Search results for "liquid"
showing 10 items of 4351 documents
ChemInform Abstract: A Straightforward Copper-Free Palladium Methodology for the Selective Alkynylation of a Wide Variety of S-, O-, and N-Based Mono…
2009
Abstract High-yield alkynylations are successfully achieved by a simple and widely accessible catalytic system for an unprecedented variety of heterocyclic bromides and chlorides in position -2, -3 or -5: pyridine, quinoline, thiophene, furan, thiazole, benzothiazole, pyrimidine, pyridazine, pyrazine, dioxepin halides are efficiently functionalized in short time reactions. This copper-free methodology employs 1 mol % palladium only, with inexpensive PPh3 and amine base. The ionic liquid solvent allows a straigtforward separation of products and recycling opportunity. Unsuitable substrates and secondary reactions are also reported in order to point out further progress in cross-coupling usin…
Analysis of mycotoxins in barley using ultra high liquid chromatography high resolution mass spectrometry: comparison of efficiency and efficacy of d…
2012
The effectiveness of four extraction methods (modified QuEChERS, matrix solid-phase dispersion (MSPD), solid-liquid extraction (SLE) and solid-phase extraction (SPE) clean-up) were evaluated for simultaneous determination of 32 mycotoxins produced by the genus Fusarium, Claviceps, Aspergillus, Penicillium and Alternaria in barley by ultra high pressure liquid chromatography coupled to ultra-high resolution mass spectrometry (UHPLC-Orbitrap(®) MS). The efficiency and efficacy of extraction methods were evaluated and compared in number of extracted mycotoxins and obtained recoveries. From the one point of view, QuEChERS procedure was fast and easy, as well as it was able to successfully extra…
Quantitative and qualitative control of antineoplastic preparations: Gravimetry versus HPLC.
2019
This article compares gravimetry vs. high-performance liquid chromatography (HPLC) as quality control (QC) methods for paclitaxel, docetaxel and oxaliplatin preparations. We aimed at assessing the preparation method reliability in our hospital, evaluating compounding accuracy and estimating the influence of personnel training and standardized homogenization on compounding accuracy. Agreement, correlation, concordance, accuracy and precision between methods were evaluated for each drug. Conforming preparation percentages (CPs) at different tolerance limits (TLs) and compounding accuracy were calculated for each method and drug. Compounding accuracy was compared before and after personnel tra…
Determination of five pesticide residues in oranges by matrix solid-phase dispersion and liquid chromatography to estimate daily intake of consumers.
2001
Abstract Residues of benzoylphenylurea insecticides (diflubenzuron, hexaflumuron, and flufenuxuron), carboxamide acaricides (hexythiazox), and carbamate insecticides (benfuracarb) were determined in 150 orange fruit samples from September 1998 to June 1999, to estimate exposure of the Valencian population to oranges contaminated with these newly developed pesticides. The method for monitoring these residues is based on matrix solid-phase dispersion and liquid chromatography with UV or atmospheric pressure chemical ionization/mass spectrometry (APCI/MS) detection. Orange samples representing 11 varieties were collected from an agricultural cooperative and examined for the 5 pesticides. In 74…
Matrix solid-phase dispersion microextraction and determination by high-performance liquid chromatography with UV detection of pesticide residues in …
1999
A multiresidue method based on matrix solid-phase dispersion (MSPD) microextraction was studied to determine the carbamate, benfuracarb, and urea insecticides, diflubenzuron, flufenoxuron hexaflumuron and hexythiazox, used in control of citrus pests. Optimisation of different parameters, such as the type of solid support for matrix dispersion, elution solvents and the clean-up step were carried out. The method used 0.5 g of orange sample, C8 bonded silica as MSPD sorbent and dichloromethane as eluting solvent. Recoveries, at spiked concentrations below the maximum residue levels established by Spanish Government, were between 74 and 84% with relative standard deviations ranging from 2 to 4%…
Complementary mobile-phase optimisation for resolution enhancement in high-performance liquid chromatography.
2000
An optimisation methodology in high-performance liquid chromatography (HPLC) is presented for the selection of two or more mobile phases having an optimal complementary resolution. The complementary mobile phases (CMPs) are selected in such a way that each one resolves optimally only some compounds in the mixture, while the remainder, resolved by the other mobile phase(s), can overlap among them. The methodology is based on the computation of a peak purity measurement for each solute, using an asymmetrical peak model for peak simulation. Two global resolution criteria (product of elementary resolutions and worst elementary resolution) and two methods for solving the problem (a systematic ex…
Carotenoids and Color of Fruit Juice and Milk Beverage Mixtures
2007
Seventeen commercially available, "ready to drink" fortified beverages consisting of mixtures of fruit juices and milk were analyzed to evaluate their carotenoid profile (including their Z/E stereoisomers) and color during their commercial shelf life. Lightness (L*) was found to be correlated with the content of milk in the mixtures (r= 0.649) whereas red-yellow colors were correlated with the contents of alpha-carotene, beta-cryptoxanthin, and beta-carotene supplied by the fruit. The beverages stored under refrigeration (4 +/- 2 degrees C) showed higher luminosity (L*) and higher saturation of color (C*) and yellowness (b*). Differences (P < 0.05) in the levels of carotenoids were found am…
Fit-for-purpose chromatographic method for the determination of amikacin in human plasma for the dosage control of patients
2015
In this paper, a simple, rapid and sensitive method based on liquid chromatography with fluorimetric detection (HPLC-FLD) for the determination of amikacin (AMK) in human plasma is developed. Determination is performed by pre-column derivatization of AMK with ortho-phtalaldehyde (OPA) in presence of N-acetyl-L-cysteine (NAC) at pH 9.5 for 5 min at 80 °C. In our knowledge, this is the first time that NAC has been used in AMK derivatization. Derivatization conditions (pH, AMK/OPA/NAC molar ratios, temperature and reaction time) are optimized to obtain a single and stable, at room temperature, derivative. Separation of the derivative is achieved on a reversed phase LC column (Kromasil C18, 5 μ…
Pressurized liquid extraction combined with capillary electrophoresis–mass spectrometry as an improved methodology for the determination of sulfonami…
2007
A new analytical method, based on capillary electrophoresis and tandem mass spectrometry (CE-MS2), is proposed and validated for the identification and simultaneous quantification of 12 sulfonamides (SAs) in pork meat. The studied SAs include sulfathiazole, sulfadiazine, sulfamethoxypyridazine, sulfaguanidine, sulfanilamide, sulfadimethoxyne, sulfapyridine, sulfachloropyridazine, sulfisoxazole, sulfasalazine, sulfabenzamide and sulfadimidine. Different parameters (i.e. separation buffer, sheath liquid, electrospray conditions) were optimized to obtain an adequate CE separation and high MS sensitivity. MS2 experiments using an ion trap as analyzer, operating in the selected reaction monitori…
Absence Ochratoxin A in soy sauce
2004
A method is described for the determination of ochratoxin A (OTA) in soy sauce using phosphate-buffered saline (PBS) extraction, an immunoaffinity clean-up, a liquid chromatographic determination with fluorescence detection (LC-FD) and confirmation with LC-FD after methylation of OTA. Recoveries of OTA spiked to soy sauce samples at 0.25 ng/ml level were 90% with relative standard deviations of 4%. The limit of detection was 0.01 ng/ml for OTA using the proposed method. Furthermore, the proposed method was applied to 60 soy sauce samples from China and Japan and none of them were found to contain OTA.