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Ppb Level (ppb + level)
Selected AbstractsAnalysis of sub-ppb levels of Fe(II), Co(II), and Ni(II) by electrokinetic supercharging preconcentration, CZE separation, and in-capillary derivatizationELECTROPHORESIS, Issue 20 2007Marek Urbanek Abstract The analysis of sub-ppb levels of Fe(II), Co(II), and Ni(II) in heat exchanger fluids of nuclear power plants is needed to monitor corrosion. A method involving preconcentration with electrokinetic supercharging (electrokinetic injection with transient ITP), CZE separation, and in-capillary derivatization with ortho -phenanthroline (o -Phe) for direct UV detection was thus developed. First, a multizone BGE was loaded into the capillary by successive hydrodynamic introduction of zones of (i) o -Phe-containing BGE, (ii) BGE for the zonal separation, and (iii) ammonium-based leading electrolyte. Metal cations were electrokinetically injected and stacked at the capillary inlet behind this last leading zone. Finally, a terminating electrolyte zone was hydrodynamically introduced. When a constant voltage was applied, metal ions kept on concentrating isotachophoretically, then separated in CZE mode, were complexed by migrating through an o -Phe zone, and finally detected by direct absorbance. To detect extremely thin peaks, it was attempted for the first time to focus the derivatization reagent by inducing a second transient ITP, before labeling analytes, already separated in CZE mode. With this arrangement, LODs were about 30,ppt in pure water. In heat exchanger fluid matrices containing 1000,ppm bore and 2,ppm lithium, only Fe(II) cation was detected among the three cations of interest at the 1,ppb level using the present method, and its LOD was about ten times higher, due to the lower loading rate during electrokinetic injection. [source] Breath gas aldehydes as biomarkers of lung cancerINTERNATIONAL JOURNAL OF CANCER, Issue 11 2010Patricia Fuchs Abstract There is experimental evidence that volatile substances in human breath can reflect presence of neoplasma. Volatile aldehydes were determined in exhaled breath of 12 lung cancer patients, 12 smokers and 12 healthy volunteers. Alveolar breath samples were collected under control of expired CO2. Reactive aldehydes were transformed into stable oximes by means of on-fiber-derivatization (SPME-OFD). Aldehyde concentrations in the ppt and ppb level were determined by means of gas chromatography-mass spectrometry (GC-MS). Exhaled concentrations were corrected for inspired values. Exhaled C1,C10 aldehydes could be detected in all healthy volunteers, smokers and lung cancer patients. Concentrations ranged from 7 pmol/l (161 pptV) for butanal to 71 nmol/l (1,582 ppbV) for formaldehyde. Highest inspired concentrations were found for formaldehyde and acetaldehyde (0,55 nmol/l and 0,13 nmol/l, respectively). Acetaldehyde, propanal, butanal, heptanal and decanal concentrations showed no significant differences for cancer patients, smokers and healthy volunteers. Exhaled pentanal, hexanal, octanal and nonanal concentrations were significantly higher in lung cancer patients than in smokers and healthy controls (ppentanal = 0.001; phexanal = 0.006; poctanal = 0.014; pnonanal = 0.025). Sensitivity and specificity of this method were comparable to the diagnostic certitude of conventional serum markers and CT imaging. Lung cancer patients could be identified by means of exhaled pentanal, hexanal, octanal and nonanal concentrations. Exhaled aldehydes reflect aspects of oxidative stress and tumor-specific tissue composition and metabolism. Noninvasive recognition of lung malignancies may be realized if analytical skills, biochemical knowledge and medical expertise are combined into a joint effort. [source] A comparative study of several HPLC methods for determining free amino acid profiles in honeyJOURNAL OF SEPARATION SCIENCE, JSS, Issue 9-10 2005José Luis Bernal Abstract A study of the viability of three derivatizing reagents for obtaining amino acid profiles in honey through high performance liquid chromatography (HPLC) is presented. A method using diode array detection based on a reaction with diethyl ethoxymethylene malonate (DEMM) and two other methods using fluorescence detection based on derivatization with fluorenylmethyl chloroformate (FMOC-Cl) and 6-aminoquinolyl- N -hydroxysuccinimidyl carbamate (AQC) have been developed. The three methods yield detection limits close to the ppb level, but vary in relation to other analytical characteristics. The use of methyl chloroformate derivatives allows the profile to be obtained with the greatest sensitivity within a short time frame. On applying such methods to honey samples of diverse botanical origin, we observe that the proline values obtained are always lower than those found using the official spectrophotometric method, thereby underlining the advisability of using HPLC methods to reduce uncertainty in these results. [source] Determination of lead content in medicinal plants by pre-concentration flow injection analysis,flame atomic absorption spectrometryPHYTOCHEMICAL ANALYSIS, Issue 6 2009Marina M. A. Campos Abstract Introduction , Although medicinal plants are widely used throughout the world, few studies have been carried out concerning the levels of heavy metal contaminants present. Such metals are highly toxic to living organisms even in low concentrations owing to their cumulative effect. The present paper describes the the development of a pre-concentration flow injection analysis-flame atomic absorption spectrometric system to determine the lead content in medicinal plants at the ppb level. Objective , To develop a pre-concentration flow injection analysis-flame atomic absorption spectrometric system to determine the lead content in medicinal plants at the ppb level. Methodology , A pre-concentration flow system was coupled to a flame atomic absorption spectrometer. The plant samples were analysed after nitroperchloric digestion. The proposed system was optimised by evaluating the following parameters: nature, concentration and volume of the eluent solution, elution flow rate, elution