Gunshot residue particles formed by using ammunitions that have mercury fulminate based primers.

PubMed

Zeichner, A; Levin, N; Dvorachek, M

1992-11-01

Ammunition having mercury fulminate-based primers are commonly manufactured by Eastern Bloc countries and used extensively in the Middle East. Gunshot residue (GSR) particles formed by firing these types of ammunition were examined. It was observed that much lower percentage of mercury-containing GSR particles were found in samples taken from a shooter as compared to the percentage of such particles in samples from cartridge cases. This fact must therefore be taken into account when interpreting case results. A plausible explanation for the results described is proposed.

Number of viable bacteria and presumptive antibiotic residues in milk fed to calves on commercial dairies.

PubMed

Selim, S A; Cullor, J S

1997-10-15

To assess the number of bacteria and presumptive antibiotic residues in milk fed to calves and to identify those bacteria and the antibiotic susceptibility of selected bacterial strains. Cross-sectional prospective study. 189 samples obtained from 12 local dairies. Samples of waste milk and milk-based fluids (eg, milk replacer, colostrum, bulk-tank milk) were obtained. Cumulative number of viable bacteria was determined. Bacteria were cultured aerobically, and antibiotic susceptibility testing of selected strains was performed. Presumptive antibiotic residues were detected by use of test kits. Geometric mean of the cumulative number of bacteria for waste milk samples was significantly higher than for other types of milk or milk-based products. Streptococcus sp (84/165 samples) and Enterobacteriaceae (83/165 samples) were the predominant bacteria identified, followed by Staphylococcus sp (68/165 samples). Escherichia coli was the gram-negative species most commonly isolated (52/165 samples; 32%); however, none were strain O157. Salmonella sp or Mycoplasma sp were not isolated. Of 189 samples, 119 (63%) were positive when tested for beta-lactams or tetracycline by use of 2 commercially available assays. In vitro, some bacteria were resistant to commonly used antibiotics. Waste milk that has not been effectively treated (eg, pasteurization) to reduce microbial load prior to use as calf feed should be used with caution, because it may contain a high number of bacteria that may be pathogenic to cattle and human beings. Antibiotic residues that would constitute violative amounts and existence of multiple antibiotic resistant bacterial strains are concerns in calf health management and dairy food safety.

Topics in Statistical Calibration

DTIC Science & Technology

2014-03-27

on a parametric bootstrap where, instead of sampling directly from the residuals , samples are drawn from a normal distribution. This procedure will...addition to centering them (Davison and Hinkley, 1997). When there are outliers in the residuals , the bootstrap distribution of x̂0 can become skewed or...based and inversion methods using the linear mixed-effects model. Then, a simple parametric bootstrap algorithm is proposed that can be used to either

Detection of poly(ethylene glycol) residues from nonionic surfactants in surface water by1h and13c nuclear magnetic resonance spectrometry

USGS Publications Warehouse

Leenheer, J.A.; Wershaw, R. L.; Brown, P.A.; Noyes, T.I.

1991-01-01

??? Poly(ethylene glycol) (PEG) residues were detected in organic solute isolates from surface water by 1H nuclear magnetic resonance spectrometry (NMR), 13C NMR spectrometry, and colorimetric assay. PEG residues were separated from natural organic solutes in Clear Creek, CO, by a combination of methylation and chromatographic procedures. The isolated PEG residues, characterized by NMR spectrometry, were found to consist of neutral and acidic residues that also contained poly(propylene glycol) moieties. The 1H NMR and the colorimetric assays for poly(ethylene glycol) residues were done on samples collected in the lower Mississippi River and tributaries between St. Louis, MO, and New Orleans, LA, in July-August and November-December 1987. Aqueous concentrations for poly(ethylene glycol) residues based on colorimetric assay ranged from undetectable to ???28 ??g/L. Concentrations based on 1H NMR spectrometry ranged from undetectable to 145 ??g/L.

Influence of veneer thickness on residual stress profile in veneering ceramic: measurement by hole-drilling.

PubMed

Mainjot, Amélie K; Schajer, Gary S; Vanheusden, Alain J; Sadoun, Michaël J

2012-02-01

The veneering process of frameworks induces residual stresses and can initiate cracks when combined with functional stresses. The stress distribution within the veneering ceramic as a function of depth is a key factor influencing failure by chipping. This is a well-known problem with Yttria-tetragonal-zirconia-polycrystal based fixed partial dentures. The objective of this study is to investigate the influence of veneer thickness on the stress profile in zirconia- and metal-based structures. The hole-drilling method, often used for engineering measurements, was adapted for use with veneering ceramic. The stress profile was measured in bilayered disc samples of 20 mm diameter, with a 1 mm thick zirconia or metal framework. Different veneering ceramic thicknesses were performed: 1 mm, 1.5 mm, 2 mm, 2.5 mm and 3 mm. All samples exhibited the same type of stress vs. depth profile, starting with compressive at the ceramic surface, decreasing with depth up to 0.5-1.0 mm from the surface, and then becoming compressive again near the framework, except for the 1.5 mm-veneered zirconia samples which exhibited interior tensile stresses. Stresses in the surface of metal samples were not influenced by veneer thickness. Variation of interior stresses at 1.2 mm from the surface in function of veneer thickness was inverted for metal and zirconia samples. Veneer thickness influences in an opposite way the residual stress profile in metal- and in zirconia-based structures. A three-step approach and the hypothesis of the crystalline transformation are discussed to explain the less favorable residual stress development in zirconia samples. Copyright © 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Correcting for the influence of sampling conditions on biomarkers of exposure to phenols and phthalates: a 2-step standardization method based on regression residuals.

PubMed

Mortamais, Marion; Chevrier, Cécile; Philippat, Claire; Petit, Claire; Calafat, Antonia M; Ye, Xiaoyun; Silva, Manori J; Brambilla, Christian; Eijkemans, Marinus J C; Charles, Marie-Aline; Cordier, Sylvaine; Slama, Rémy

2012-04-26

Environmental epidemiology and biomonitoring studies typically rely on biological samples to assay the concentration of non-persistent exposure biomarkers. Between-participant variations in sampling conditions of these biological samples constitute a potential source of exposure misclassification. Few studies attempted to correct biomarker levels for this error. We aimed to assess the influence of sampling conditions on concentrations of urinary biomarkers of select phenols and phthalates, two widely-produced families of chemicals, and to standardize biomarker concentrations on sampling conditions. Urine samples were collected between 2002 and 2006 among 287 pregnant women from Eden and Pélagie cohorts, from which phthalates and phenols metabolites levels were assayed. We applied a 2-step standardization method based on regression residuals. First, the influence of sampling conditions (including sampling hour, duration of storage before freezing) and of creatinine levels on biomarker concentrations were characterized using adjusted linear regression models. In the second step, the model estimates were used to remove the variability in biomarker concentrations due to sampling conditions and to standardize concentrations as if all samples had been collected under the same conditions (e.g., same hour of urine collection). Sampling hour was associated with concentrations of several exposure biomarkers. After standardization for sampling conditions, median concentrations differed by--38% for 2,5-dichlorophenol to +80 % for a metabolite of diisodecyl phthalate. However, at the individual level, standardized biomarker levels were strongly correlated (correlation coefficients above 0.80) with unstandardized measures. Sampling conditions, such as sampling hour, should be systematically collected in biomarker-based studies, in particular when the biomarker half-life is short. The 2-step standardization method based on regression residuals that we proposed in order to limit the impact of heterogeneity in sampling conditions could be further tested in studies describing levels of biomarkers or their influence on health.

Health risk for children and adults consuming apples with pesticide residue.

PubMed

Lozowicka, Bozena

2015-01-01

The presence of pesticide residues in apples raises serious health concerns, especially when the fresh fruits are consumed by children, particularly vulnerable to the pesticide hazards. This study demonstrates the results from nine years of investigation (2005-2013) of 696 samples of Polish apples for 182 pesticides using gas and liquid chromatography and spectrophotometric techniques. Only 33.5% of the samples did not contain residues above the limit of detection. In 66.5% of the samples, 34 pesticides were detected, of which maximum residue level (MRL) was exceeded in 3%. Multiple residues were present in 35% of the samples with two to six pesticides, and one sample contained seven compounds. A study of the health risk for children, adults and the general population consuming apples with these pesticides was performed. The pesticide residue data have been combined with the consumption of apples in the 97.5 percentile and the mean diet. A deterministic model was used to assess the chronic and acute exposures that are based on the average and high concentrations of residues. Additionally, the "worst-case scenario" and "optimistic case scenario" were used to assess the chronic risk. In certain cases, the total dietary pesticide intake calculated from the residue levels observed in apples exceeds the toxicological criteria. Children were the group most exposed to the pesticides, and the greatest short-term hazard stemmed from flusilazole at 624%, dimethoate at 312%, tebuconazole at 173%, and chlorpyrifos methyl and captan with 104% Acute Reference Dose (ARfD) each. In the cumulative chronic exposure, among the 17 groups of compounds studied, organophosphate insecticides constituted 99% acceptable daily intake (ADI). The results indicate that the occurrence of pesticide residues in apples could not be considered a serious public health problem. Nevertheless, an investigation into continuous monitoring and tighter regulation of pesticide residues is recommended. Copyright © 2014 Elsevier B.V. All rights reserved.

Analysis of beta-lactam antibiotics in incurred raw milk by rapid test methods and liquid chromatography coupled with electrospray ionization tandem mass spectrometry.

PubMed

Riediker, S; Diserens, J M; Stadler, R H

2001-09-01

A recently developed confirmatory LC-MS method has been applied to the quantification of five major beta-lactam antibiotics in suspect raw bovine milk samples that gave a positive response with receptor-based (BetaStar) and rapid microbial inhibitory screen tests (Delvotest SP). In total, 18 presumptive positive raw milk samples were reanalyzed; 16 samples showed traces of antibiotic residues that could be identified and quantified by the LC-MS method, ranging from the limits of confirmation up to 38 microg/kg. Of the positive samples, only five (approximately 30%) were found to be violative of EU maximum residue limits. The most frequently detected antibiotic residues were cloxacillin and penicillin G, the former often in combination with amoxicillin or ampicillin. This study compares the results obtained by the three methods on identical samples and addresses how these relate to certain criteria such as sensitivity and selectivity. Furthermore, the limitations of the LC-MS method and the potential impact of the presence of frequently more than one residue in the same milk sample on the response of the rapid test methods are discussed.

Molecular cancer classification using a meta-sample-based regularized robust coding method.

PubMed

Wang, Shu-Lin; Sun, Liuchao; Fang, Jianwen

2014-01-01

Previous studies have demonstrated that machine learning based molecular cancer classification using gene expression profiling (GEP) data is promising for the clinic diagnosis and treatment of cancer. Novel classification methods with high efficiency and prediction accuracy are still needed to deal with high dimensionality and small sample size of typical GEP data. Recently the sparse representation (SR) method has been successfully applied to the cancer classification. Nevertheless, its efficiency needs to be improved when analyzing large-scale GEP data. In this paper we present the meta-sample-based regularized robust coding classification (MRRCC), a novel effective cancer classification technique that combines the idea of meta-sample-based cluster method with regularized robust coding (RRC) method. It assumes that the coding residual and the coding coefficient are respectively independent and identically distributed. Similar to meta-sample-based SR classification (MSRC), MRRCC extracts a set of meta-samples from the training samples, and then encodes a testing sample as the sparse linear combination of these meta-samples. The representation fidelity is measured by the l2-norm or l1-norm of the coding residual. Extensive experiments on publicly available GEP datasets demonstrate that the proposed method is more efficient while its prediction accuracy is equivalent to existing MSRC-based methods and better than other state-of-the-art dimension reduction based methods.

A Simple Joint Estimation Method of Residual Frequency Offset and Sampling Frequency Offset for DVB Systems

NASA Astrophysics Data System (ADS)

Kwon, Ki-Won; Cho, Yongsoo

This letter presents a simple joint estimation method for residual frequency offset (RFO) and sampling frequency offset (STO) in OFDM-based digital video broadcasting (DVB) systems. The proposed method selects a continual pilot (CP) subset from an unsymmetrically and non-uniformly distributed CP set to obtain an unbiased estimator. Simulation results show that the proposed method using a properly selected CP subset is unbiased and performs robustly.

Determination of organochlorine pesticide and polychlorinated biphenyl residues in fatty fish by tandem solid-phase extraction cleanup.

