Home About us Contact
|
Home About us Contact | ||
|
|
||
Excellent Recovery (excellent + recovery)
Selected AbstractsApplication of FAIMS to anabolic androgenic steroids in sport drug testingDRUG TESTING AND ANALYSIS, Issue 11-12 2009Sven Guddat Abstract Mass spectrometric identification of anabolic androgenic steroids challenges standard doping-control methods. To reveal a doping offence the presence of prohibited anabolic androgenic steroids at trace levels in the picogram-per-millilitre range must be confirmed as reliable. Human urine samples containing epitrenbolone, metandienone metabolite (17, -hydroxymethyl-17,-methyl-18-norandrost-1,4,13-trien-3-one), stanozolol, 16,-hydroxystanozolol and 4,-hydroxystanozolol were analysed using LC-FAIMS-MS/MS. These substances are prohibited in sport according to World Anti-Doping Agency (WADA) regulations. Glucuronides were hydrolysed and prepared by liquid-liquid extraction. Excellent recovery and precision were obtained for all compounds. Linear calibration results for epitrenbolone and metandienone metabolite were obtained and concentration information could be determined in the ranges of reliable response between 750,1200 and 100,600 pg/mL, respectively. Limits of detection were estimated at 25 pg/mL (stanozolol), 50 pg/mL (metandienone metabolite, 16,-hydroxystanozolol), 100 pg/mL (4,-hydroxystanozolol) and 500 pg/mL (epitrenbolone). The assay was applied to doping-control samples. For all analytes, LC-FAIMS-MS/MS resulted in excellent interference removal, which effectively extends the post-dose detection time. Copyright © 2009 John Wiley & Sons, Ltd. [source] Gold-Nanocluster-Based Fluorescent Sensors for Highly Sensitive and Selective Detection of Cyanide in WaterADVANCED FUNCTIONAL MATERIALS, Issue 6 2010Yanlan Liu Abstract A novel, gold-nanocluster-based fluorescent sensor for cyanide in aqueous solution, which is based on the cyanide etching-induced fluorescence quenching of gold nanoclusters, is reported. In addition to offering high selectivity due to the unique Elsner reaction between cyanide and the gold atoms of gold nanoclusters, this facile, environmentally friendly and cost-effective method provides high sensitivity. With this sensor, the lowest concentration to quantify cyanide ions could be down to 200,×,10,9,M, which is approximately 14 times lower than the maximum level (2.7,×,10,6,M) of cyanide in drinking water permitted by the World Health Organization (WHO). Furthermore, several real water samples spiked with cyanide, including local groundwater, tap water, pond water, and lake water, are analyzed using the sensing system, and experimental results show that this fluorescent sensor exhibits excellent recoveries (over 93%). This gold-nanocluster-based fluorescent sensor could find applications in highly sensitive and selective detection of cyanide in food, soil, water, and biological samples. [source] Synthesis of cyclodextrin-based polymers and their use as debittering agentsJOURNAL OF APPLIED POLYMER SCIENCE, Issue 4 2008Arianna Binello Abstract Cyclodextrins (CDs) and their derivatives are used to suppress unpleasant tastes and odors or to achieve a controlled release of certain food constituents. This article describes the synthesis by nonconventional methods of (1) crosslinked, insoluble CD polymers and (2) water-soluble, CD-grafted carboxymethylchitosan and carboxymethylcellulose. The CD polymers were obtained by the reaction of ,-CD with one of the following crosslinking agents: epichlorohydrin, diphenyl carbonate, or hexamethylene diisocyanate. Their preparations were usually carried out under high-intensity ultrasound, which resulted in much shorter reaction times and narrower distributions of particle size (as determined by scanning electron microscopy measurements). A novel, insoluble CD polymer was obtained by reticulation under microwaves of propargyl-,-CD with 1,3-bis(azidomethyl)benzene through Huisgen 1,3-dipolar cycloaddition. Short columns packed with the insoluble polymers were found to efficiently sequester naringin from aqueous solutions; successively, they could be easily regenerated by a counter-current ethanol wash that also achieved an excellent recovery of the flavonoid. Differential scanning calorimetry thermograms showed that the crosslinked CD polymers formed inclusion complexes with naringin. The soluble polymers also interacted with bitter flavonoids of citrus fruits (naringin and limonin), as shown by the results of sensorial panel tests, in which they behaved as bitter-masking agents. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008 [source] Muscle preservation using an implantable electrical system after nerve injury and repairMICROSURGERY, Issue 6 2001F.R.C.S.(C), Stephen C. Nicolaidis M.D. The value of continuous electrical stimulation of denervated muscles after nerve injury and repair has been clearly shown in a series of laboratory experiments in three animal models. This experimental background, which showed improved muscle preservation and better functional results, evolved into a clinical study that included 15 patients with peripheral nerve injuries in the upper extremities, 3 patients with brachial plexus injuries, and three patients with facial nerve paralysis. Improved functional results were obtained using this implantable system, which were similar to those achieved with the animal experiments. All patients had muscle stimulation for extended periods ranging from 127 to 346 days. Analysis of the results showed satisfactory nerve regeneration on clinical examination and with electromyographic studies. Functional muscle analysis varied somewhat from patient to patient, but every patient had a satisfactory to excellent recovery. The results from this study have clearly shown the benefits of continuous muscle stimulation using an implantable electrical system after nerve injury and repair expansion of the project to a larger patient cohort is indicated. © 2001 