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High Recovery (high + recovery)
Selected AbstractsMultiresidue analysis of 47 pesticides in cooked wheat flour and polished rice by liquid chromatography with tandem mass spectrometry ,BIOMEDICAL CHROMATOGRAPHY, Issue 4 2009Sung Jung Lee Abstract Liquid chromatography in conjunction with tandem mass spectrometry was used to directly quantify of 47 pesticide residues from cooked wheat flour and polished rice, which are the most widely consumed cereals in the Republic of Korea. The sample clean-up was carried out according to the method established by the Korea Food and Drug Administration. The mobile phase for liquid chromatograpy separation consisted of water and 5 mm methanolic ammonium formate. Tandem mass spectroscopy experiments were performed in electrospray ionization positive mode and the multiple reaction monitoring mode. The matrix effects estimated for the 47 pesticides had a mean value of 99% and ranged from 45 to 147%. High recoveries (70,140%) and relative standard deviations (,20%) were achieved for most of the pesticides tested. The method used in this study allowed for rapid quantification and identification of low levels of pesticides in cooked wheat flour and polished rice samples. Of the screened pesticide residues, only tricyclazole and fenobucarb were found in polished rice samples. However, no samples contained residues above the MRL established by the Korea Food and Drug Administration. Copyright © 2008 John Wiley & Sons, Ltd. [source] Enrichment of peptides from plasma for peptidome analysis using multiwalled carbon nanotubesJOURNAL OF SEPARATION SCIENCE, JSS, Issue 6 2007Xin Li Abstract Human plasma contains a complex matrix of proteolytically derived peptides (plasma peptidome) that may provide a correlate of biological events occurring in the entire organism. Analyzing these peptides from a small amount of serum/plasma is difficult due to the complexity of the sample and the low levels of these peptides. Here, we describe a novel peptidome analysis approach using multiwalled carbon nanotubes (MWCNTs) as an alternative adsorbent to capture endogenous peptides from human plasma. Harvested peptides were analyzed by using liquid chromatography-mass spectrometry as a means of detecting and assessing the adsorbed molecules. The improved sensitivity and resolution obtained by using liquid chromatography-mass spectrometry allowed detection of 2521 peptide features (m/z 300,1800 range) in about 50 ,L of plasma. 374 unique peptides were identified with high confidence by two-dimensional liquid chromatography system coupled to a nano-spray ionization linear ion trap-mass spectrometer. High recovery of BSA digest peptides enriched with MWCNTs, in both standard buffer and high abundance protein solution, was observed. Comparative studies showed that MWCNTs were superior to C18 and C8 for the capture of the smaller peptides. This approach could hold promise of routine plasma peptidome analysis. [source] Equilibrium theory analysis of dual reflux PSA for separation of a binary mixtureAICHE JOURNAL, Issue 10 2004Armin D. Ebner A dual reflux (DR) PSA cycle that combines the features of a conventional (stripping reflux) PSA cycle with those of a new enriching reflux PSA cycle is analyzed to show its potential for separating gas mixtures. On the basis of isothermal equilibrium theory applied to linear isotherms, the ultimate separation is carried out where the binary feed is separated into two pure components with 100% recovery of each component. This very idealized analysis reveals that such a separation is possible over a wide range of conditions, even with pressure ratios as low as 1.1. This analysis also reveals that low throughputs and high heavy component recycle ratios are inherently associated with DR PSA cycles, both of which may be detrimental to the process economics. High throughputs and low heavy product recycle ratios are indeed achievable, but only when using low pressure ratios and less selective adsorbents, both counterintuitive results that make sense when considering the perfect separation is always being achieved. Although these trends may not carry over to actual practice, because the model developed here is overly simplified and invalid under certain conditions, this analysis shows that it may indeed be entirely feasible to separate a binary gas mixture into two relatively pure components with very high recoveries using a DR PSA cycle operating with a very low pressure ratio and, hence, expenditure of energy. © 2004 American Institute of Chemical Engineers AIChE J, 50: 2418,2429, 2004 [source] Performance of electrospun nanofibers for SPE of drugs from aqueous solutionsJOURNAL OF SEPARATION SCIENCE, JSS, Issue 18 2008Xue-jun Kang Abstract A novel extraction technique was reported. The solid phase material, nanofiber, was prepared by electrospinning using polystyrene. Twenty different drugs (10 ,g/L in water) were extracted using 1 mg of nanofibers within 5 min. The analytes can be desorpted from the fibers with 50 ,L of the methanol and then monitored by LC coupled to a UV detector. Packed-fiber SPE (PFSPE) provide high recoveries (>50%) for some relatively non-polar drugs (log P >1.5) (n -octanol-to-water partition ratio), and relatively low recoveries (9.9,39.8%) for the drugs within the log P window below 1. Experimental optimization of the technique has been carried out using seven representative drugs, edaravone, cinchonine, quinine, voriconazole, chlordiazepoxide, verapamil, and rutonding. Except for edaravone, the maximum yields of seven drugs (0.2 ,g/L) from water samples were approximately 100%, and were 33.7,88.2% from human plasma. The advantageous aspect of the technique encompasses high throughput, high sensitivity, simplicity, low cost, and green chemistry. [source] Quantification of polyphenols with potential antioxidant properties in wines using reverse phase HPLCJOURNAL OF SEPARATION SCIENCE, JSS, Issue 12 2008Neuza Paixão Abstract A RP-HPLC method with photodiode array detection (DAD) was developed to separate, identify and quantify simultaneously the most representative phenolic compounds present in Madeira and Canary Islands wines. The optimized chromatographic method was carefully validated in terms of linearity, precision, accuracy and sensitivity. A high repeatability and a good stability of phenolics retention times (< 3%) were obtained, as well as relative peak area. Also high recoveries were achieved, over 80.3%. Polyphenols calibration curves showed a good linearity (r2 >0.994) within test ranges. Detection limits ranged between 0.03 and 11.5 ,g/mL for the different polyphenols. A good repeatability was obtained, with intra-day variations less than 7.9%. The described method was successfully applied to quantify several polyphenols in 26 samples of different kinds of wine (red, rosé and white wines) from Madeira and Canary Islands. Gallic acid was by far the most predominant acid. It represents more than 65% of all phenolics, followed by p -coumaric and caffeic acids. The major flavonoid found in Madeira wines was trans -resveratrol. In some wines, (,)-epicatechin was also found in highest amount. Canary wines were shown to be rich in gallic, caffeic and p -coumaric acids and quercetin. [source] Contents of hypericin and pseudohypericin in five commercial products of St John's wort (Hypericum perforatum)JOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE, Issue 5 2004Zhao-Jun Wang Abstract Hypericin and pseudohypericin are the two major dianthrones of St John's wort (SJW, Hypericum perforatum) that are reported to have antidepressant and antiviral effects. In this study we used methanol extracts of five commercial SJW products to determine the two congeners using a modified reverse phase HPLC method with gradient elution. One SJW product is specified by the manufacturer to contain 340 µg hypericin per tablet (170 mg extract), while the other four products are specified to contain 900 µg hypericin per tablet (300 mg); none of the products is claimed to contain pseudohypericin. Our results showed that the actual contents of hypericin in these products ranged from 1.7 to 38.5% of the claimed amounts. However, the amounts of pseudohypericin were in general much higher than those of hypericin. When hypericin and pseudohypericin were combined as total hypericin, the four products that supposedly contain 900 µg per tablet were found to contain 26, 484, 587 and 615 µg total hypericin per tablet, or 2.9, 53.8, 65.2 and 68.3% of the claimed hypericin contents respectively. The product which supposedly contains 340 µg hypericin per tablet was found to contain 388 µg total hypericin per tablet, or 114% of the claimed hypericin content. The relatively low hypericin contents measured in these products are not a result of losses during extraction, because the two congeners had high recoveries (93.7 and 94.3% for hypericin and pseudohypericin respectively) when added before methanolic extraction to an SJW product with known amounts of the two congeners. Thus our results show that the commercial SJW products vary greatly in their amounts of total hypericin and that pseudohypericin, rather than hypericin, is the major hypericin in these products. Copyright © 2004 Society of Chemical Industry [source] Scaleable purification process for gene therapy retroviral vectorsTHE JOURNAL OF GENE MEDICINE, Issue 4 2007Teresa Rodrigues Abstract Background Retroviral vectors (RVs) constitute one of the preferred gene therapy tools against inherited and acquired diseases. Development of scaleable downstream processes allowing purification under mild conditions and yielding viral preparations with high titer, potency and purity is critical for the success of clinical trials and subsequent clinical use of this technology. Methods A purification process for murine leukaemia virus (MLV)-derived vector supernatants was developed based on membrane separation and anion-exchange chromatography (AEXc). Initial clarification of the vector stocks was performed using 0.45 µm membranes followed by concentration with 500 kDa molecular weight cut-off (MWCO) membranes; further purification was performed by AEXc using a tentacle matrix bearing DEAE functional ligands. Finally, concentration/diafiltration