PubMed

Schenck, F J; Calderon, L; Podhorniak, L V

1996-01-01

A rapid, multiresidue solid-phase extraction (SPE) technique for determination of organochlorine pesticide and polychlorinated biphenyl (PCB) residues in nonfatty fish was modified for use with fatty fish. In the modified procedures, samples are extracted with acetonitrile, and the extract is cleaned up with both C18 and Florisil SPE columns. Residues are determined by gas chromatography with electron capture detection. The original method was modified for use with fatty fish by reducing the amount of tissue extracted and by using an improved Florisil SPE cleanup. Recovery data are presented for 24 fortified organochlorine pesticide residues (0.12 ppm) and 3 fortified PCB residues (0.80 ppm) from flounder, bluefish, and shad samples, which contained 0.8, 5.4, and 22.6% fat, respectively. For the 3 types of fish, recoveries of 23 of 24 fortified organochlorine pesticide residues ranged from 55 to 129%, and recoveries of 3 fortified PCB residues ranged from 55 to 104%. There were no significant differences in recovery based on fish species and/or fat content for the majority of residues studied. This SPE method and the official AOAC method yielded comparable results for fish containing incurred organochlorine residues.

Comprehensive profiling and marker identification in non-volatile citrus oil residues by mass spectrometry and nuclear magnetic resonance.

PubMed

Marti, Guillaume; Boccard, Julien; Mehl, Florence; Debrus, Benjamin; Marcourt, Laurence; Merle, Philippe; Delort, Estelle; Baroux, Lucie; Sommer, Horst; Rudaz, Serge; Wolfender, Jean-Luc

2014-05-01

The detailed characterization of cold-pressed lemon oils (CPLOs) is of great importance for the flavor and fragrance (F&F) industry. Since a control of authenticity by standard analytical techniques can be bypassed using elaborated adulterated oils to pretend a higher quality, a combination of advanced orthogonal methods has been developed. The present study describes a combined metabolomic approach based on UHPLC-TOF-MS profiling and (1)H NMR fingerprinting to highlight metabolite differences on a set of representative samples used in the F&F industry. A new protocol was set up and adapted to the use of CPLO residues. Multivariate analysis based on both fingerprinting methods showed significant chemical variations between Argentinian and Italian samples. Discriminating markers identified in mixtures belong to furocoumarins, flavonoids, terpenoids and fatty acids. Quantitative NMR revealed low citropten and high bergamottin content in Italian samples. The developed metabolomic approach applied to CPLO residues gives some new perspectives for authenticity assessment. Copyright © 2013 Elsevier Ltd. All rights reserved.

A simple, fast and cheap non-SPE screening method for antibacterial residue analysis in milk and liver using liquid chromatography-tandem mass spectrometry.

PubMed

Martins, Magda Targa; Melo, Jéssica; Barreto, Fabiano; Hoff, Rodrigo Barcellos; Jank, Louise; Bittencourt, Michele Soares; Arsand, Juliana Bazzan; Schapoval, Elfrides Eva Scherman

2014-11-01

In routine laboratory work, screening methods for multiclass analysis can process a large number of samples in a short time. The main challenge is to develop a methodology to detect as many different classes of residues as possible, combined with speed and low cost. An efficient technique for the analysis of multiclass antibacterial residues (fluoroquinolones, tetracyclines, sulfonamides and trimethoprim) was developed based on simple, environment-friendly extraction for bovine milk, cattle and poultry liver. Acidified ethanol was used as an extracting solvent for milk samples. Liver samples were treated using EDTA-washed sand for cell disruption, methanol:water and acidified acetonitrile as extracting solvent. A total of 24 antibacterial residues were detected and confirmed using liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS), at levels between 10, 25 and 50% of the maximum residue limit (MRL). For liver samples a metabolite (sulfaquinoxaline-OH) was also monitored. A validation procedure was conducted for screening purposes in accordance with European Union requirements (2002/657/EC). The detection capability (CCβ) false compliant rate was less than 5% at the lowest level for each residue. Specificity and ruggedness were also discussed. Incurred and routine samples were analyzed and the method was successfully applied. The results proved that this method can be an important tool in routine analysis, since it is very fast and reliable. Copyright © 2014. Published by Elsevier B.V.

Research on florfenicol residue in coastal area of dalian (northern china) and analysis of functional diversity of the microbial community in marine sediment.

PubMed

Zong, Humin; Ma, Deyi; Wang, Juying; Hu, Jiangtao

2010-02-01

An analytical method based on high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) has been developed to investigate florfenicol residues. Among 11 stations, florfenicol was detected in six water samples. The concentrations of florfenicol in the six samples were 64.2 microg L(-1), 390.6 microg L(-1), 1.1 x 10(4) microg L(-1), 29.8 microg L(-1), 61.6 microg L(-1), 34.9 microg L(-1), respectively. These results showed that high levels of florfenicol were observed in water samples collected from stations influenced by aquaculture discharges. However, no florfenicol residue was detected in the sediment samples. Furthermore, the functional diversities of microbial community in four marine sediment samples were analyzed by Biolog microplate. For the sediment samples from the stations where antibacterials had been used, the functional diversity of microbial community was much lower than those from the stations where antibacterials were not used.

Spatial Autocorrelation Approaches to Testing Residuals from Least Squares Regression.

PubMed

Chen, Yanguang

2016-01-01

In geo-statistics, the Durbin-Watson test is frequently employed to detect the presence of residual serial correlation from least squares regression analyses. However, the Durbin-Watson statistic is only suitable for ordered time or spatial series. If the variables comprise cross-sectional data coming from spatial random sampling, the test will be ineffectual because the value of Durbin-Watson's statistic depends on the sequence of data points. This paper develops two new statistics for testing serial correlation of residuals from least squares regression based on spatial samples. By analogy with the new form of Moran's index, an autocorrelation coefficient is defined with a standardized residual vector and a normalized spatial weight matrix. Then by analogy with the Durbin-Watson statistic, two types of new serial correlation indices are constructed. As a case study, the two newly presented statistics are applied to a spatial sample of 29 China's regions. These results show that the new spatial autocorrelation models can be used to test the serial correlation of residuals from regression analysis. In practice, the new statistics can make up for the deficiencies of the Durbin-Watson test.

Chemometric classification of gunshot residues based on energy dispersive X-ray microanalysis and inductively coupled plasma analysis with mass-spectrometric detection

NASA Astrophysics Data System (ADS)

Steffen, S.; Otto, M.; Niewoehner, L.; Barth, M.; Bro¿żek-Mucha, Z.; Biegstraaten, J.; Horváth, R.

2007-09-01

A gunshot residue sample that was collected from an object or a suspected person is automatically searched for gunshot residue relevant particles. Particle data (such as size, morphology, position on the sample for manual relocation, etc.) as well as the corresponding X-ray spectra and images are stored. According to these data, particles are classified by the analysis-software into different groups: 'gunshot residue characteristic', 'consistent with gunshot residue' and environmental particles, respectively. Potential gunshot residue particles are manually checked and - if necessary - confirmed by the operating forensic scientist. As there are continuing developments on the ammunition market worldwide, it becomes more and more difficult to assign a detected particle to a particular ammunition brand. As well, the differentiation towards environmental particles similar to gunshot residue is getting more complex. To keep external conditions unchanged, gunshot residue particles were collected using a specially designed shooting device for the test shots revealing defined shooting distances between the weapon's muzzle and the target. The data obtained as X-ray spectra of a number of particles (3000 per ammunition brand) were reduced by Fast Fourier Transformation and subjected to a chemometric evaluation by means of regularized discriminant analysis. In addition to the scanning electron microscopy in combination with energy dispersive X-ray microanalysis results, isotope ratio measurements based on inductively coupled plasma analysis with mass-spectrometric detection were carried out to provide a supplementary feature for an even lower risk of misclassification.

Quantification of 2D elemental distribution maps of intermediate-thick biological sections by low energy synchrotron μ-X-ray fluorescence spectrometry

NASA Astrophysics Data System (ADS)

Kump, P.; Vogel-Mikuš, K.

2018-05-01

Two fundamental-parameter (FP) based models for quantification of 2D elemental distribution maps of intermediate-thick biological samples by synchrotron low energy μ-X-ray fluorescence spectrometry (SR-μ-XRF) are presented and applied to the elemental analysis in experiments with monochromatic focused photon beam excitation at two low energy X-ray fluorescence beamlines—TwinMic, Elettra Sincrotrone Trieste, Italy, and ID21, ESRF, Grenoble, France. The models assume intermediate-thick biological samples composed of measured elements, the sources of the measurable spectral lines, and by the residual matrix, which affects the measured intensities through absorption. In the first model a fixed residual matrix of the sample is assumed, while in the second model the residual matrix is obtained by the iteration refinement of elemental concentrations and an adjusted residual matrix. The absorption of the incident focused beam in the biological sample at each scanned pixel position, determined from the output of a photodiode or a CCD camera, is applied as a control in the iteration procedure of quantification.

Recovery of Precious and Base Metals from Waste Printed Circuit Boards Using a Sequential Leaching Procedure

NASA Astrophysics Data System (ADS)

Batnasan, Altansukh; Haga, Kazutoshi; Shibayama, Atsushi

2018-02-01

This paper considers the issue of recycling of waste printed circuit boards (WPCBs) containing precious and base metals in appreciable amounts. High-pressure oxidative leaching (HPOL) with dilute sulfuric acid resulted in removal of a significant amount of base metals from a WPCB ash sample obtained by incineration at 800°C. The parameters investigated in the precious metal leaching from WPCB residue after HPOL included the sulfuric acid concentration, thiourea concentration, oxidant concentration, leaching temperature, and leaching time. Recovery of gold, silver, and palladium of 100%, 81%, and 13% from the WPCB residue sample was achieved by thiourea leaching under optimized conditions. The results show that the efficiency of precious metal dissolution from the WPCB sample using thiourea solution depended strongly on the concentration of both thiourea and oxidant.

Recovery of Precious and Base Metals from Waste Printed Circuit Boards Using a Sequential Leaching Procedure

NASA Astrophysics Data System (ADS)

Batnasan, Altansukh; Haga, Kazutoshi; Shibayama, Atsushi

2017-12-01

This paper considers the issue of recycling of waste printed circuit boards (WPCBs) containing precious and base metals in appreciable amounts. High-pressure oxidative leaching (HPOL) with dilute sulfuric acid resulted in removal of a significant amount of base metals from a WPCB ash sample obtained by incineration at 800°C. The parameters investigated in the precious metal leaching from WPCB residue after HPOL included the sulfuric acid concentration, thiourea concentration, oxidant concentration, leaching temperature, and leaching time. Recovery of gold, silver, and palladium of 100%, 81%, and 13% from the WPCB residue sample was achieved by thiourea leaching under optimized conditions. The results show that the efficiency of precious metal dissolution from the WPCB sample using thiourea solution depended strongly on the concentration of both thiourea and oxidant.

Solid phase microextraction and gas chromatography-mass spectrometry methods for residual solvent assessment in seized cocaine and heroin.

PubMed

Cabarcos, Pamela; Herbello-Hermelo, Paloma; Álvarez-Freire, Iván; Moreda-Piñeiro, Antonio; Tabernero, María Jesús; Bermejo, Ana María; Bermejo-Barrera, Pilar

2016-09-01

A simple sample pre-treatment method based on solid phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) has been optimized and validated for the assessment of 15 residual solvents (2-propanol, 2-methylpentane, 3-methylpentane, acetone, ethyl acetate, benzene, hexane, methylcyclohexane, methylcyclopentane, m-xylene, propyl acetate, toluene, 1,2,4-trimethylbenzene, dichloromethane, and ethylbenzene) in seized illicit cocaine and heroin. DMSO and DMF as sample diluents were found to offer the best residual solvent transference to the head space for further adsorption onto the SPME fiber, and the developed method therefore showed high sensitivity and analytical recovery. Variables affecting SPME were fully evaluated by applying an experimental design approach. Best conditions were found when using an equilibration time of 5 min at 70 °C and headspace sampling of residual solvents at the same temperature for 15 min. Method validation, performed within the requirements of international guidelines, showed excellent sensitivity, as well as intra- and inter-day precision and accuracy. The proposed methodology was applied to 96 cocaine samples and 14 heroin samples seized in Galicia (northwestern Spain) within 2013 and 2014.

MODELED RESIDENTIAL CHLORPYRIFOS EXPOSURE AND DOSE TO CHILDREN VIA DERMAL SURFACE RESIDUE CONTACT AND NON-DIETARY INGESTION

EPA Science Inventory

A physically-based stochastic model has been applied to estimate residential chlorpyrifos exposure and dace to children via the non-dietary ingestion and dermal residue contact pathways. Time-location-activity data for 2825 children were sampled from national surveys to generat...

Dispersed and piled woody residues volumes in coastal Douglas-fir cutblocks determined using high-resolution imagery from a UAV and from ground-based surveys.