Wiley-Liss, Inc. MICROSURGERY 21:241,247 2001 [source] Quantitative analyses of indoloquinazoline alkaloids in Fructus Evodiae by high-performance liquid chromatography with atmospheric pressure chemical ionization tandem mass spectrometryRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 20 2006Yan Zhou Fructus Evodiae (Wuzhuyu), the fruits of Evodia rutaecarpa and related varieties, is widely used in traditional Chinese medicine. The bioactive constituents include the indoloquinazoline alkaloids rutaecarpine, evodiamine and dehydroevodiamine. A new assay based on high-performance liquid chromatography/atmospheric pressure chemical ionization tandem mass spectrometry (HPLC/UV/APCI-MS/MS) was developed for the measurement of the indoloquinazoline alkaloids in commercial Fructus Evodiae products. Initially, the MS/MS fragmentation pathways of indoloquinazoline alkaloids were investigated to identify fragment ions that might be useful for the sensitive and selective detection of trace indoloquinazoline alkaloids during LC/MS/MS. Then, quantitative MS analysis of five indoloquinazoline alkaloids in 12 commercial Fructus Evodiae products from different geographical sources was performed. Analyte recovery was in the range of 97.5,105.3% for all with relative standard deviations (RSDs) below 6%, the intra-assay and inter-assay RSDs were less than 7%, and good linear relationships were shown with correlation coefficients for the analytes exceeding 0.999. Therefore, this LC/MS/MS assay facilitated the rapid quantitative analysis of rutaecarpine, evodiamine, evodiamide, 14-formyldihydrorutaecarpine and dehydroevodiamine in 12 commercial Fructus Evodiae products with excellent recovery, repeatability, accuracy and sensitivity. This method is simple and specific and can be used for identification and quality control of this traditional Chinese remedy. Copyright © 2006 John Wiley & Sons, Ltd. [source] Defining the Canonical Form of T-Cell-Mediated Rejection in Human Kidney TransplantsAMERICAN JOURNAL OF TRANSPLANTATION, Issue 4 2010K. S. Famulski Banff defines T-cell-mediated rejection (TCMR) using nonspecific lesions and arbitrary cutoffs, with no external gold standard. We reexamined features of TCMR using exclusively molecular definition independent of histopathology. The definition was derived from mouse kidney transplants with fully developed TCMR, and is based on high expression of transcripts reflecting IFNG effects and alternative macrophage activation. In 234 human kidney transplant biopsies for cause phenotyped by microarrays, we identified 26 biopsies meeting these criteria. After excluding three biopsies with unrelated diseases, all 23 biopsies had typical Banff lesions of TCMR (inflammation, tubulitis), with v lesions in 10/23. Banff histopathology diagnosed 18 as TCMR, 1 as mixed and 4 as borderline. Despite marked changes in transcriptome indicating tissue injury and dedifferentiation, all kidneys with molecularly defined TCMR, even with v lesions or late rejection, demonstrated excellent recovery of function at 6 months with no graft loss (mean follow-up 2.5 years). Thus TCMR defined exclusively by molecules manifests TCMR,related lesions and function impairment, but good recovery and survival, even with late rejection or arteritis. This combination of pathologic, clinical and molecular features constitutes the typical or canonical T-cell-mediated rejection. [source] Stable isotope dilution analysis of N-acetylaspartic acid in urine by liquid chromatography electrospray ionization tandem mass spectrometryBIOMEDICAL CHROMATOGRAPHY, Issue 9 2007Osama Y. Al-Dirbashi Abstract N -acetylaspartic acid (NAA) is a specific urinary marker for Canavan disease, an autosomal recessive leukodystrophy. We developed a ,dilute and shoot' stable isotope dilution liquid chromatography tandem mass spectrometry (LC-MS/MS) method for determination of NAA in urine. Deuterated internal standard d3 -NAA was added to untreated urine and the mixture was injected into the LC-MS/MS system operated in the negative ion mode. Chromatography was carried out on a C8 minibore column using 50% acetonitrile solution containing 0.05% formic acid at a flow rate of 0.25 mL/min. The retention time was 1.6 min and the turnaround time was 2.2 min. NAA and d3 -NAA were analyzed in multiple reaction monitoring mode. Calibrators and quality control samples were prepared in pooled control urine. The assay was linear up to 2000 µmol/L with limit of quantification at 1 µmol/L (S/N = 12). Interassay and intraassay coefficients of variation were less than 7% and recovery at three different concentrations was 98.9,102.5%. The LC-MS/MS method for NAA as described involves no extraction and no derivatization, showed no interference and gave excellent recovery with low variability and short analytical time. The method was successfully applied for the retrospective analysis of urine from 21 Canavan disease cases. Copyright © 2007 John Wiley & Sons, Ltd. [source] Purification and Concentration of Alkaline Phosphatase by Selective Permeabilization of Escherichia coli Using Reverse Micellar SolutionsBIOTECHNOLOGY PROGRESS, Issue 6 2003Ritu Bansal-Mutalik Recovery of alkaline phosphatase (AP) from the periplasm of Escherichia coli using reverse micellar solutions (RMSs) of sodium dioctyl sulfosuccinate (AOT) in aliphatic hydrocarbons has been attempted. A variety of surface-active agents, solvents, and reverse micellar conditions were screened, and an excellent recovery of the enzyme in a concentrated form, with a high purification factor, was obtained in a single-step process. The permeabilization process strongly depended on the water content of the RMS as well as on the amount of water coating the microbial cell surface. The product was almost free from nucleic acids. In addition, because of the low affinity of AOT and the organic solvent for the aqueous phase, contamination by the permeabilizing agents would also be negligible. [source] | ||||||||||||||||