efficiency, pre-concentration flow rate and pre-concentration time. Results , The proposed system exhibited good performance with high precision and repeatability (RSD , 2.36%), excellent linearity (r = 0.9999), low sample consumption (10.5 mL per determination) and an analytical throughput of 55 samples/h. Lead concentrations ranged from 3.37 ± 0.25 to 7.03 ± 0.51 ,g/g in dry material. This concentration interval is greater than that previously published in the literature. Conclusion , The inclusion of a pre-concentration column in the flow manifold improved the sensitivity of the spectrometer. Thus, it was possible to determine the analyte at the ng/mL level in sample solutions of medicinal plants. This is a very important accomplishment, especially when the cumulative effect of heavy metals in living organisms is considered. Copyright © 2009 John Wiley & Sons, Ltd. [source] An original approach to determining traces of tetracycline antibiotics in milk and eggs by solid-phase extraction and liquid chromatography/mass spectrometryRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 14 2002Federica Bruno An original and highly specific method able to identify and quantify traces of five tetracycline antibiotics (TCAs) in milk and eggs is presented. This method uses a single solid-phase extraction (SPE) cartridge for simultaneous extraction and purification of TCAs in the above matrices. After diluting 5,mL of intact whole milk or 2,g egg samples with Na2EDTA-containing water, samples are passed through a 0.5-g Carbograph 4 extraction cartridge. After analyte elution from the SPE cartridge, an aliquot of the final extract is injected into a liquid chromatography/mass spectrometry (LC/MS) instrument equipped with an electrospray ion source and a single quadrupole. MS data acquisition is performed in the positive-ion mode and by a time-scheduled multiple-ion selected ion-monitoring program. With methanol as organic modifier, the in-source collision-induced dissociation (CID) process generated fragment ions able to pick up one methanol molecule. In several cases, these methanol-adduct fragment ions have m/z values higher than those of the protonated molecules. This event is rarely encountered in MS, thus making the analysis of TCAs by this method extremely specific. Compared with a conventional published method, the present protocol extracted larger amounts of TCAs from both milk and egg and decreased the analysis time by a factor of 3. Recovery of TCAs in milk at the 25-ppb level ranged between 81 and 96% with relative standard deviation (RSD) no larger than 9%. Recovery of TCAs in egg at the 50-ppb level ranged between 72 and 92% with RSD no larger than 7%. Estimated limits of quantification(S/N,=,10) of the method were 2,9 ppb TCAs in whole milk and 2,19 ppb TCAs in eggs. Copyright© 2002 John Wiley & Sons, Ltd. [source] Determination of trace cationic impurities in butylmethylimidazolium-based ionic liquids: From transient to comprehensive single-capillary counterflow isotachophoresis-zone electrophoresisELECTROPHORESIS, Issue 23 2006Marek Urbánek Abstract Determination of impurities in ionic liquids (ILs) remains a difficult task. In this work, the hyphenation of isotachophoretic,(ITP) preconcentration to zone electrophoresis,(ZE) has been explored for the trace analysis of the cationic impurities Na+, Li+, and methylimidazolium (MI+) in butylmethylimidazolium (BMI+)-based ILs. Simultaneous detection of UV-transparent and UV-absorbing impurities was ensured by a BGE composed of creatinine-acetate buffer. To induce ITP, three different strategies were evaluated: (i),Sample self-stacking ensured by the addition of ammonium acetate (NH4Ac) to 25,50-fold diluted IL solution (transient ITP). (ii),Complete ITP-ZE separation performed in a single capillary: ITP was realized in discontinuous electrolytes comprising an 80,mM NH4Ac, 40,mM acetic acid, 30,mM ,-CD, pH,5.05, leading electrolyte,(LE) and a 10,mM creatinine, 10,mM acetic acid, pH,4.9, terminating electrolyte,(TE). To create the ZE stage, the ITP stack of analytes was moved back toward the capillary inlet by pressure and simultaneously the capillary was filled with the BGE. This protocol made it possible to accommodate a 2.5-times diluted IL sample. (iii),Complete counterflow ITP-ZE with continuous electrokinetic sample supply: the ITP stage was performed in a capillary filled with a 150,mM NH4Ac, 75,mM acetic acid, 30,mM ,-CD, pH,5.0 LE, with 40-times diluted IL at the capillary inlet. BMI+ from IL acts as the terminating ion. The LODs reached in this latter case were at the 10 and 1,ppb levels for MI+ and Li+ in diluted IL matrix, respectively. [source] Selected ion flow tube mass spectrometry (SIFT-MS) for on-line trace gas analysisMASS SPECTROMETRY REVIEWS, Issue 5 2005David Smith Abstract Selected ion flow tube mass spectrometry (SIFT-MS) is a new analytical technique for the real-time quantification of several trace gases simultaneously in air and breath. It relies on chemical ionization of the trace gas molecules in air/breath samples introduced into helium carrier gas using H3O+, NO+, and O precursor ions. Reactions between the precursor ions and trace gas molecules proceed for an accurately defined time, the precursor and product ions being detected and counted by a downstream mass spectrometer, thus effecting quantification. Absolute concentrations of trace gases in single breath exhalation can be determined by SIFT-MS down to ppb levels, obviating sample collection and calibration. Illustrative examples of SIFT-MS studies include (i) analysis of gases from combustion engines, animals and their waste, and food; (ii) breath and urinary headspace studies of metabolites, ethanol metabolism, elevated acetone during ovulation, and exogenous compounds; and (iii) urinary infection and the presence of tumors, the influence of dialysis on breath ammonia, acetone, and isoprene, and acetaldehyde released by cancer cells in vitro. Flowing afterglow mass spectrometry (FA-MS) is briefly described, which allows on-line quantification of deuterium in breath water vapor. © 2004 Wiley Periodicals, Inc., Mass Spec Rev 24:661,700, 2005 [source] | ||||||||||