NASA Astrophysics Data System (ADS)

Trofymow, J. A.; Gougeon, F.

2015-12-01

After forest harvest significant amounts of woody residues are left dispersed on site and some subsequently piled and burned. Quantification of residues is required for estimating C budgets, billable waste, harvest efficiency, bioenergy potential and smoke emissions. Trofymow (et al 2014 CJFR) compared remote sensing methods to ground-based waste and residue survey (WRS) methods for residue piles in 4 cutblocks in the Oyster River (OR) area in coastal BC. Compared to geospatial methods using 15cm orthophotos and LiDAR acquired in 2011 by helicopter, the WRS method underestimated pile wood by 30% to 50% while a USFS volume method overestimated pile wood by 50% if site specific packing ratios were not used. A geospatial method was developed in PCI Geomatica to analyze 2-bit images of logs >15cm diameters to determine dispersed wood residues in OR and compare to WRS methods. Across blocks, geospatial and WRS method wood volumes were correlated (R2=0.69), however volumes were 2.5 times larger for the geospatial vs WRS method. Methods for dispersed residues could not be properly compared as individual WRS plots were not georeferenced, only 12 plots were sampled in total, and low-resolution images poorly resolved logs. Thus, a new study in 2 cutblocks in the Northwest Bay (NWB) area acquired 2cm resolution RGB air-photography in 2014-15 using an Aeryon Sky Ranger UAV prior to and after burn pile construction. A total of 57 dispersed WRS plots and 24 WRS pile or accumulation plots were georeferenced and measured. Stero-pairs were used to generate point-clouds for pile bulk volumes. Images processed to 8-bit grey scale are being analyzed with a revised PCI method that better accounts for log overlaps. WRS methods depend on a good sample of plots and accurate determination of stratum (dispersed, roadside, piles, accumulations) areas. Analysis of NWB blocks shows WRS field methods for stratum area differ by 5-20% from that determined using orthophotos. Plot-level wood volumes in each plot and stratum determined by geospatial and WRS methods will be compared. While geospatial methods for residue determination is a 100% sample, compared to sample-based WRS method, difficulties in resolving logs in the images may mean the best method for determining residues requires a combination of geospatial and ground plot measurements. .

Pesticide residues in stone fruits from the south-eastern region of Poland in 2012-2104.

PubMed

Słowik-Borowiec, Magdalena; Szpyrka, Ewa; Rupar, Julian; Matyaszek, Aneta; Podbielska, Magdalena

2015-01-01

Peaches, sour cherries, nectarines, apricots, plums and cherries are fruit commonly known as "stone fruit". Their nutritional properties namely, vitamins, minerals, fiber and numerous microelements, make them a very important component of human diet. As fruit trees can be attacked by numerous diseases and pests, chemical protection of these crops is used. Therefore, it is important that the relevant governmental agencies or institutions ensure correct application of pesticides. The aim of the study was to evaluate the occurrence of pesticide residues in stone fruits south-eastern region of Poland in 2012-2014 in order to provide data to estimate health risk to consumers. Validated analytical methods based on liquid / liquid extraction coupled with gas chromatography with electron capture and nitrogen phosphorus detection (GC-ECD/NPD) and spectrophotometry (dithiocarbamates residues) were used for the analysis. 92 samples of stone fruits were tested for the presence of pesticide residues. 13 of all samples (14%) contained pesticide residues. 7 active substances were detected, including 5 fungicides: boscalide, bupirimate, difenoconazole, dithiocarbamates and captan, and 2 insecticides: cypermethrin and pirimicarb. In the analysed samples, the use of not recommended plant protection products in orchard crops were found. However, neither maximum residue levels (MRLs) recommended by the Regulation (EC) No 396/2005 were exceeded nor pesticides being unapproved by the Regulation (EC) No 1107/2009 detected in the analysed samples. Lack of plant protection products for control specific diseases or pests in crops results in the use of formulations not recommended for use in certain orchard crops. On a basis of results reported in previous years it can be concluded that occurrence of pesticide residues in stone fruit samples dropped significantly.

Development of a field testing protocol for identifying Deepwater Horizon oil spill residues trapped near Gulf of Mexico beaches.

PubMed

Han, Yuling; Clement, T Prabhakar

2018-01-01

The Deepwater Horizon (DWH) accident, one of the largest oil spills in U.S. history, contaminated several beaches located along the Gulf of Mexico (GOM) shoreline. The residues from the spill still continue to be deposited on some of these beaches. Methods to track and monitor the fate of these residues require approaches that can differentiate the DWH residues from other types of petroleum residues. This is because, historically, the crude oil released from sources such as natural seeps and anthropogenic discharges have also deposited other types of petroleum residues on GOM beaches. Therefore, identifying the origin of these residues is critical for developing effective management strategies for monitoring the long-term environmental impacts of the DWH oil spill. Advanced fingerprinting methods that are currently used for identifying the source of oil spill residues require detailed laboratory studies, which can be cost-prohibitive. Also, most agencies typically use untrained workers or volunteers to conduct shoreline monitoring surveys and these worker will not have access to advanced laboratory facilities. Furthermore, it is impractical to routinely fingerprint large volumes of samples that are collected after a major oil spill event, such as the DWH spill. In this study, we propose a simple field testing protocol that can identify DWH oil spill residues based on their unique physical characteristics. The robustness of the method is demonstrated by testing a variety of oil spill samples, and the results are verified by characterizing the samples using advanced chemical fingerprinting methods. The verification data show that the method yields results that are consistent with the results derived from advanced fingerprinting methods. The proposed protocol is a reliable, cost-effective, practical field approach for differentiating DWH residues from other types of petroleum residues.

Development of a field testing protocol for identifying Deepwater Horizon oil spill residues trapped near Gulf of Mexico beaches

PubMed Central

Han, Yuling

2018-01-01

The Deepwater Horizon (DWH) accident, one of the largest oil spills in U.S. history, contaminated several beaches located along the Gulf of Mexico (GOM) shoreline. The residues from the spill still continue to be deposited on some of these beaches. Methods to track and monitor the fate of these residues require approaches that can differentiate the DWH residues from other types of petroleum residues. This is because, historically, the crude oil released from sources such as natural seeps and anthropogenic discharges have also deposited other types of petroleum residues on GOM beaches. Therefore, identifying the origin of these residues is critical for developing effective management strategies for monitoring the long-term environmental impacts of the DWH oil spill. Advanced fingerprinting methods that are currently used for identifying the source of oil spill residues require detailed laboratory studies, which can be cost-prohibitive. Also, most agencies typically use untrained workers or volunteers to conduct shoreline monitoring surveys and these worker will not have access to advanced laboratory facilities. Furthermore, it is impractical to routinely fingerprint large volumes of samples that are collected after a major oil spill event, such as the DWH spill. In this study, we propose a simple field testing protocol that can identify DWH oil spill residues based on their unique physical characteristics. The robustness of the method is demonstrated by testing a variety of oil spill samples, and the results are verified by characterizing the samples using advanced chemical fingerprinting methods. The verification data show that the method yields results that are consistent with the results derived from advanced fingerprinting methods. The proposed protocol is a reliable, cost-effective, practical field approach for differentiating DWH residues from other types of petroleum residues. PMID:29329313

Residual pyrethroids in fresh horticultural products in Sonora, Mexico.

PubMed

Aldana-Madrid, Maria L; Valenzuela-Quintanar, Ana I; Silveira-Gramont, Maria I; Rodríguez-Olibarría, Guillermo; Grajeda-Cota, Patricia; Zuno-Floriano, Fabiola G; Miller, Marion G

2011-10-01

This study was conducted to evaluate the presence of cyhialothrin, cyfluthrin, cypermethrin, fenvalerate, and deltamethrin in vegetables produced and consumed in Sonora, Mexico. A total of 345 samples were collected from cluster sampling of markets and fields. Approximately 9% of the samples tested positive for pyrethroids (residue range 0.004-0.573 mg kg(-1)). Based on the results, the potential toxicological risk of human exposure to the pyrethroid insecticides measured in vegetables appears to be minimal, with the estimated exposure being 1,000 times lower than admissible levels. © Springer Science+Business Media, LLC 2011

Multivariate Optimization for Extraction of Pyrethroids in Milk and Validation for GC-ECD and CG-MS/MS Analysis

PubMed Central

Zanchetti Meneghini, Leonardo; Rübensam, Gabriel; Claudino Bica, Vinicius; Ceccon, Amanda; Barreto, Fabiano; Flores Ferrão, Marco; Bergold, Ana Maria

2014-01-01

A simple and inexpensive method based on solvent extraction followed by low temperature clean-up was applied for determination of seven pyrethroids residues in bovine raw milk using gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) and gas chromatography with electron-capture detector (GC-ECD). Sample extraction procedure was established through the evaluation of seven different extraction protocols, evaluated in terms of analyte recovery and cleanup efficiency. Sample preparation optimization was based on Doehlert design using fifteen runs with three different variables. Response surface methodologies and polynomial analysis were used to define the best extraction conditions. Method validation was carried out based on SANCO guide parameters and assessed by multivariate analysis. Method performance was considered satisfactory since mean recoveries were between 87% and 101% for three distinct concentrations. Accuracy and precision were lower than ±20%, and led to no significant differences (p < 0.05) between results obtained by GC-ECD and GC-MS/MS techniques. The method has been applied to routine analysis for determination of pyrethroid residues in bovine raw milk in the Brazilian National Residue Control Plan since 2013, in which a total of 50 samples were analyzed. PMID:25380457

Harvest time residues of pendimethalin and oxyfluorfen in vegetables and soil in sugarcane-based intercropping systems.

PubMed

Kaur, Navneet; Bhullar, Makhan S

2015-05-01

Terminal residues of pendimethalin and oxyfluorfen applied in autumn sugarcane- and vegetables-based intercropping systems were analyzed in peas (Pisum sativum), cabbage (Brassica oleracea), garlic (Allium sativum), gobhi sarson (Brassica napus), and raya (Brassica juncea). The study was conducted in winter season in 2010-2011 and in 2011-2012 at Ludhiana, India. Pendimethalin at 0.56 kg and 0.75 kg ha(-1) was applied immediately after sowing of gobhi sarson, raya, peas, garlic, and 2 days before transplanting of cabbage seedlings. Oxyfluorfen at 0.17 kg and 0.23 kg ha(-1) was applied immediately after sowing of peas and garlic and 2 days before transplanting of cabbage seedlings intercropped in autumn sugarcane. Representative samples of these vegetables were collected at 75, 90, 100, and 165 days after application of herbicides and analyzed by high-performance liquid chromatograph (HPLC) with diode array detector for residues. The residue level of pendimethalin and oxyfluorfen in mature vegetables was found to be below the limit of quantification which is 0.05 mg kg(-1) for both the herbicides. The soil samples were collected at 0, 7, 15, 30, 45, and 60 days after the application of their herbicides. The residues of herbicides in soil samples were found to be below the detectability limit of 0.05 mg kg(-1) after 60 days in case of pendimethalin and after 45 days in case of oxyfluorfen.

Establishing and performing targeted multi-residue analysis for lipid mediators and fatty acids in small clinical plasma samples.

USDA-ARS?s Scientific Manuscript database

LC-MS/MS and GC-MS based targeted metabolomics is typically conducted by analyzing and quantifying a cascade of metabolites with methods specifically developed for the metabolite class. Here we describe an approach for the development of multi-residue analytical profiles, calibration standards, and ...

Optimisation of recovery protocols for double-base smokeless powder residues analysed by total vaporisation (TV) SPME/GC-MS.

PubMed

Sauzier, Georgina; Bors, Dana; Ash, Jordan; Goodpaster, John V; Lewis, Simon W

2016-09-01

The investigation of explosive events requires appropriate evidential protocols to recover and preserve residues from the scene. In this study, a central composite design was used to determine statistically validated optimum recovery parameters for double-base smokeless powder residues on steel, analysed using total vaporisation (TV) SPME/GC-MS. It was found that maximum recovery was obtained using isopropanol-wetted swabs stored under refrigerated conditions, then extracted for 15min into acetone on the same day as sample collection. These parameters were applied to the recovery of post-blast residues deposited on steel witness surfaces following a PVC pipe bomb detonation, resulting in detection of all target components across the majority of samples. Higher overall recoveries were obtained from plates facing the sides of the device, consistent with the point of first failure occurring in the pipe body as observed in previous studies. The methodology employed here may be readily applied to a variety of other explosive compounds, and thus assist in establishing 'best practice' procedures for explosive investigations. Copyright © 2016 Elsevier B.V. All rights reserved.

