0000000000004728
AUTHOR
Rafael L. Rodríguez
Analysis of thiabendazole and procymidone in fruits and vegetables by capillary electrophoresis–electrospray mass spectrometry
Abstract A capillary electrophoresis–mass spectrometry method for determining procymidone and thiabendazole in apples, grapes, oranges, pears, strawberries and tomatoes is described. Separation is achieved using a buffer of formic acid–ammonium formate at pH 3.5 with 2% of methanol. Fungicide residues present in the sample are preconcentrated by both solid-phase extraction and injection of large sample volumes into the capillary by a stacking technique, to obtain lower detection limits. Ionization is performed at atmospheric pressure in an electrospray type source and detection is carried out using positive ionization and selected ion monitoring modes. The quantitation limits are 0.005 and …
Capillary electrophoresis for the determination of pesticide residues
Capillary electrophoresis (CE) is becoming an advantageous tool for determining pesticide residues in environmental matrices because of its simplicity and high separation efficiency. However, inadequate limits of detection (LODs) and a lack of selective detectors limit the technique. The present review gives an overview of current developments in off-column and on-column approaches to trace enrichment in analysing real samples, and summarises the determination of pesticides residues by conventional CE as well as by the emerging techniques, such as CE-mass spectrometry (MS). The usefulness of these approaches in environmental applications is documented.
Off-line solid-phase microextraction and capillary electrophoresis mass spectrometry to determine acidic pesticides in fruits.
A method based on solid-phase microextraction (SPME) and capillary electrophoresis/mass spectrometry (CE/ MS) is described for determining simultaneously five acidic pesticides (o-phenylphenol, ioxynil, haloxyfop, acifluorfen, picloram) in fruits. The CE device is coupled to an electrospray interface by a commercial sheath-flow adapter. Emphasis is placed on fulfillment of the speed and sensitivity requirements. The best separation is achieved using 32 mM ammonium formate/acid formic buffer at pH 3.1, with a working voltage of 25 kV. The MS detection of the five pesticides was performed in negative ionization mode. Full-scan spectra with base peaks corresponding to [M-H]- were obtained exce…
Supplemental Perioperative Oxygen and the Risk of Surgical Wound Infection<SUBTITLE>A Randomized Controlled Trial</SUBTITLE>
ContextSupplemental perioperative oxygen has been variously reported to halve or double the risk of surgical wound infection.ObjectiveTo test the hypothesis that supplemental oxygen reduces infection risk in patients following colorectal surgery.Design, Setting, and PatientsA double-blind, randomized controlled trial of 300 patients aged 18 to 80 years who underwent elective colorectal surgery in 14 Spanish hospitals from March 1, 2003, to October 31, 2004. Wound infections were diagnosed by blinded investigators using Centers for Disease Control and Prevention criteria. Baseline patient characteristics, anesthetic treatment, and potential confounding factors were recorded.InterventionsPati…
Capillary zone electrophoresis for the determination of thiabendazole, prochloraz and procymidone in grapes
Capillary zone electrophoresis with UV detection was applied to the simultaneous determination of thiabendazole, prochloraz and procymidone in grapes. Electrolyte conditions such as pH, composition and concentration of the buffer, addition of organic solvent and working voltage were checked to obtain a high-performance separation of the three fungicides (by measurement of separation efficiency and resolution). The most critical parameter was the pH of the running buffer. The best separation was achieved in 4 mM phosphate solution at pH 3.5. The repeatability of the migration times, expressed as RSD, was <0.44%. The three peaks were completely resolved with a separation efficiency up to 100 …
Laboratory evidence for asymmetric accretion structure upon slanted matter impact in young stars
Aims. Investigating the process of matter accretion onto forming stars through scaled experiments in the laboratory is important in order to better understand star and planetary system formation and evolution. Such experiments can indeed complement observations by providing access to the processes with spatial and temporal resolution. A previous investigation revealed the existence of a two-component stream: a hot shell surrounding a cooler inner stream. The shell was formed by matter laterally ejected upon impact and refocused by the local magnetic field. That laboratory investigation was limited to normal incidence impacts. However, in young stellar objects, the complex structure of magne…
Determination of urea-derived pesticides in fruits and vegetables by solid-phase preconcentration and capillary electrophoresis
A multiresidue analytical method based on solid-phase extraction (SPE) enrichment combined with capillary electrophoresis (CE), using micellar electrokinetic capillary chromatography (MEKC), was developed to determine ten substituted urea pesticides in orange and tomato samples. Several factors such as pH, composition and concentration of the buffer, concentration of surfactant, addition of organic solvent, and working voltage were optimized to obtain the best compound separation in the shortest time. Separation can be achieved in 7 min using a micellar aqueous pH 9 buffer composed of 4 mM borate and 35 mM sodium dodecyl sulfate. After an SPE procedure, which provided a 10-fold enrichment, …
Toxicological Assessment of Recombinant Xylanase X22 in Wine
Toxicological evaluation of xylanase X(22) from Aspergillus nidulans expressed in a wine yeast strain was carried out. The safety of the X(22) intake was assessed by digestibility, bioinformatic, and mouse short-term repeated dosing studies, although X(22) shows resistance to proteolytic degradation in the gastrointestinal system, is a minority protein component (<0.5 10(-)(6) %) of the produced wine, and shows no significant amino acid sequence homology to any known food allergens. The 4-week oral toxicity study was performed in Swiss mice at a dose level of 0.01, 0.1, or 1 mg/kg/day (these dosages correlate to 8, 80, and 800 times, respectively, the enzyme amount contained in 250 mL of wi…
Analysis of post-harvest fungicides by micellar electrokinetic chromatography.