was performed by 500 kDa MWCO membranes. To validate final product quality the process was scaled up 16-fold. Results Optimization of microfiltration membrane pore size and ultrafiltration transmembrane pressure allowed the recovery of nearly 100% infectious particles. Further purification of the RVs by AEXc resulted in high removal of protein contaminants while maintaining high recoveries of infectious vectors (77 ± 11%). Up-scaling of the process resulted in high titer vector preparations, 3.2 × 108 infectious particles (IP)/ml (85-fold concentration), with an overall recovery reaching 26%. The process yielded vectors with transduction efficiencies higher than the starting material and more than 99% pure, relative to protein contamination. Conclusions The combination of membrane separation and AEXc processes results in a feasible and scaleable purification strategy for MLV-derived vectors, allowing the removal of inhibitory contaminants thus yielding pure vectors with increased transduction efficiencies. Copyright © 2007 John Wiley & Sons, Ltd. [source] Equilibrium theory analysis of rectifying PSA for heavy component productionAICHE JOURNAL, Issue 8 2002Armin D. Ebner An isothermal equilibrium theory analysis, based on linear isotherms and a binary feed stream, was carried out to evaluate the feasibility of a rectifying PSA process for producing a pure heavy component at high recovery. Analytic expressions were derived to describe the performance of this process at the periodic state. The performance was also analyzed in terms of the different concentration and velocity profiles exhibited during various cycle steps that included the analysis of complex shock and simple wave interactions. Based on a parametric study, periodic behavior was established for a wide range of process conditions; and a design study with the PCB activated carbon,H2,CH4 system at 25°C further demonstrated the feasibility of a rectifying PSA cycle for producing a 100% CH4 stream from a dilute feed stream (y = 0.01) with a respectable recovery (80%), and reasonable process conditions. It also demonstrated the potential usefulness of an actual rectifying PSA process for bulk gas separation and purification. [source] Use of Single-Walled Carbon Nanotubes as Reinforcing Fillers in UV-Curable Epoxy SystemsMACROMOLECULAR MATERIALS & ENGINEERING, Issue 8 2008Marco Sangermano Abstract CNT were dispersed in an epoxy matrix and cured by means of UV light. An increase on elastic modulus and Tg values was measured by DMTA analysis and attributed to the constraint effect of CNT on polymer chain mobility. Excellent scratch resistant coatings characterized by high critical load, small cracks and high recovery were obtained in the presence of a very low CNT content (0.025 wt.-%). TEM analysis showed some isolated CNT and some cluster agglomerations of size of about 250 nm. It was shown that it was possible to decrease the surface resistivity of the cured samples by three orders of magnitude in the presence of 0.1 wt.-% of SWCNT content. [source] Rapid determination of short-chain fatty acids in colonic contents and faeces of humans and rats by acidified water-extraction and direct-injection gas chromatographyBIOMEDICAL CHROMATOGRAPHY, Issue 8 2006Guohua Zhao Abstract Short-chain fatty acids (SCFAs) have attracted much attention recently because of their positive physiological effects. In this work, a rapid and reliable gas chromatographic method for determination of eight SCFAs, in colonic and faecal samples from rats and humans has been developed and validated. The methodology involves extraction of the SCFAs in water before a direct injection procedure on a FFAP capillary column. A stock standard solution containing acetic acid, propionic acid, n -butyric acid, i -butyric acid, n -valeric acid, i -valeric acid, n -caproic acid and n -heptanoic acid was prepared and used. A high line-arity (r2 > 0.9990), low quantification limit (2.38,30.14 µm) and high recovery for most acids were obtained. Acidification of faecal samples was found to be crucial for quantitative determination of the SCFAs, and adjustment of pH to 2,3 was regarded as necessary. Glass wool inserted in the glass liner of the injection port proved effective in preventing the contamination of the column by non-volatiles, and 12% formic acid reduced the ghost peak that appeared gradually after several injections. After validation, the methodology was applied on two faecal samples from rats fed diets containing different amount of dietary fibre and one faecal sample from human fed a normal diet to test the accuracy of the developed method. Copyright © 2005 John Wiley & Sons, Ltd. [source] Mechanistic study of membrane concentration and recovery of Listeria monocytogenesBIOTECHNOLOGY & BIOENGINEERING, Issue 3 2005Wan-Tzu Chen Abstract Detection of the foodborne pathogen Listeria monocytogenes requires that food samples be processed to remove proteins and lipids, concentrate microorganisms to a detectable concentration, and recover the concentrated cells in a small volume compatible with micron-scale biochips. Mechanistic considerations addressed