MCCE analysis of the pKas of introduced buried acids and bases in staphylococcal nuclease.

PubMed

Gunner, M R; Zhu, Xuyu; Klein, Max C

2011-12-01

The pK(a)s of 96 acids and bases introduced into buried sites in the staphylococcal nuclease protein (SNase) were calculated using the multiconformation continuum electrostatics (MCCE) program and the results compared with experimental values. The pK(a)s are obtained by Monte Carlo sampling of coupled side chain protonation and position as a function of pH. The dependence of the results on the protein dielectric constant (ε(prot)) in the continuum electrostatics analysis and on the Lennard-Jones non-electrostatics parameters was evaluated. The pK(a)s of the introduced residues have a clear dependence on ε(prot,) whereas native ionizable residues do not. The native residues have electrostatic interactions with other residues in the protein favoring ionization, which are larger than the desolvation penalty favoring the neutral state. Increasing ε(prot) scales both terms, which for these residues leads to small changes in pK(a). The introduced residues have a larger desolvation penalty and negligible interactions with residues in the protein. For these residues, changing ε(prot) has a large influence on the calculated pK(a). An ε(prot) of 8-10 and a Lennard-Jones scaling of 0.25 is best here. The X-ray crystal structures of the mutated proteins are found to provide somewhat better results than calculations carried out on mutations made in silico. Initial relaxation of the in silico mutations by Gromacs and extensive side chain rotamer sampling within MCCE can significantly improve the match with experiment. Copyright © 2011 Wiley-Liss, Inc.

Spatial Autocorrelation Approaches to Testing Residuals from Least Squares Regression

PubMed Central

Chen, Yanguang

2016-01-01

In geo-statistics, the Durbin-Watson test is frequently employed to detect the presence of residual serial correlation from least squares regression analyses. However, the Durbin-Watson statistic is only suitable for ordered time or spatial series. If the variables comprise cross-sectional data coming from spatial random sampling, the test will be ineffectual because the value of Durbin-Watson’s statistic depends on the sequence of data points. This paper develops two new statistics for testing serial correlation of residuals from least squares regression based on spatial samples. By analogy with the new form of Moran’s index, an autocorrelation coefficient is defined with a standardized residual vector and a normalized spatial weight matrix. Then by analogy with the Durbin-Watson statistic, two types of new serial correlation indices are constructed. As a case study, the two newly presented statistics are applied to a spatial sample of 29 China’s regions. These results show that the new spatial autocorrelation models can be used to test the serial correlation of residuals from regression analysis. In practice, the new statistics can make up for the deficiencies of the Durbin-Watson test. PMID:26800271

Influence of cooling rate on residual stress profile in veneering ceramic: measurement by hole-drilling.

PubMed

Mainjot, Amélie K; Schajer, Gary S; Vanheusden, Alain J; Sadoun, Michaël J

2011-09-01

The manufacture of dental crowns and bridges generates residual stresses within the veneering ceramic and framework during the cooling process. Residual stress is an important factor that control the mechanical behavior of restorations. Knowing the stress distribution within the veneering ceramic as a function of depth can help the understanding of failures, particularly chipping, a well-known problem with Yttria-tetragonal-zirconia-polycrystal based fixed partial dentures. The objective of this study is to investigate the cooling rate dependence of the stress profile in veneering ceramic layered on metal and zirconia frameworks. The hole-drilling method, often used for engineering measurements, was adapted for use with veneering ceramic. The stress profile was measured in bilayered disc samples 20 mm in diameter, with a 0.7 mm thick metal or Yttria-tetragonal-zirconia-polycrystal framework and a 1.5mm thick veneering ceramic. Three different cooling procedures were investigated. The magnitude of the stresses in the surface of the veneering ceramic was found to increase with cooling rate, while the interior stresses decreased. At the surface, compressive stresses were observed in all samples. In the interior, compressive stresses were observed in metal samples and tensile in zirconia samples. Cooling rate influences the magnitude of residual stresses. These can significantly influence the mechanical behavior of metal-and zirconia-based bilayered systems. The framework material influenced the nature of the interior stresses, with zirconia samples showing a less favorable stress profile than metal. Copyright © 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Matrix-Matching as an Improvement Strategy for the Detection of Pesticide Residues.

PubMed

Giacinti, Géraldine; Raynaud, Christine; Capblancq, Sophie; Simon, Valérie

2016-05-01

More than 90% of the pesticides residues in apples are located in the peel. We developed a gas chromatography/ion trap tandem mass spectrometry method for investigating all detectable residues in the peel of 3 apple varieties. Sample preparation is based on the use of the Quick Easy Cheap Effective Rugged and Safe method on the whole fruit, the flesh, and the peel. Pesticide residues were quantified with solvent-matched and matrix-matched standards, by spiking apple sample extracts. Matrix effects dependent on the type of extract (fruit, flesh, or peel) and the apple variety were detected. The best data processing methods involved normalizing matrix effect rates by matrix-matched internal/external calibration. Boscalid, captan, chlorpyrifos, fludioxonil, and pyraclostrobin were the most frequently detected pesticides. However, their concentrations in the whole fruit were below European maximum residue levels. Despite negative matrix effects, the residues in peel were detected at concentrations up to 10 times higher than those in whole fruits. Consequently, other pesticide residues present at concentrations below the limit of quantification in the whole fruit were detected in the peel. © 2016 Institute of Food Technologists®

Residual antibiotics in decontaminated human cardiovascular tissues intended for transplantation and risk of falsely negative microbiological analyses.

PubMed

Buzzi, Marina; Guarino, Anna; Gatto, Claudio; Manara, Sabrina; Dainese, Luca; Polvani, Gianluca; Tóthová, Jana D'Amato

2014-01-01

We investigated the presence of antibiotics in cryopreserved cardiovascular tissues and cryopreservation media, after tissue decontamination with antibiotic cocktails, and the impact of antibiotic residues on standard tissue bank microbiological analyses. Sixteen cardiovascular tissues were decontaminated with bank-prepared cocktails and cryopreserved by two different tissue banks according to their standard operating procedures. Before and after decontamination, samples underwent microbiological analysis by standard tissue bank methods. Cryopreserved samples were tested again with and without the removal of antibiotic residues using a RESEP tube, after thawing. Presence of antibiotics in tissue homogenates and processing liquids was determined by a modified agar diffusion test. All cryopreserved tissue homogenates and cryopreservation media induced important inhibition zones on both Staphylococcus aureus- and Pseudomonas aeruginosa-seeded plates, immediately after thawing and at the end of the sterility test. The RESEP tube treatment markedly reduced or totally eliminated the antimicrobial activity of tested tissues and media. Based on standard tissue bank analysis, 50% of tissues were found positive for bacteria and/or fungi, before decontamination and 2 out of 16 tested samples (13%) still contained microorganisms after decontamination. After thawing, none of the 16 cryopreserved samples resulted positive with direct inoculum method. When the same samples were tested after removal of antibiotic residues, 8 out of 16 (50%) were contaminated. Antibiotic residues present in tissue allografts and processing liquids after decontamination may mask microbial contamination during microbiological analysis performed with standard tissue bank methods, thus resulting in false negatives.

Residual Antibiotics in Decontaminated Human Cardiovascular Tissues Intended for Transplantation and Risk of Falsely Negative Microbiological Analyses

PubMed Central

Gatto, Claudio; Manara, Sabrina; Dainese, Luca; Polvani, Gianluca; Tóthová, Jana D'Amato

2014-01-01

We investigated the presence of antibiotics in cryopreserved cardiovascular tissues and cryopreservation media, after tissue decontamination with antibiotic cocktails, and the impact of antibiotic residues on standard tissue bank microbiological analyses. Sixteen cardiovascular tissues were decontaminated with bank-prepared cocktails and cryopreserved by two different tissue banks according to their standard operating procedures. Before and after decontamination, samples underwent microbiological analysis by standard tissue bank methods. Cryopreserved samples were tested again with and without the removal of antibiotic residues using a RESEP tube, after thawing. Presence of antibiotics in tissue homogenates and processing liquids was determined by a modified agar diffusion test. All cryopreserved tissue homogenates and cryopreservation media induced important inhibition zones on both Staphylococcus aureus- and Pseudomonas aeruginosa-seeded plates, immediately after thawing and at the end of the sterility test. The RESEP tube treatment markedly reduced or totally eliminated the antimicrobial activity of tested tissues and media. Based on standard tissue bank analysis, 50% of tissues were found positive for bacteria and/or fungi, before decontamination and 2 out of 16 tested samples (13%) still contained microorganisms after decontamination. After thawing, none of the 16 cryopreserved samples resulted positive with direct inoculum method. When the same samples were tested after removal of antibiotic residues, 8 out of 16 (50%) were contaminated. Antibiotic residues present in tissue allografts and processing liquids after decontamination may mask microbial contamination during microbiological analysis performed with standard tissue bank methods, thus resulting in false negatives. PMID:25397402

Resampling-based Methods in Single and Multiple Testing for Equality of Covariance/Correlation Matrices

PubMed Central

Yang, Yang; DeGruttola, Victor

2016-01-01

Traditional resampling-based tests for homogeneity in covariance matrices across multiple groups resample residuals, that is, data centered by group means. These residuals do not share the same second moments when the null hypothesis is false, which makes them difficult to use in the setting of multiple testing. An alternative approach is to resample standardized residuals, data centered by group sample means and standardized by group sample covariance matrices. This approach, however, has been observed to inflate type I error when sample size is small or data are generated from heavy-tailed distributions. We propose to improve this approach by using robust estimation for the first and second moments. We discuss two statistics: the Bartlett statistic and a statistic based on eigen-decomposition of sample covariance matrices. Both statistics can be expressed in terms of standardized errors under the null hypothesis. These methods are extended to test homogeneity in correlation matrices. Using simulation studies, we demonstrate that the robust resampling approach provides comparable or superior performance, relative to traditional approaches, for single testing and reasonable performance for multiple testing. The proposed methods are applied to data collected in an HIV vaccine trial to investigate possible determinants, including vaccine status, vaccine-induced immune response level and viral genotype, of unusual correlation pattern between HIV viral load and CD4 count in newly infected patients. PMID:22740584

Resampling-based methods in single and multiple testing for equality of covariance/correlation matrices.

PubMed

Yang, Yang; DeGruttola, Victor

2012-06-22

Traditional resampling-based tests for homogeneity in covariance matrices across multiple groups resample residuals, that is, data centered by group means. These residuals do not share the same second moments when the null hypothesis is false, which makes them difficult to use in the setting of multiple testing. An alternative approach is to resample standardized residuals, data centered by group sample means and standardized by group sample covariance matrices. This approach, however, has been observed to inflate type I error when sample size is small or data are generated from heavy-tailed distributions. We propose to improve this approach by using robust estimation for the first and second moments. We discuss two statistics: the Bartlett statistic and a statistic based on eigen-decomposition of sample covariance matrices. Both statistics can be expressed in terms of standardized errors under the null hypothesis. These methods are extended to test homogeneity in correlation matrices. Using simulation studies, we demonstrate that the robust resampling approach provides comparable or superior performance, relative to traditional approaches, for single testing and reasonable performance for multiple testing. The proposed methods are applied to data collected in an HIV vaccine trial to investigate possible determinants, including vaccine status, vaccine-induced immune response level and viral genotype, of unusual correlation pattern between HIV viral load and CD4 count in newly infected patients.

Metagenome enrichment approach used for selection of oil-degrading bacteria consortia for drill cutting residue bioremediation.

PubMed

Guerra, Alaine B; Oliveira, Jorge S; Silva-Portela, Rita C B; Araújo, Wydemberg; Carlos, Aline C; Vasconcelos, Ana Tereza R; Freitas, Ana Teresa; Domingos, Yldeney Silva; de Farias, Mirna Ferreira; Fernandes, Glauber José Turolla; Agnez-Lima, Lucymara F

2018-04-01

Drill cuttings leave behind thousands of tons of residues without adequate treatment, generating a large environmental liability. Therefore knowledge about the microbial community of drilling residue may be useful for developing bioremediation strategies. In this work, samples of drilling residue were enriched in different culture media in the presence of petroleum, aiming to select potentially oil-degrading bacteria and biosurfactant producers. Total DNA was extracted directly from the drill cutting samples and from two enriched consortia and sequenced using the Ion Torrent platform. Taxonomic analysis revealed the predominance of Proteobacteria in the metagenome from the drill cuttings, while Firmicutes was enriched in consortia samples. Functional analysis using the Biosurfactants and Biodegradation Database (BioSurfDB) revealed a similar pattern among the three samples regarding hydrocarbon degradation and biosurfactants production pathways. However, some statistical differences were observed between samples. Namely, the pathways related to the degradation of fatty acids, chloroalkanes, and chloroalkanes were enriched in consortia samples. The degradation colorimetric assay using dichlorophenolindophenol as an indicator was positive for several hydrocarbon substrates. The consortia were also able to produce biosurfactants, with biosynthesis of iturin, lichnysin, and surfactin among the more abundant pathways. A microcosms assay followed by gas chromatography analysis showed the efficacy of the consortia in degrading alkanes, as we observed a reduction of around 66% and 30% for each consortium in total alkanes. These data suggest the potential use of these consortia in the bioremediation of drilling residue based on autochthonous bioaugmentation. Copyright © 2018 Elsevier Ltd. All rights reserved.

