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Development of on-line monolith-based in-tube solid phase microextraction for the sensitive determination of triazoles in environmental waters.

In this work, a convenient and sensitive method for the determination of triazoles in environmental waters was developed by on-line combining in-tube solid phase microextraction (IT-SPME) and high performance liquid chromatography with diode array detector (HPLC-DAD). To extract triazoles effectively, poly (4-vinyl pyridine-co-ethylene dimethacrylate) monolith was in-situ fabricated and utilized as the extraction phase of IT-SPME. A series of key extraction parameters including desorption solvent, sample volume, adsorption and desorption flow rate, pH value and ionic strength in sample matrix were optimized thoroughly. Under the most favorable conditions (volume of sample, 6.0 mL; adsorption flow rate, 0.2 mL/min; desorption solvent, 80.0 µL mixture of ACN/water (70/30, v/v); desorption flow rate, 50.0 µL/min; sample pH value, 8.0; ionic strength did not be adjusted), the developed monolith-based IT-SPME could extract target analytes effectively and expected analytical merits were achieved. The limits of detection (S/N = 3) and limits of quantification (S/N = 10) were in the ranges of 0.014-0.031 µg/L and 0.11-0.074 µg/L, respectively. Satisfactory method reproducibility was obtained by intra-day and inter-day precisions, with relative standard deviations (RSDs) lower than 10%. The optimized IT-SPME-HPLC-DAD method was then applied to detect triadimenol, triazolone and hexaconazole in water samples including lake, river and sewage waters. The spiked recoveries were 78.9-106% and the RSDs were in the range of 0.2-7.2%. The results well evidence that the proposed method is convenient, accurate, sensitive, practical and environmentally friendly for the determination of triazoles in environmental waters.

1039 related Products with: Development of on-line monolith-based in-tube solid phase microextraction for the sensitive determination of triazoles in environmental waters.

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High-throughput determination of valproate in human samples by modified QuEChERS extraction and GC-MS/MS.

A new high-throughput method was developed for analysis of valproate in human plasma samples by QuEChERS extraction and gas chromatography-tandem mass spectrometry (GC-MS/MS). Plasma samples (0.2 ml) spiked with valproate and secobarbital-d (internal standard) were diluted with 1.3 ml of distilled water. Acetonitrile (1 ml) was added followed by 0.4 g MgSO and 0.1 g NaOAC. After a centrifugation step (2000 g for 10 min), 1 ml of the supernatant was transferred to a dispersive-solid phase extraction (dSPE) tube containing 150 mg MgSO and 50 mg C. This mixture was vortexed and centrifuged at 3000 g for 5 min, and then the upper layer was evaporated to dryness under a stream of nitrogen. The residue was dissolved in 40 μl ethyl acetate, and a 1-μl aliquot was injected into the GC-MS/MS. The GC separation of the compounds was achieved on a fused-silica capillary column Rxi-5Sil MS (30 m × 0.25 mm i.d.; 0.25-µm film thickness) and detected by MS/MS operating in electron ionization ion source mode. The regression equations showed excellent linearity (r > 0.9997) from 50 to 5000 ng/ml for plasma, with limit of detection of 10 ng/ml. The extraction efficiency of valproate for plasma ranged between 71.2%-103.5%. The coefficient of variation was <18.5%. The method was successfully applied to actual analyses of an autopsy case. This method can be useful for simple and reliable measurements of valproate in clinical and toxicological analyses; it can be integrated in screening and simultaneous determination methods for multiple drugs and poisons in the further studies.

1251 related Products with: High-throughput determination of valproate in human samples by modified QuEChERS extraction and GC-MS/MS.

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In-tube electro-membrane extraction with a sub-microliter organic solvent consumption as an efficient technique for synthetic food dyes determination in foodstuff samples.