in this research include the roles of membrane structure, pore size, and detergents in maximizing recovery of cells from a complex biological fluid. The fluid in this case was a food sample (hotdog extract) inoculated with L. monocytogenes. This study showed how membrane filtration using a syringe filter is able to concentrate L. monocytogenes by 95× with up to 95% recovery of living microorganisms by concentrating 50 mL of food sample into a volume of 500 ,L. Tween 20 was added to the sample to prevent irreversible adsorption of the microorganism to the membrane and thereby help to ensure high recovery. Comparison of polycarbonate, mixed cellulose, nylon, and PVDF membranes with 0.2 to 0.45 ,m pores showed the 0.2 ,m polycarbonate membrane with straight through, mono-radial pores gives the highest recovery of living microorganisms. The mixed cellulose, nylon, and PVDF membranes have a fibrous structure whose characteristic openings are much larger than their effective pore size cut-offs of 0.22 or 0.45 ,m. We define conditions for rapid membrane-based cell concentration and recovery that has the potential to supplant enrichment steps that require a day or more. This approach has the added benefit of facilitating examination of a large amount of fluid volume by reducing its volume to a range that is compatible with the microliter scales of biochip or other biosensor detection systems. © 2004 Wiley Periodicals, Inc. [source] Application of a PEG/salt aqueous two-phase partition system for the recovery of monoclonal antibodies from unclarified transgenic tobacco extractBIOTECHNOLOGY JOURNAL, Issue 9 2009Dimitris Platis Abstract Aqueous two-phase partition systems (ATPS) have been widely used for the separation of a large variety of biomolecules. In the present report, the application of a polyethylene glycol/phosphate (PEG/phosphate) ATPS for the separation of anti-HIV monoclonal antibodies 2G12 (mAb 2G12) and 4E10 (mAb 4E10) from unclarified transgenic tobacco crude extract was investigated. Optimal conditions that favor opposite phase partitioning of plant debris/mAb as well as high recovery and purification were found to be 13.1% w/w (PEG 1500), 12.5% w/w (phosphate) at pH 5 with a phase ratio of 1.3 and 8.25% w/w unclarified tobacco extract load. Under these conditions, mAb 2G12 and mAb 4E10 were partitioned at the bottom phosphate phase with 85 and 84% yield and 2.4- and 2.1-fold purification, respectively. The proposed ATPS was successfully integrated in an affinity-based purification protocol, using Protein A, yielding antibodies of high purity and yield. In this study, ATPS was shown to be suitable for initial protein recovery and partial purification of mAb from unclarified transgenic tobacco crude extract. [source] Optimization of Isopropanol and Ammonium Sulfate Precipitation Steps in the Purification of Plasmid DNABIOTECHNOLOGY PROGRESS, Issue 4 2006S. S. Freitas Large-scale processes used to manufacture grams of plasmid DNA (pDNA) should be cGMP compliant, economically feasible, and environmentally friendly. Alcohol and salt precipitation techniques are frequently used in plasmid DNA (pDNA) downstream processing, as concentration and prepurification steps, respectively. This work describes a study of a standard 2-propanol (IsopOH; 0.7 v/v) and ammonium sulfate (AS; 2.5 M) precipitation. When inserted in a full process, this tandem precipitation scheme represents a high economic and environmental impact due to the large amounts of the two precipitant agents and their environmental relevance. Thus, major goals of the study were the minimization of precipitants and the selection of the best operating conditions for high pDNA recovery and purity. The pDNA concentration in the starting Escherichia coli alkaline lysate strongly affected the efficiency of IsopOH precipitation as a concentration step. The results showed that although an IsopOH concentration of at least 0.6 (v/v) was required to maximize recovery when using lysates with less than 80 ,g pDNA/mL, concentrations as low as 0.4 v/v could be used with more concentrated lysates (170 ,g pDNA/mL). Following resuspension of pDNA pellets generated by 0.6 v/v IsopOH, precipitation at 4 °C with 2.4 M AS consistently resulted in recoveries higher than 80% and in removal of more than 90% of the impurities (essentially RNA). An experimental design further indicated that AS concentrations could be reduced down to 2.0 M, resulting in an acceptable purity (21,23%) without compromising recovery (84,86%). Plasmid recovery and purity after the sequential IsopOH/AS precipitation could be further improved by increasing the concentration factor (CF) upon IsopOH precipitation from 2 up to 25. Under these conditions, IsopOH and AS concentrations of 0.60 v/v and 1.6 M resulted in high recovery (,100%) and purity (32%). In conclusion, it is possible to reduce substantially the mass of precipitation agents used without affecting recovery, if a small concession is made regarding purity. This directly translates into an improvement of the process economics and in a reduction of the environmental impact of the process. [source] | |||||||||||||