Modeling the Residual Stresses in Reactive Resins-Based Materials: a Case Study of Photo-Sensitive Composites for Dental Applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Grassia, Luigi; D'Amore, Alberto

Residual stresses in reactive resins-based composites are associated to the net volumetric contraction (shrinkage) arising during the cross-linking reactions. Depending on the restoration geometry (the ratio of the free surface area to the volume of the cavity) the frozen-in stresses can be as high as the strength of the dental composites. This is the main reason why the effectiveness and then the durability of restorations with composites remains quite lower than those realized with metal alloys based materials. In this paper we first explore the possibility to circumvent the mathematical complexity arising from the determination of residual stresses in reactivemore » systems three-dimensionally constrained. Then, the results of our modeling approach are applied to a series of commercially available composites showing that almost all samples develop residual stresses such that the restoration undergoes failure as soon as it is realized.« less

Burst Ductility of Zirconium Clads: The Defining Role of Residual Stress

NASA Astrophysics Data System (ADS)

Kumar, Gulshan; Kanjarla, A. K.; Lodh, Arijit; Singh, Jaiveer; Singh, Ramesh; Srivastava, D.; Dey, G. K.; Saibaba, N.; Doherty, R. D.; Samajdar, Indradev

2016-08-01

Closed end burst tests, using room temperature water as pressurizing medium, were performed on a number of industrially produced zirconium (Zr) clads. A total of 31 samples were selected based on observed differences in burst ductility. The latter was represented as total circumferential elongation or TCE. The selected samples, with a range of TCE values (5 to 35 pct), did not show any correlation with mechanical properties along axial direction, microstructural parameters, crystallographic textures, and outer tube-surface normal ( σ 11) and shear ( τ 13) components of the residual stress matrix. TCEs, however, had a clear correlation with hydrostatic residual stress ( P h), as estimated from tri-axial stress analysis on the outer tube surface. Estimated P h also scaled with measured normal stress ( σ 33) at the tube cross section. An elastic-plastic finite element model with ductile damage failure criterion was developed to understand the burst mechanism of zirconium clads. Experimentally measured P h gradients were imposed on a solid element continuum finite element (FE) simulation to mimic the residual stresses present prior to pressurization. Trends in experimental TCEs were also brought out with computationally efficient shell element-based FE simulations imposing the outer tube-surface P h values. Suitable components of the residual stress matrix thus determined the burst performance of the Zr clads.

Risk-based approach to developing a national residue sampling plan for testing under European Union regulation for veterinary medicinal products and coccidiostat feed additives in domestic animal production.

PubMed

Danaher, Martin; Shanahan, Conor; Butler, Francis; Evans, Rhodri; O'Sullivan, Dan; Glynn, Denise; Camon, Tim; Lawlor, Peadar; O'Keeffe, Michael

2016-07-01

A ranking system for veterinary medicinal products and coccidiostat feed additives has been developed as a tool to be applied in a risk-based approach to the residue testing programme for foods of animal origin in the Irish National Residue Control Plan (NRCP). Three characteristics of substances that may occur as residues in food are included in the developed risk ranking system: Potency, as measured by the acceptable daily intake assigned by the European Medicines Agency Committee for Medicinal Products for Veterinary Use, to each substance; Usage, as measured by the three factors of Number of Doses, use on Individual animals or for Group treatment, and Withdrawal Period; and Residue Occurrence, as measured by the number of Non-Compliant Samples in the NRCP. For both Number of Doses and Non-Compliant Samples, data for the 5-year period 2008-12 have been used. The risk ranking system for substances was developed for beef cattle, sheep and goats, pigs, chickens and dairy cattle using a scoring system applied to the various parameters described above to give an overall score based on the following equation: Potency × Usage (Number of Doses + Individual/Group Use + Withdrawal Period) × Residue Occurrence. Applying this risk ranking system, the following substances are ranked very highly: antimicrobials such as amoxicillin (for all species except pigs), marbofloxacillin (for beef cattle), oxytetracycline (for all species except chickens), sulfadiazine with trimethoprim (for pigs and chickens) and tilmicosin (for chickens); antiparasitic drugs, such as the benzimidazoles triclabendazole (for beef and dairy cattle), fenbendazole/oxfendazole (for sheep/goats and dairy cattle) and albendazole (for dairy cattle), the avermectin ivermectin (for beef cattle), and anti-fluke drugs closantel and rafoxanide (for sheep/goats); the anticoccidials monensin, narasin, nicarbazin and toltrazuril (for chickens). The risk ranking system described is a relatively simple system designed to provide a reliable basis for selecting the veterinary medicinal products and coccidiostat feed additives that might be prioritised for residue testing.

A survey of organochlorine pesticide residues in cheese samples from three Mexican regions.

PubMed

Albert, L A; Alpuche, L; Bárcenas, C; Rendón, J

1990-01-01

Organochlorine pesticide residues were determined in cheese samples from three Mexican regions. All samples were found to be contaminated by these residues: p,p'-DDE was present in 100% of the samples. Other pesticides found with high frequencies were HCB, three of the BHC isomers, as well as heptachlor and its epoxide. Also found, although less frequently, were residues of p,p'-DDD, p,p'-DDT, aldrin, dieldrin and endrin. Samples from the region known as Comarca Lagunera had the highest number of pesticides per sample. The highest concentrations of residues were found in cheese samples from the Soconusco and the Comarca Lagunera regions.

Risk assessment for children exposed to DDT residues in various milk types from the Greek market.

PubMed

Tsakiris, Ioannis N; Goumenou, Marina; Tzatzarakis, Manolis N; Alegakis, Athanasios K; Tsitsimpikou, Christina; Ozcagli, Eren; Vynias, Dionysios; Tsatsakis, Aristidis M

2015-01-01

The occurrence of residues of DDT and its metabolites was monitored in 196 cow milk samples of various pasteurized commercial types collected from the Greek market. Residue levels were determined by GC-MS analysis. In 97.4% of the samples at least one DDT isomer or one of the DDT metabolites was detected, in levels not exceeding the maximum permitted residue level by the EU. Hazard Index for both carcinogenic and non-carcinogenic effects was estimated under two assumptions: a) using DDT concentrations from positive samples and b) imputing LOD/2 as an arbitrary concentration for negative samples. No statistically significant differences in detected or summed residue (p > 0.05) concentrations between different milk types were observed, with the exception of specific metabolites of DDT in some milk types. Exposure assessment scenarios were developed for children aged 1, 3, 5, 7 and 12 years old based on estimated body weights and daily milk consumption. Hazard Indices for non-carcinogenic effects were below 0.109 covering also carcinogenic effects according to WHO approach. The cancer risk values for carcinogenic effects according to the US EPA Cancer Benchmark Concentration approach, ranged from 0.4 to 18. For both effects the highest values were calculated for the 1- to 3-year-old age groups. Copyright © 2014 Elsevier Ltd. All rights reserved.

Monitoring and exposure assessment of pesticide residues in cowpea (Vigna unguiculata L. Walp) from five provinces of southern China.

PubMed

Huan, Zhibo; Xu, Zhi; Luo, Jinhui; Xie, Defang

2016-11-01

Residues of 14 pesticides were determined in 150 cowpea samples collected in five southern Chinese provinces in 2013 and 2014.70% samples were detected one or more residues. 61.3% samples were illegal mainly because of detection of unauthorized pesticides. 14.0% samples contained more than three pesticides. Deterministic and probabilistic methods were used to assess the chronic and acute risk of pesticides in cowpea to eight subgroups of people. Deterministic assessment showed that the estimated short-term intakes (ESTIs) of carbofuran were 1199.4%-2621.9% of the acute reference doses (ARfD) while the rates were 985.9%-4114.7% using probabilistic assessment. Probabilistic assessment showed 4.2%-7.8% subjects may suffer from unacceptable acute risk from carbofuran contaminated cowpeas from the five provinces (especially children). But undue concern is not necessary, because all the estimations are based on conservative assumption. Copyright © 2016 Elsevier Inc. All rights reserved.

Occurrence and estimation of pesticide residues in edible minor crops in southeastern Poland in 2013-2014.

PubMed

Podbielska, Magdalena; Szpyrka, Ewa; Matyaszek, Aneta; Słowik-Borowiec, Magdalena; Rupar, Julian; Kurdziel, Anna

2016-07-01

This paper presents the results of official control of pesticide residues in minor crops collected in southeastern Poland in 2013-2014. Compliance of used pesticides with applicable law was also verified, and determined residues were compared to maximum residue levels (MRLs) provided for in Regulation (EC) No. 395/2005. A total of 583 samples of 25 different types of fresh fruit and vegetables were analyzed for pesticide residues. Pesticide residues were detected in 158 samples (27.1 % of the analyzed samples). According to the European Commission Health & Consumer Protection Directorate-General (SANCO) guidelines document, MRL violations were understood as cases where a residue level exceeded the MRL after the uncertainty of the method (50 %) was considered. MRL violations were found in four samples. The usage of unauthorized pesticides was detected in 5.8 % of analyzed samples. Substances banned in Poland were found in two samples. Fungicides were the most frequently detected group of pesticides. Pesticide residues were most commonly found in fruit samples (19.4 % of all analyzed samples), mainly in gooseberry, redcurrant, and huckleberry. The majority of samples were compliant with MRLs, which means that they were suitable for trade.

Quantitative analysis of fungicide azoxystrobin in agricultural samples with rapid, simple and reliable monoclonal immunoassay.

PubMed

Watanabe, Eiki; Miyake, Shiro

2013-01-15

This work presents analytical performance of a kit-based direct competitive enzyme-linked immunosorbent assay (dc-ELISA) for azoxystrobin detection in agricultural products. The dc-ELISA was sufficiently sensitive for analysis of residue levels close to the maximum residue limits. The dc-ELISA did not show cross-reactivity to other strobilurin analogues. Absorbance decreased with the increase of methanol concentration in sample solution from 2% to 40%, while the standard curve became most linear when the sample solution contained 10% methanol. Agricultural samples were extracted with methanol, and the extracts were diluted with water to 10% methanol adequate. No significant matrix interference was observed. Satisfying recovery was found for all of spiked samples and the results were well agreed with the analysis with liquid chromatography. These results clearly indicate that the kit-based dc-ELISA is suitable for the rapid, simple, quantitative and reliable determination of the fungicide. Copyright © 2012 Elsevier Ltd. All rights reserved.

Improving regression-model-based streamwater constituent load estimates derived from serially correlated data

USGS Publications Warehouse

Aulenbach, Brent T.

2013-01-01

A regression-model based approach is a commonly used, efficient method for estimating streamwater constituent load when there is a relationship between streamwater constituent concentration and continuous variables such as streamwater discharge, season and time. A subsetting experiment using a 30-year dataset of daily suspended sediment observations from the Mississippi River at Thebes, Illinois, was performed to determine optimal sampling frequency, model calibration period length, and regression model methodology, as well as to determine the effect of serial correlation of model residuals on load estimate precision. Two regression-based methods were used to estimate streamwater loads, the Adjusted Maximum Likelihood Estimator (AMLE), and the composite method, a hybrid load estimation approach. While both methods accurately and precisely estimated loads at the model’s calibration period time scale, precisions were progressively worse at shorter reporting periods, from annually to monthly. Serial correlation in model residuals resulted in observed AMLE precision to be significantly worse than the model calculated standard errors of prediction. The composite method effectively improved upon AMLE loads for shorter reporting periods, but required a sampling interval of at least 15-days or shorter, when the serial correlations in the observed load residuals were greater than 0.15. AMLE precision was better at shorter sampling intervals and when using the shortest model calibration periods, such that the regression models better fit the temporal changes in the concentration–discharge relationship. The models with the largest errors typically had poor high flow sampling coverage resulting in unrepresentative models. Increasing sampling frequency and/or targeted high flow sampling are more efficient approaches to ensure sufficient sampling and to avoid poorly performing models, than increasing calibration period length.