A simple and efficient extraction technique with a sub-microliter organic solvent consumption termed as in-tube electro-membrane extraction (IEME) is introduced. This method is based upon the electro-kinetic migration of ionized compounds by the application of an electrical potential difference. For this purpose, a thin polypropylene (PP) sheet placed inside a tube acts as a support for the membrane solvent, and 30μL of an aqueous acceptor solution is separated by this solvent from 1.2mL of an aqueous donor solution. This method yielded high extraction recoveries (63-81%), and the consumption of the organic solvent used was only 0.5μL. By performing this method, the purification is high, and the utilization of the organic solvent, used as a mediator, is very simple and repeatable. The proposed method was evaluated by extraction of four synthetic food dyes (Amaranth, Ponceau 4R, Allura Red, and Carmoisine) as the model analytes. Optimization of variables affecting the method was carried out in order to achieve the best extraction efficiency. These variables were the type of membrane solvent, applied extraction voltage, extraction time, pH range, and concentration of salt added. Under the optimized conditions, IEME-HPLC-UV provided a good linearity in the range of 1.00-800ngmL(-1), low limits of detection (0.3-1ngmL(-1)), and good extraction repeatabilities (RSDs below 5.2%, n=5). It seems that this design is a proper one for the automation of the method. Also the consumption of the organic solvent in a sub-microliter scale, and its simplicity, high efficiency, and high purification can help one getting closer to the objectives of the green chemistry.

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New analytical spiral tube assembly for separation of proteins by counter-current chromatography.

A new spiral column assembly for analytical separation by counter-current chromatography is described. The column is made from a plastic spiral tube support which has 12 interwoven spiral grooves. The PTFE tubing of 1.6mm ID was first flattened by extruding through a narrow slit and inserted into the grooves to make 5 spiral layers with about 60ml capacity. The performance of the spiral column assembly was tested with separation of three stable protein samples including cytochrome C, myoglobin and lysozyme in a polymer phase system composed of polyethylene glycol 1000 and dibasic potassium phosphate each at 12.5% (w/w) in water. At 2ml/min, three protein samples were well resolved in 1h. The separation time may be further shortened by application of higher revolution speed and flow rate by improving the strength of the spiral tube support in the future.

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Prematurely born infants' response to resuscitation via an endotracheal tube or a face mask.

Prematurely born infants may be resuscitated in the labour suite via a face mask or an endotracheal tube.

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Analysis of amino acids in tobacco by derivatization and dispersive liquid-liquid microextraction based on solidification of floating organic droplet method.

A new one-step derivatization and microextraction technique was developed for determination of amino acids in tobacco samples. In the proposed method, amino acids were derivatized with isobutyl chloroformate (IBCF) in aqueous solution. The derivatives were extracted by dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO). Parameters affecting the extraction efficiency were investigated in detail. The optimum conditions were as follows: a mixture of 500μL acetone, containing 40μL 2-dodecanol, was rapidly injected by syringe into the 2mL water sample. After centrifugation, the 2-dodecanol droplets were floated at the top of the tube. Then, the tube was cooled in an ice bath. After 5min the solvent had solidified and was then transferred into a conical vial; it melted quickly at room temperature and it was injected into a gas chromatograph for analysis. Under the optimum conditions, the limits of detection were of the order of 0.12-2.82μg/mL. The calibration curves showed good linearity over the investigated concentration range between 0.5 and 200μg/mL with a coefficient of estimation (R(2))>0.9887 for GC-MS (SIM). The proposed method is an alternative approach to the quantification of amino acids in tobacco samples.

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Determination of zolpidem in human hair by micropulverized extraction based on the evaluation of relative extraction efficiency of seven psychoactive drugs from an incurred human hair specimen.

A micropulverization method for rapid extraction of psychoactive drugs from hair was developed. A hair sample (10mg) was micropulverized for 10min at 42Hz with 0.2mL of 45% (w/v) aqueous ammonium phosphate (pH 8.4). Liquid-liquid extraction was carried out in the same tube using acetonitrile, and the organic layer was removed and filtered. Conventional methods, including solid-liquid extraction with an ammonium phosphate solution or methanol, were also employed, and the relative extraction efficiencies of amitriptyline, nortriptyline, norfludiazepam, flunitrazepam, 7-aminoflunitrazepam, mianserin and zolpidem with these methods from an incurred human hair specimen were compared using liquid chromatography/tandem mass spectrometry. The highest extraction efficiencies for all the analytes were achieved using the method developed here, even though the extraction time (10min) was short. Overnight methanol extraction has frequently been used for hair analysis; however, the extraction efficiency was not sufficient for amines. The method was successfully applied to the quantification of zolpidem in human hair. The range of quantification was 1-25,000pg/mg, and interday accuracy and precision (n=5) at three concentrations were 1.8-8.8% and 3.3-8.1%, respectively. The developed method was applied to three actual (incurred) samples, for which the concentrations of zolpidem were determined to be 78.9-18,300 (pg/mg).

