kg-1. Furan was ubiquitous, and 74% of the samples contained acrylamid…
X-ray analysis on the nanogram to microgram scale using porous complexes
2012
X-ray single-crystal diffraction (SCD) analysis has the intrinsic limitation that the target molecules must be obtained as single crystals. Here we report a protocol for SCD analysis that does not require the crystallization of the sample. In our method, tiny crystals of porous complexes are soaked in a solution of the target, such that the complexes can absorb the target molecules. Crystallographic analysis clearly determines the absorbed guest structures along with the host frameworks. Because the SCD analysis is carried out on only one tiny crystal of the complex, the required sample mass is of the nanogram–microgram order. We demonstrate that as little as about 80 nanograms of a sample …
Retrospective screening of pesticide metabolites in ambient air using liquid chromatography coupled to high-resolution mass spectrometry
2015
A new methodology for the retrospective screening of pesticide metabolites in ambient air was developed, using liquid chromatography coupled to Orbitrap high-resolution mass spectrometry (UHPLC-HRMS), including two systematic workflows (i) post-run target screening (suspect screening) and (ii) non-target screening. An accurate-mass database was built and used for the post-run screening analysis. The database contained 240 pesticide metabolites found in different matrixes such as air, soil, water, plants, animals and humans. For non-target analysis, a "fragmentation-degradation" relationship strategy was selected. The proposed methodology was applied to 31 air samples (PM10) collected in the…
On-line preconcentration strategies for analyzing pesticides in fruits and vegetables by micellar electrokinetic chromatography.
2007
Five pesticides (fludioxonil, procymidone, pyriproxyfen, dinoseb and carbendazim) were separated in reversed migration micellar electrokinetic chromatography (RM-MEKC) using 20 mmol l(-1) phosphate buffer at pH 2.3, containing 25 mmol l(-1) sodium dodecylsulfate and 10% methanol. Three on-line concentration strategies, sweeping (SW), normal stacking with reversed migration and a water plug (SRW) and stacking with reverse migration and removal of sample matrix using polarity switching (SRMM), were compared. About 10-, 30- and 50-fold increases in detection sensitivity, compared with standard hydrodynamic injection (5 s at 0.5 psi), were observed with SW, SRW and SRMM, respectively. Limits of…
Pharmacokinetics of oligodeoxynucleotides encapsulated in liposomes: effect of lipid composition and preparation method
2000
1. The effect of the method employed to prepare liposomes and their lipid composition were evaluated in terms of the encapsulation efficiency and pharmacokinetic features of two oligodeoxynucleotides of a 21 mer: the normal (N-Odn) and the phosphorothioate (S-Odn) oligodeoxynucleotide. 2. Liposomes were prepared by the classical method of multilamellar vesicles (MV) and by the dehydration-rehydration method (DR). Two lipid mixtures were used to prepare liposomes--the predominant lipid being phosphatidylcholine (PC) and sphingomyelin (SM) respectively. 3. The DR method for liposome preparation provided the highest encapsulation efficiency, regardless of liposome lipid composition and the typ…
Processes during preparation of lead/acid battery positive plates from tetrabasic lead sulfate (4BS) pastes
1993
Abstract Tthe processes studied during this investigation were paste mixing and curing. Tetrabasic lead sulfate 4BS pastes were prepared by solution and paste methods both from α-PbO and mill oxides, and the development of 4BS was carried out already during the paste mixing stage. the 4BS pastes were characterized by SEM, TEM, XRD and wet-chemical methods, and the results were compared with those obtained from the characterization of corresponding tribasic lead sulfate (3BS) pastes. The preparation method was found to be one dominating factor affecting both the morphology and structure of 4BS active masses. The selection of raw material gave an additional effect on the morphology. Additiona…
Spectroscopic studies of 5,5′-dimethoxy-3,3,′-disulfobutyl-9-ethylthiacarbocyanine (DDTC) in solutions and immobilized in sol-gel matrices
1998
Abstract Absorption spectra of 5,5′-dimethoxy-3,3,′-disulfobutyl-9-ethylthiacarbocyanine (DDTC) in aqueous solutions and immobilized in xerogels prepared by the sol-gel method were obtained. Influence of pH, detergent (Triton X-100), ethanol addition and sol-gel preparation method on the dye aggregation equilibria and its photostability were investigated. In liquid solutions lowering of pH, as well as addition of the detergent, shift the aggregation equilibrium towards the DDTC monomeric form. However, while more acidic conditions result in a decrease of the dye stability, addition of the detergent has a slightly stabilizing effect on the dye. However, addition of ethanol drastically reduce…
Die bestimmung der molekulargewichtsverteilung von nichtkristallisierenden polymeren mit dem elektronenmikroskop. I. Präparationsmethoden und kontrol…
1970
Bei der elektronenmikroskopischen Abbildung von Einzelmolekulen treten eine Reihe von praparativen Schwierigkeiten auf, welche dazu gefuhrt haben, das man trotz zahlreicher Arbeiten diese Methode bisher noch nicht zu einem Standardverfahren entwickeln konnte. Ein Haupthindernis stellt das Auftreten von Artefakten dar, die den nichtkristallinen Polymermolekulen tauschend ahnlich sehen. Zur Erkennung und Vermeidung dieser „Scheinmolekule” ist es notwendig, quantitative Praparations- und Kontrollmethoden zu entwickeln. Es eignen sich zwei Verfahren: einmal die sogenannte Tropfenmethode und zum anderen die Gefriertrocknungsmethode. Mit Hilfe dieser Verfahren gelingt es, das Artefaktproblem zu l…