A method based on solid-phase extraction (SPE) and micellar electrokinetic chromatography (MEKC) was developed for the simultaneous determination of carbendazim, imazalil, methylthiophanate, O-phenylphenol, prochloraz, procimidone, thiabendazole and triadimefon residues in grape, lettuce, orange and tomato. Selectivity and resolution were studied changing the pH and the concentration of the buffer, the type and concentration of surfactant and the methanol content in the mobile phase. A buffer consisting of 4 mM borate with 75 mM sodium cholate (pH 9.2) gave the best results. The recoveries of the fungicides in spiked fruit and vegetable samples ranged from 30 to 105%, and the limits of dete…
INGENIERÍA GENÉTICA E INDUSTRIA AGROALIMENTARIA: VENTAJAS E INCONVENIENTES GENETIC ENGINEERING AND FOOD INDUSTRY: ADVANTAGES AND INCONVENIENCES EXEÑERÍA XENÉTICA E INDUSTRIA AGROALIMENTARIA: VENTAXAS EINCONVINTES
Abstract Resumen Resumo Nowadays biotechnology allows to perform accurate changes on the genetic material of organisms, being a very important tool in food industry. However just a few recombinant products can be found in the market, as a result of the social repulse against these kind of foods. According to the Community Normative, it is necessary to evaluate the safety for human being and environment security previous to introducing a recombinant food into the market. In this work, the recommended protocols for several organisms to attend this evaluation on a rational way are reviewed. These protocols are fundamentally based on the SAFEST elements (Safety Assessment of Food by Equivalence…
Effects of radiation in accretion regions of classical T Tauri stars
Models and observations indicate that the impact of matter accreting onto the surface of young stars produces regions at the base of accretion columns, in which optically thin and thick plasma components coexist. Thus an accurate description of these impacts requires to account for the effects of absorption and emission of radiation. We study the effects of radiation emerging from shock-heated plasma in impact regions on the structure of the pre-shock downfalling material. We investigate if a significant absorption of radiation occurs and if it leads to a pre-shock heating of the accreting gas. We developed a radiation hydrodynamics model describing an accretion column impacting onto the su…
Radiation Magnetohydrodynamic Models and Spectral Signatures of Plasma Flows Accreting onto Classical T Tauri Stars
CTTSs are young stars accreting mass from their circumstellar disks. The material falls into the star at free fall velocity and hits the stellar surface producing shocks, that heat the plasma at few million degrees. In the last twenty years the X-ray and UV observations of these systems have raised several questions. In particular, the observed X-ray luminosity is systematically below the value predicted by theoretical models, and the UV lines show complex profiles which cannot be easily interpreted with current accretion models based only on magnetohydrodynamical effects. To tackle these problems we modeled the structure and the dynamics of the plasma in the impact region using 3D magnetoh…
Liquid chromatographic–mass spectrometric determination of post-harvest fungicides in citrus fruits
Liquid chromatography (LC)-atmospheric pressure ionisation (API)-mass spectrometry (MS) has been used to determine residues of five fungicides in oranges with a minimum sample cleanup. Atmospheric pressure chemical ionisation (APCI) and electrospray (ES) were compared and both gave similar results in terms of sensitivity and structural information. The main ions were [M+H]+ for carbendazim, imazalil, thiophanate methyl and thiabendazole, and [M+H-C4H9NHCO]+ for benomyl. Samples were extracted with sodium sulphate and ethyl acetate. Although benomyl and thiophanate methyl were transformed through the extraction procedure to carbendazim, the method showed good precision (13%) and recovery (70…