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Pipette tip solid-phase extraction and ultra-performance liquid chromatography/mass spectrometry based rapid analysis of picrosides from Picrorhiza scrophulariiflora.

Pipette tip solid-phase extraction (PT-SPE) is a technique popular in sample preparation of biological fluids and protein hydrolysates. In this study, we developed a microtechnic using a pipette tip packed with C18 as sorbent for extraction and purification of bioactive compounds, picroside-I, II and III, in crude herbal extracts from Picrorhiza scrophulariiflora (P. scrophulariiflora). Compared to conventional SPE, PT-SPE is fast, easy to operate, and the tools are very accessible (pipette tip and tube, without expensive SPE set-up). Moreover, it is also cost-effective because significant amount of sorbent and solvents can be saved. The eluate was analyzed by ultra-performance liquid chromatography and tandem mass spectrometry (UPLC-MS/MS). Afterwards, the method was fully validated and the results demonstrated that the PT-SPE-UPLC-MS/MS method is an excellent technique for analysis of the herbal medicine. Finally, this PT-SPE-UPLC-MS/MS strategy was successfully applied to analyze the crude extracts from P. scrophulariiflora samples within 10min (2min for PT-SPE and 8min for UPLC), 3.5mL solvents (including water, 0.3mL for PT-SPE and 3.2mL for UPLC), and 2mg C18 sorbent for each sample. We believe this method to be very practical and, in particular, to be suitable for widespread herbal medicine analysis.

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Proton pump inhibitor administration via nasogastric tube in pediatric practice: comparative analysis with protocol optimization.

Proton pump inhibitors (PPIs) are largely prescribed to children because their efficacy and tolerance are now well-established. One disadvantage resides in the absence of liquid form which causes problems for their administration in nasogastric tubes. Indeed, the absence of use recommendations involves many misuses responsible for inefficiency and/or tube obstruction. We tried to evaluate if PPIs can be administered through pediatric nasogastric tubes. We administered four PPIs (Omeprazole, esomeprazole, lansoprazole and lansoprazole orally disintegrating tablet) through nasogastric tubes. For each PPI a study plan was drawn up to assess the influence of different variables: the volume of water to dissolve or put in suspension the PPIs (2ml or 5ml), the volume of tube flush-through water post-PPI administration (2ml, 5ml or 10ml), the length (50cm or 125cm) and the diameter (6 or 8 French) of the polyurethane tubes. For each assay an analysis of each active ingredient at the tube outlet by UV spectrometry was carried out. All 6 F tubes were obstructed by PPIs. Through 8 F tubes, we observed a mean recovery of active ingredient of 86.2% for lansoprazole orally disintegrating tablet, 36.9% for esomeprazole but only 7.1% for lansoprazole and 3.9% for omeprazole. It is disadvised using omeprazole and lansoprazole through 8 F nasogastric tubes because no condition ensures the transit of an efficient concentration of active ingredient. For esomeprazole, the best conditions of administration were a water volume of 5ml and a rinse volume of 5ml but only a half of the microgranules administered were recovered. The most satisfactory results were obtained with lansoprazole orally disintegrating tablet. A 5ml volume of water diluent for suspension and a 10ml volume of flush-through water made it possible to deliver the full lansoprazole dose administered.

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Bosentan reduces oxidative burst in acid aspiration-induced lung injury in rats.

Acid aspiration induces lung injury by causing an intense inflammatory reaction. Neutrophils are attracted by various cytokines, such as TNFbeta, and release reactive oxygen species, which then cause acute lung injury. Endothelin antagonists, such as bosentan, have been found to possess anti-inflammatory properties.

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