Pesticide residues determination in Polish organic crops in 2007-2010 applying gas chromatography-tandem quadrupole mass spectrometry.

PubMed

Walorczyk, Stanisław; Drożdżyński, Dariusz; Kowalska, Jolanta; Remlein-Starosta, Dorota; Ziółkowski, Andrzej; Przewoźniak, Monika; Gnusowski, Bogusław

2013-08-15

A sensitive, accurate and reliable multiresidue method based on the application of gas chromatography-tandem quadrupole mass spectrometry (GC-QqQ-MS/MS) has been established for screening, identification and quantification of a large number of pesticide residues in produce. The method was accredited in compliance with PN-EN ISO/IEC 17025:2005 standard and it was operated under flexible scope as PB-11 method. The flexible scope of accreditation allowed for minor modifications and extension of the analytical scope while using the same analytical technique. During the years 2007-2010, the method was used for the purpose of verification of organic crop production by multiresidue analysis for the presence of pesticides. A total of 528 samples of differing matrices such as fruits, vegetables, cereals, plant leaves and other green parts were analysed, of which 4.4% samples contained pesticide residues above the threshold value of 0.01 mg/kg. A total of 20 different pesticide residues were determined in the samples. Copyright © 2013 Elsevier Ltd. All rights reserved.

Design of a novel noninvasive spectrometer for pesticide residues monitor

NASA Astrophysics Data System (ADS)

Ren, Zhong; Liu, Guodong; Huang, Zhen

2014-11-01

Although the gas or liquid chromatography had been widely used into pesticide residues monitoring, some drawbacks such as time-consuming, complicated operation and especially the destructivity for samples were existed. To overcome the limits of destructive detection methods, the noninvasive detection method based on spectroscopy was used to detect the pesticide residues in this paper. To overcome low resolution and light-efficiency due to the drawbacks of the classical plane and holography concave gratings, a novel noninvasive spectrometer for pesticide residues monitor (PRM) based on volume holography transmission (VHT) grating was designed. Meanwhile, a custom-built splitting light system for PRM based on the VHT grating was developed. In addition, the linear charge coupled device (CCD) with combined data acquisition (DAQ) card and the virtual-PRM based on LabVIEW were respectively used as the spectral acquisition hardware and software-platform. Experimental results showed that the spectral resolution of this spectrometer reached 2nm, and the VHT grating's diffraction efficiency was gotten via the simulation experiment.

Validation of cystatin C-based equations for evaluating residual renal function in patients on continuous ambulatory peritoneal dialysis.

PubMed

Zhong, Hui; Zhang, Wei; Qin, Min; Gou, ZhongPing; Feng, Ping

2017-06-01

Residual renal function needs to be assessed frequently in patients on continuous ambulatory peritoneal dialysis (CAPD). A commonly used method is to measure creatinine (Cr) and urea clearance in urine collected over 24 h, but collection can be cumbersome and difficult to manage. A faster, simpler alternative is to measure levels of cystatin C (CysC) in serum, but the accuracy and reliability of this method is controversial. Our study aims to validate published CysC-based equations for estimating residual renal function in patients on CAPD. Residual renal function was measured by calculating average clearance of urea and Cr in 24-h urine as well as by applying CysC- or Cr-based equations published by Hoek and Yang. We then compared the performance of the equations against the 24-h urine results. In our sample of 255 patients ages 47.9 ± 15.6 years, the serum CysC level was 6.43 ± 1.13 mg/L. Serum CysC level was not significantly associated with age, gender, height, weight, body mass index, hemoglobin, intact parathyroid hormone, normalized protein catabolic rate or the presence of diabetes. In contrast, serum CysC levels did correlate with peritoneal clearance of CysC and with levels of prealbumin and high-sensitivity C-reactive protein. Residual renal function was 2.56 ± 2.07 mL/min/1.73 m 2 based on 24-h urine sampling, compared with estimates (mL/min/1.73 m 2 ) of 2.98 ± 0.66 for Hoek's equation, 2.03 ± 0.97 for Yang's CysC-based equation and 2.70 ± 1.30 for Yang's Cr-based equation. Accuracies within 30%/50% of measured residual renal function for the three equations were 29.02/48.24, 34.90/56.86 and 31.37/54.90. The three equations for estimating residual renal function showed similar limits of agreement and differed significantly from the measured value. Published CysC-based equations do not appear to be particularly reliable for patients on CAPD. Further development and validation of CysC-based equations should take into account peritoneal clearance of CysC and other relevant factors. © The Author 2016. Published by Oxford University Press on behalf of ERA-EDTA. All rights reserved.

Numerical simulation of residual stress in laser based additive manufacturing process

NASA Astrophysics Data System (ADS)

Kalyan Panda, Bibhu; Sahoo, Seshadev

2018-03-01

Minimizing the residual stress build-up in metal-based additive manufacturing plays a pivotal role in selecting a particular material and technique for making an industrial part. In beam-based additive manufacturing, although a great deal of effort has been made to minimize the residual stresses, it is still elusive how to do so by simply optimizing the processing parameters, such as beam size, beam power, and scan speed. Amid different types of additive manufacturing processes, Direct Metal Laser Sintering (DMLS) process uses a high-power laser to melt and sinter layers of metal powder. The rapid solidification and heat transfer on powder bed endows a high cooling rate which leads to the build-up of residual stresses, that will affect the mechanical properties of the build parts. In the present work, the authors develop a numerical thermo-mechanical model for the measurement of residual stress in the AlSi10Mg build samples by using finite element method. Transient temperature distribution in the powder bed was assessed using the coupled thermal to structural model. Subsequently, the residual stresses were estimated with varying laser power. From the simulation result, it found that the melt pool dimensions increase with increasing the laser power and the magnitude of residual stresses in the built part increases.

Monitoring of Pesticide Residues in Commonly Used Fruits and Vegetables in Kuwait.

PubMed

Jallow, Mustapha F A; Awadh, Dawood G; Albaho, Mohammed S; Devi, Vimala Y; Ahmad, Nisar

2017-07-25

The presence of pesticide residues in primary and derived agricultural products raises serious health concerns for consumers. The aim of this study was to assess the level of pesticide residues in commonly consumed fruits and vegetables in Kuwait. A total of 150 samples of different fresh vegetables and fruits were analyzed for the presence of 34 pesticides using the quick easy cheap effective rugged and safe (QuEChERS) multi-residue extraction, followed by gas chromatography-mass spectrometry (GC-MS) or liquid chromatography-tandem mass spectrometry (LC - MS / MS). Pesticide residues above the maximum residue limits (MRL) were detected in 21% of the samples and 79% of the samples had no residues of the pesticides surveyed or contained residues below the MRL. Multiple residues were present in 40% of the samples with two to four pesticides, and four samples were contaminated with more than four pesticide residues. Of the pesticides investigated, 16 were detected, of which imidacloprid, deltamethrin, cypermethrin, malathion, acetamiprid, monocrotophos, chlorpyrifos-methyl, and diazinon exceeded their MRLs. Aldrin, an organochlorine pesticide, was detected in one apple sample, with residues below the MRL. The results indicate the occurrence of pesticide residues in commonly consumed fruits and vegetables in Kuwait, and pointed to an urgent need to develop comprehensive intervention measures to reduce the potential health risk to consumers. The need for the regular monitoring of pesticide residues and the sensitization of farmers to better pesticide safety practices, especially the need to adhere to recommended pre-harvest intervals is recommended.

30 CFR 1206.174 - How do I value gas production when an index-based method cannot be used?

Code of Federal Regulations, 2011 CFR

2011-07-01

... dispositions of like-quality gas in the same field (or, if necessary to obtain a reasonable sample, from the..., quality of gas, residue gas, or gas plant products, volume, and such other factors as may be appropriate... consideration of other information relevant in valuing like-quality gas, residue gas, or gas plant products...

Optical instrument development for detection of pesticide residue in apple surface

NASA Astrophysics Data System (ADS)

Dhakal, Sagar; Li, Yongyu; Peng, Yankun; Chao, Kuanglin; Qin, Jianwei

2013-05-01

Apple is the world largest produced and consumed fruit item. At the same time, apple ranks number one among the fruit item contaminated with pesticide. This research focuses on development of laboratory based self-developed software and hardware for detection of commercially available organophosphorous pesticide (chlorpyrifos) in apple surface. A laser light source of 785nm was used to excite the sample, and Raman spectroscopy assembled with CCD camera was used for optical data acquisition. A hardware system was designed and fabricated to clamp and rotate apple sample of varying size maintaining constant working distance between optical probe and sample surface. Graphical Users Interface (GUI) based on LabView platform was developed to control the hardware system. The GUI was used to control the Raman system including CCD temperature, exposure time, track height and track centre, data acquisition, data processing and result prediction. Different concentrations of commercially available 48% chlorpyrifos pesticide solutions were prepared and gently placed in apple surface and dried. Raman spectral data at different points from same apple along the equatorial region were then acquired. The results show that prominent peaks at 341cm-1, 632cm-1 and 680 cm-1 represent the pesticide residue. The laboratory based experiment was able to detect pesticide solution of 20ppm within 3 seconds. A linear relation between Raman intensity and pesticide residue was developed with accuracy of 97.8%. The result of the research is promising and thus is a milestone for developing industrially desired real time, non-invasive pesticide residue detection technology in future.

Residual Agar Determination in Bacterial Spores by Electrospray Ionization Mass Spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wahl, Karen L.; Colburn, Heather A.; Wunschel, David S.

2010-02-15

Presented here is an analytical method to detect residual agar from a bacterial spore sample as an indication of culturing on an agar plate. This method is based on the resolubilization of agar polysaccharide from a bacterial spore sample, enzymatic digestion, followed by electrospray ionization tandem mass spectrometry (ESI-MSn) analysis for detection of a specific agar fragment ion. A range of Bacillus species and strains were selected to demonstrate the effectiveness of this approach. The characteristic agar fragment ion was detected in the spores grown on agar that were washed from 1 to 5 times, irradiated or non-irradiated and notmore » in the spores grown in broth. A sample containing approximately 108 spores is currently needed for confident detection of residual agar from culture on agar plates in the presence of bacterial spores with a limit of detection of approximately 1 ppm agar spiked into a broth-grown spore sample. The results of a proficiency test with 42 blinded samples are presented demonstrating the utility of this method with no false positives and only 3 false negatives for samples that were below the detection level of the method as documented.« less

Autoclave sterilization of instruments used on women with cervical neoplasia is an effective method of eradicating residual human papillomavirus DNA: a polymerase chain reaction-based evaluation.

PubMed

Estes, Jacob M; Kirby, Tyler O; Huh, Warner K

2007-01-01

To determine whether autoclave sterilization eradicates human papillomavirus (HPV) DNA on specula and instruments used to treat women with cervical neoplasia. Specula and instruments used in two referral colposcopy clinics were evaluated to determine the PGMY9/11 primer system's ability to amplify residual HPV DNA. Each speculum and instrument was sampled with a Dacron swab and stored in PreservCyt solution (Cytyc Corporation, Marlborough, MA) at 4 degrees C. DNA amplification was performed under standard conditions with appropriate controls followed by HPV typing using the reverse line blot test (Roche Molecular Systems, Alameda, CA). Once validated, the same polymerase chain reaction method was used on autoclave-sterilized specula and biopsy instruments and heated glass bead- and Cidex bath (Johnson & Johnson, New Brunswick, NJ)-sterilized instruments. All results, with appropriate positive and negative controls, were confirmed in triplicate. A total of 140 instruments (70 used and 70 autoclaved) were sampled for residual HPV DNA. Five samples in the contaminated specula arm were excluded from analysis secondary to insufficient sampling. Of the remaining samples, 52.3% (34/65) of contaminated instruments-both specula and biopsy instruments-had detectable HPV DNA. Fifty-five percent of contaminated biopsy instruments (11/20) were positive and 51.1% of contaminated specula (23/45) were positive. All 70 autoclaved samples (50 specula and 20 biopsy instruments) were negative for residual HPV DNA or beta-globin. One instrument in the glass bead and Cidex group that was presumed sterile was positive for HPV 16 DNA. The PGMY9/11 primer system is an effective method to detect residual HPV DNA. Autoclave sterilization appears to eradicate HPV DNA to levels undetectable with this sensitive assay, whereas heated glass beads followed by Cidex bath appears to be inadequate methods. These results suggest that autoclave sterilization is effective when using nondisposable instruments and should be the method of choice in studies using polymerase chain reaction-based amplification of HPV DNA.

Residual stress profiles in veneering ceramic on Y-TZP, alumina and ZTA frameworks: measurement by hole-drilling.

PubMed

Fukushima, K A; Sadoun, M J; Cesar, P F; Mainjot, A K

2014-02-01

The residual stress profile developed within the veneering ceramic during the manufacturing process is an important predicting factor in chipping failures, which constitute a well-known problem with yttria-tetragonal-zirconia polycrystal (Y-TZP) based restorations. The objectives of this study are to measure and to compare the residual stress profile in the veneering ceramic layered on three different polycrystalline ceramic framework materials: Y-TZP, alumina polycrystal (AL) and zirconia toughened alumina (ZTA). The stress profile was measured with the hole-drilling method in bilayered disk samples of 19 mm diameter with a 0.7 mm thick Y-TZP, AL or ZTA framework and a 1.5mm thick layer of the corresponding veneering ceramic. The AL samples exhibited increasing compressive stresses with depth, while compressive stresses switching into interior tensile stresses were measured in Y-TZP samples. ZTA samples exhibited compressive stress at the ceramic surface, decreasing with depth up to 0.6mm from the surface, and then becoming compressive again near the framework. Y-TZP samples exhibited a less favorable stress profile than those of AL and ZTA samples. Results support the hypothesis of the occurrence of structural changes within the Y-TZP surface in contact with the veneering ceramic to explain the presence of tensile stresses. Even if the presence of Y-TZP in the alumina matrix seems to negatively affect the residual stress profiles in ZTA samples in comparison with AL samples, the registered profiles remain positive in terms of veneer fracture resistance. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Determination of residual monomers resulting from the chemical polymerization process of dental materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Boboia, S.; Moldovan, M.; Ardelean, I.

The residual monomer present in post-polymerized dental materials encourages premature degradation of the reconstructed tooth. That is why the residual monomer should be quantified in a simple, fast, accurate and reproducible manner. In our work we propose such an approach for accurate determination of the residual monomer in dental materials which is based on low-field nuclear magnetic resonance (NMR) relaxometry. The results of the NMR approach are compared with those of the high performance liquid chromatography (HPLC) technique. The samples under study contain the main monomers (2,2-bis[4-(2-hydroxy-3-methacryloyloxypropoxy)phenyl]propane and triethylene glycol dimethacrylate) constituting the liquid phase of most dental materials andmore » an initiator. Two samples were analyzed with different ratios of chemical initiation systems: N,N-dimethyl-p-toluide: benzoyl peroxide (1:2 and 0.7:1.2). The results obtained by both techniques highlight that by reducing the initiator the polymerization process slows down and the amount of residual monomer reduces. This prevents the premature degradation of the dental fillings and consequently the reduction of the biomaterial resistance.« less

The topomer-sampling model of protein folding

PubMed Central

Debe, Derek A.; Carlson, Matt J.; Goddard, William A.

1999-01-01

Clearly, a protein cannot sample all of its conformations (e.g., ≈3100 ≈ 1048 for a 100 residue protein) on an in vivo folding timescale (<1 s). To investigate how the conformational dynamics of a protein can accommodate subsecond folding time scales, we introduce the concept of the native topomer, which is the set of all structures similar to the native structure (obtainable from the native structure through local backbone coordinate transformations that do not disrupt the covalent bonding of the peptide backbone). We have developed a computational procedure for estimating the number of distinct topomers required to span all conformations (compact and semicompact) for a polypeptide of a given length. For 100 residues, we find ≈3 × 107 distinct topomers. Based on the distance calculated between different topomers, we estimate that a 100-residue polypeptide diffusively samples one topomer every ≈3 ns. Hence, a 100-residue protein can find its native topomer by random sampling in just ≈100 ms. These results suggest that subsecond folding of modest-sized, single-domain proteins can be accomplished by a two-stage process of (i) topomer diffusion: random, diffusive sampling of the 3 × 107 distinct topomers to find the native topomer (≈0.1 s), followed by (ii) intratopomer ordering: nonrandom, local conformational rearrangements within the native topomer to settle into the precise native state. PMID:10077555

Organochlorine and organophosphorus pesticide residues in fodder and milk samples along Musi river belt, India.

PubMed

Kotinagu, Korrapati; Krishnaiah, Nelapati

2015-04-01

The present study was conducted to find the organochlorine pesticide (OCP) and organophosphorus pesticide (OPP) residues in fodder and milk samples along Musi river belt, India. Fodder and milk samples collected from the six zones of Musi river belt, Hyderabad India were analyzed by gas chromatography with electron capture detector for OCP residues and pulsated flame photometric detector for the presence of OPP residues. The gas chromatographic analysis of fodder samples of Zone 5 of Musi river showed the residues of dicofol at concentration of 0.07±0.0007 (0.071-0.077). Among organophosphorus compounds, dimetheoate was present in milk samples collected from Zone 6 at a level of 0.13±0.006 (0.111-0.167). The residues of OCPs, OPPs and cyclodies were below the detection limit in the remaining fodder and milk samples collected from Musi river belt in the present study. The results indicate that the pesticide residues in fodder and milk samples were well below the maximum residue level (MRL) values, whereas dicofol in fodder and dimethoate in milk were slightly above the MRL values specified by EU and CODEX.

Organochlorine and organophosphorus pesticide residues in fodder and milk samples along Musi river belt, India

PubMed Central

Kotinagu, Korrapati; Krishnaiah, Nelapati

2015-01-01

Aim: The present study was conducted to find the organochlorine pesticide (OCP) and organophosphorus pesticide (OPP) residues in fodder and milk samples along Musi river belt, India. Materials and Methods: Fodder and milk samples collected from the six zones of Musi river belt, Hyderabad India were analyzed by gas chromatography with electron capture detector for OCP residues and pulsated flame photometric detector for the presence of OPP residues. Results: The gas chromatographic analysis of fodder samples of Zone 5 of Musi river showed the residues of dicofol at concentration of 0.07±0.0007 (0.071-0.077). Among organophosphorus compounds, dimetheoate was present in milk samples collected from Zone 6 at a level of 0.13±0.006 (0.111-0.167). The residues of OCPs, OPPs and cyclodies were below the detection limit in the remaining fodder and milk samples collected from Musi river belt in the present study. Conclusion: The results indicate that the pesticide residues in fodder and milk samples were well below the maximum residue level (MRL) values, whereas dicofol in fodder and dimethoate in milk were slightly above the MRL values specified by EU and CODEX. PMID:27047132

Accurate determination of residual acrylic acid in superabsorbent polymer of hygiene products by headspace gas chromatography.

PubMed

Zhang, Shu-Xin; Chai, Xin-Sheng; Jiang, Ran

2017-02-17

This work reports on a method for the determination of residual acrylic acid (AA) in the superabsorbent polymers for hygiene products by headspace analysis. It was based on water extraction for the polymer sample at a room temperature for 50min. Then, the AA in the extractant reacted with bicarbonate solution in a closed headspace sample vial, from which the carbon dioxide generated from the reaction (within 20min at 70°C) was detected by gas chromatography (GC). It was found that there is adsorption partition equilibrium of AA between solid-liquid phases. Therefore, an equation for calculating the total AA content in the original polymers sample was derived based on the above phase equilibrium. The results show that the HS-GC method has good precision (RSD<2.51%) and good accuracy (recoveries from 93 to 105%); the limit of quantification (LOQ) was 373mg/kg. The present method is rapid, accurate, and suitable for determining total residual acrylic acid in a wide variety of applications from processing of superabsorbent polymer to commercial products quality control. Copyright © 2017 Elsevier B.V. All rights reserved.

New Trends in Pesticide Residue Analysis in Cereals, Nutraceuticals, Baby Foods, and Related Processed Consumer Products.

PubMed

Raina-Fulton, Renata

2015-01-01

Pesticide residue methods have been developed for a wide variety of food products including cereal-based foods, nutraceuticals and related plant products, and baby foods. These cereal, fruit, vegetable, and plant-based products provide the basis for many processed consumer products. For cereal and nutraceuticals, which are dry sample products, a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method has been used with additional steps to allow wetting of the dry sample matrix and subsequent cleanup using dispersive or cartridge format SPE to reduce matrix effects. More processed foods may have lower pesticide concentrations but higher co-extracts that can lead to signal suppression or enhancement with MS detection. For complex matrixes, GC/MS/MS or LC/electrospray ionization (positive or negative ion)-MS/MS is more frequently used. The extraction and cleanup methods vary with different sample types particularly for cereal-based products, and these different approaches are discussed in this review. General instrument considerations are also discussed.

Analysis of sulfonamides, tilmicosin and avermectins residues in typical animal matrices with multi-plug filtration cleanup by liquid chromatography-tandem mass spectrometry detection.

PubMed

Qin, Yuhong; Jatamunua, Freedom; Zhang, Jingru; Li, Yanjie; Han, Yongtao; Zou, Nan; Shan, Jihao; Jiang, Yanbin; Pan, Canping

2017-05-15

The frequent use of various veterinary drugs could lead to residue bioaccumulation in animal tissues, which could cause dietary risks to human health. In order to quickly analyze the residues, a liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for detecting Sulfonamides, Tilmicosin and Avermectins (AVMs) residues in animal samples. For sample preparation, modified QuEChERS (quick, easy, cheap, effective, rugged and safe) and ultrasound-assisted extraction (UAE) methods were used. For sample cleanup, n-Hexane delipidation and multi-plug filtration cleanup (m-PFC) method based on primary-secondary amine (PSA) and octadecyl-silica (C18) were used, followed by LC-MS/MS analysis. It was validated on 7 animal matrices (bovine, caprine, swine meat and their kidneys, milk) at two fortified concentration levels of 5 and 100μg/kg. The recoveries ranged from 82 to 107% for all analytes with relative standard deviations (RSDs) less than 15%. Matrix-matched calibrations were performed with coefficients of determination above 0.998 for all analytes within concentration levels of 5-500μg/kg. The developed method was successfully used to analysis veterinary drugs of real animal samples from local markets. Copyright © 2017 Elsevier B.V. All rights reserved.

Discrimination of biological and chemical threat simulants in residue mixtures on multiple substrates.

PubMed

Gottfried, Jennifer L

2011-07-01

The potential of laser-induced breakdown spectroscopy (LIBS) to discriminate biological and chemical threat simulant residues prepared on multiple substrates and in the presence of interferents has been explored. The simulant samples tested include Bacillus atrophaeus spores, Escherichia coli, MS-2 bacteriophage, α-hemolysin from Staphylococcus aureus, 2-chloroethyl ethyl sulfide, and dimethyl methylphosphonate. The residue samples were prepared on polycarbonate, stainless steel and aluminum foil substrates by Battelle Eastern Science and Technology Center. LIBS spectra were collected by Battelle on a portable LIBS instrument developed by A3 Technologies. This paper presents the chemometric analysis of the LIBS spectra using partial least-squares discriminant analysis (PLS-DA). The performance of PLS-DA models developed based on the full LIBS spectra, and selected emission intensities and ratios have been compared. The full-spectra models generally provided better classification results based on the inclusion of substrate emission features; however, the intensity/ratio models were able to correctly identify more types of simulant residues in the presence of interferents. The fusion of the two types of PLS-DA models resulted in a significant improvement in classification performance for models built using multiple substrates. In addition to identifying the major components of residue mixtures, minor components such as growth media and solvents can be identified with an appropriately designed PLS-DA model.

RECOMMENDATIONS FOR SAMPLING OF TANK 18 IN F TANK FARM

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shine, G.

2009-12-14

Representative sampling is required for characterization of the residual floor material in Tank 18 prior to operational closure. Tank 18 is an 85-foot diameter, 34-foot high carbon steel tank with nominal operating volume of 1,300,000 gallons. It is a Type IV tank, and has been in service storing radioactive materials since 1959. Recent mechanical cleaning of the tank removed all mounds of material. Anticipating a low level of solids in the residual material, Huff and Thaxton [2009] developed a plan to sample the material during the final clean-up process while it would still be resident in sufficient quantities to supportmore » analytical determinations in four quadrants of the tank. Execution of the plan produced fewer solids than expected to support analytical determinations in all four quadrants. Huff and Thaxton [2009] then restructured the plan to characterize the residual floor material separately in the North and the South regions: two 'hemispheres.' This document provides sampling recommendations to complete the characterization of the residual material on the tank bottom following the guidance in Huff and Thaxton [2009] to split the tank floor into a North and a South hemisphere. The number of samples is determined from a modification of the formula previously published in Edwards [2001] and the sample characterization data for previous sampling of Tank 18 described by Oji [2009]. The uncertainty is quantified by an upper 95% confidence limit (UCL95%) on each analyte's mean concentration in Tank 18. The procedure computes the uncertainty in analyte concentration as a function of the number of samples, and the final number of samples is determined when the reduction in the uncertainty from an additional sample no longer has a practical impact on results. The characterization of the full suite of analytes in the North hemisphere is currently supported by a single Mantis rover sample obtained from a compact region near the center riser. A floor scrape sample was obtained from a compact region near the northeast riser and has been analyzed for a shortened list of key analytes. Since the unused portion of the floor scrape sample material is archived and available in sufficient quantity, additional analyses need to be performed to complete results for the full suite of constituents. The characterization of the full suite of analytes in the South hemisphere is currently supported by a single Mantis rover sample; there have been no floor scrape samples previously taken from the South hemisphere. The criterion to determine the number of additional samples was based on the practical reduction in the uncertainty when a new sample is added. This was achieved when five additional samples are obtained. In addition, two archived samples will be used if a contingency such as failing to demonstrate the comparability of the Mantis samples to the floor scrape samples occurs. To complete sampling of the Tank 18 residual floor material, three additional samples should be taken from the North hemisphere and four additional samples should be taken from the South hemisphere. One of the samples from each hemisphere will be archived in case of need. Two of the three additional samples from the North hemisphere and three of the four additional samples from the South hemisphere will be analyzed. Once the results are available, differences between the Mantis and three floor scrape samples (the sample previously obtained near NE riser plus the two additional samples that will be analyzed) results will be evaluated. If there are no statistically significant analyte concentration differences between the Mantis and floor scrape samples, those results will be combined and then UCL95%s will be calculated. If the analyte concentration differences between the Mantis and floor scrape samples are statistically significant, the UCL95%s will be calculated without the Mantis sample results. If further reduction in the upper confidence limits is needed and can be achieved by the addition of the archived samples, they will be analyzed and included in the statistical computations. Initially, the analyte concentrations in the residual material on the floor of Tank 18 will be determined separately in the North and the South hemispheres. However, if final sampling results show that differences between the North and South samples are consistent within sampling variation, then the final computations can be based on consolidating all sample results from the tank floor. Recommended locations may be subject to physical tank access and sampling constraints for the additional samples. The recommendations have been discussed in Section 4 and are based on partitioning the Tank 18 floor into an inner and an outer ring and six 60{sup o} sectors depicted in Figure 1. The location of the border between the inner and outer rings is based on dividing the residual material into two approximately equal volumes.« less

Direct determination of neonicotinoid insecticides in an analytically challenging crop such as Chinese chives using selective ELISAs.

PubMed

Watanabe, Eiki; Miyake, Shiro

2018-06-05

Easy-to-use commercial kit-based enzyme-linked immunosorbent assays (ELISAs) have been used to detect neonicotinoid dinotefuran, clothianidin and imidacloprid in Chinese chives, which are considered a troublesome matrix for chromatographic techniques. Based on their high water solubility, water was used as an extractant. Matrix interference could be avoided substantially just diluting sample extracts. Average recoveries of insecticides from spiked samples were 85-113%, with relative standard deviation of <15%. The concentrations of insecticides detected from the spiked samples with the proposed ELISA methods correlated well with those by the reference high-performance liquid chromatography (HPLC) method. The residues analyzed by the ELISA methods were consistently 1.24 times that found by the HPLC method, attributable to loss of analyte during sample clean-up for HPLC analyses. It was revealed that the ELISA methods can be applied easily to pesticide residue analysis in troublesome matrix such as Chinese chives.

Variability of pesticide residues in eggplant units collected from a field trial and marketplaces in Greece.

PubMed

Prodhan, Mohammad Dalower Hossain; Papadakis, Emmanouil-Nikolaos; Papadopoulou-Mourkidou, Euphemia

2018-04-01

Variability of pesticide residues among food items is very important when assessing the risks and food safety for the consumers. Therefore, the present study was undertaken to estimate the unit-to-unit residue variability factors for eggplant. In total, 120 samples from a trial field and 142 samples from different marketplaces in Thessaloniki, Greece, were collected to estimate the variability of pesticide residues in eggplant units. They were extracted by the QuEChERS method and the residues were determined by LC-MS/MS. For the field samples, the unit-to-unit variability factors (VFs) obtained for cypermethrin and deltamethrin residues were 2.54 and 2.51, respectively. The mean residue levels of both pesticides were higher in the composite samples than in the individual samples. The average VFs for the marketplace samples was 3.89. The eggplant units exposed to pesticides were higher in residues than the non-exposed units. The variability factors obtained in the marketplace samples were higher than those in the samples collected from the field trial. A default VF value of 3 for field trials is appropriate for use when assessing the acute dietary intake but a VF for the marketplace samples should be reconsidered with a larger data. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Analysis of imidacloprid residues in fruits, vegetables, cereals, fruit juices, and baby foods, and daily intake estimation in and around Lucknow, India.

PubMed

Kapoor, Upasana; Srivastava, M K; Srivastava, Ashutosh Kumar; Patel, D K; Garg, Veena; Srivastava, L P

2013-03-01

A total of 250 samples-including fruits, fruit juices, and baby foods (50 samples each), vegetables (70 samples), and cereals (30 samples)-were collected from Lucknow, India, and analyzed for the presence of imidacloprid residues. The QuEChERS (quick, easy, cheap, effective, rugged, and safe) method of extraction coupled with high-performance liquid chromatographic analysis were carried out, and imidacloprid residues were qualitatively confirmed by liquid chromatography-mass spectrometry. Imidacloprid was not detected in samples of fruit juices and baby foods. It was, however, detected in 38 samples of fruits, vegetables, and cereals, which is about 15.20% of the total samples. Of samples of fruits, 22% showed the presence of imidacloprid, and 2% of samples showed residues above the maximal residue limit. Although imidacloprid was detected in 24% of vegetable samples, only 5.71% showed the presence of imidacloprid above the maximal residue limit. However, 33% of cereal samples showed the presence of imidacloprid, and about 3% of samples were above the maximal residue limit. The calculated estimated daily intake ranged between 0.004 and 0.131 µg/kg body weight, and the hazard indices ranged from 0.007 to 0.218 for these food commodities. It is therefore indicated that lifetime consumption of vegetables, fruits, fruit juices, baby foods, wheat, rice, and pulses may not pose a health hazard for the population of Lucknow because the hazard indices for imidacloprid residues were below one. Copyright © 2012 SETAC.

Effect of sample initial magnetic field on the metal magnetic memory NDT result

NASA Astrophysics Data System (ADS)

Moonesan, Mahdi; Kashefi, Mehrdad

2018-08-01

One of the major concerns regarding the use of Metal Magnetic Memory (MMM) technique is the complexity of residual magnetization effect on output signals. The present study investigates the influence of residual magnetic field on stress induced magnetization. To this end, various initial magnetic fields were induced on a low carbon steel sample, and for each level of residual magnetic field, the sample was subjected to a set of 4-point bending tests and, their corresponding MMM signals were collected from the surface of the bended sample using a tailored metal magnetic memory scanning device. Results showed a strong correlation between sample residual magnetic field and its corresponding level of stress induced magnetic field. It was observed that the sample magnetic field increases with applying the bending stress as long as the initial residual magnet field is low (i.e. <117 mG), but starts decreasing with higher levels of initial residual magnetic fields. Besides, effect of bending stress on the MMM output of a notched sample was investigated. The result, again, showed that MMM signals exhibit a drop at stress concentration zone when sample has high level of initial residual magnetic field.

RECOMMENDATIONS FOR SAMPLING OF TANK 19 IN F TANK FARM

DOE Office of Scientific and Technical Information (OSTI.GOV)

Harris, S.; Shine, G.

2009-12-14

Representative sampling is required for characterization of the residual material in Tank 19 prior to operational closure. Tank 19 is a Type IV underground waste storage tank located in the F-Tank Farm. It is a cylindrical-shaped, carbon steel tank with a diameter of 85 feet, a height of 34.25 feet, and a working capacity of 1.3 million gallons. Tank 19 was placed in service in 1961 and initially received a small amount of low heat waste from Tank 17. It then served as an evaporator concentrate (saltcake) receiver from February 1962 to September 1976. Tank 19 also received the spentmore » zeolite ion exchange media from a cesium removal column that once operated in the Northeast riser of the tank to remove cesium from the evaporator overheads. Recent mechanical cleaning of the tank removed all mounds of material. Anticipating a low level of solids in the residual waste, Huff and Thaxton [2009] developed a plan to sample the waste during the final clean-up process while it would still be resident in sufficient quantities to support analytical determinations in four quadrants of the tank. Execution of the plan produced fewer solids than expected to support analytical determinations in all four quadrants. Huff and Thaxton [2009] then restructured the plan to characterize the residual separately in the North and the South regions: two 'hemispheres.' This document provides sampling recommendations to complete the characterization of the residual material on the tank bottom following the guidance in Huff and Thaxton [2009] to split the tank floor into a North and a South hemisphere. The number of samples is determined from a modification of the formula previously published in Edwards [2001] and the sample characterization data for previous sampling of Tank 19 described by Oji [2009]. The uncertainty is quantified by an upper 95% confidence limit (UCL95%) on each analyte's mean concentration in Tank 19. The procedure computes the uncertainty in analyte concentration as a function of the number of samples, and the final number of samples is determined when the reduction in the uncertainty from an additional sample no longer has a practical impact on results. The characterization of the full suite of analytes in the North and South hemispheres is currently supported by a single Mantis rover sample in each hemisphere. A floor scrape sample was obtained from a compact region near the center riser slightly in the South hemisphere and has been analyzed for a shortened list of key analytes. There is not enough additional material from the floor scrape sample material for completing the full suite of constituents. No floor scrape samples have been previously taken from the North hemisphere. The criterion to determine the number of additional samples was based on the practical reduction in the uncertainty when a new sample is added. This was achieved when five additional samples are obtained. In addition, two archived samples will be used if a contingency such as failing to demonstrate the comparability of the Mantis samples to the floor scrape samples occurs. To complete sampling of the Tank 19 residual floor material, four additional samples should be taken from the North hemisphere and four additional samples should be taken from the South hemisphere. One of the samples from each hemisphere will be archived in case of need. Three of the four additional samples from each hemisphere will be analyzed. Once the results are available, differences between the Mantis and three floor scrape sample results will be evaluated. If there are no statistically significant analyte concentration differences between the Mantis and floor scrape samples, those results will be combined and then UCL95%s will be calculated. If the analyte concentration differences between the Mantis and floor scrape samples are statistically significant, the UCL95%s will be calculated without the Mantis sample results. If further reduction in the upper confidence limits is needed and can be achieved by the addition of the archived samples, they will be analyzed and included in the statistical computations. Initially the analyte concentrations in the residual material on the floor of Tank 19 will be determined separately in the North and the South hemispheres. However, if final sampling results show that differences between the North and South samples are consistent within sampling variation, then the final computations can be based on consolidating all sample results from the tank floor. Recommended locations may be subject to physical tank access and sampling constraints for the additional samples. The recommendations have been discussed in Section 4 and are based on partitioning the Tank 19 floor into an inner and an outer ring and six 60{sup o} sectors depicted in Figure 1. The location of the border between the inner and outer rings is based on dividing the residual material into two approximately equal volumes.« less

Rapid, in situ detection of cocaine residues based on paper spray ionization coupled with ion mobility spectrometry.

PubMed

Li, Ming; Zhang, Jingjing; Jiang, Jie; Zhang, Jing; Gao, Jing; Qiao, Xiaolin

2014-04-07

In this paper, a novel approach based on paper spray ionization coupled with ion mobility spectrometry (PSI-IMS) was developed for rapid, in situ detection of cocaine residues in liquid samples and on various surfaces (e.g. glass, marble, skin, wood, fingernails), without tedious sample pretreatment. The obvious advantages of PSI are its low cost, easy operation and simple configuration without using nebulizing gas or discharge gas. Compared with mass spectrometry, ion mobility spectrometry (IMS) takes advantage of its low cost, easy operation, and simple configuration without requiring a vacuum system. Therefore, IMS is a more congruous detection method for PSI in the case of rapid, in situ analysis. For the analysis of cocaine residues in liquid samples, dynamic responses from 5 μg mL(-1) to 200 μg mL(-1) with a linear coefficient (R(2)) of 0.992 were obtained. In this case, the limit of detection (LOD) was calculated to be 2 μg mL(-1) as signal to noise (S/N) was 3 with a relative standard deviation (RSD) of 6.5% for 11 measurements (n = 11). Cocaine residues on various surfaces such as metal, glass, marble, wood, skin, and fingernails were also directly analyzed before wiping the surfaces with a piece of paper. The LOD was calculated to be as low as 5 ng (S/N = 3, RSD = 6.3%, n = 11). This demonstrates the capability of the PSI-IMS method for direct detection of cocaine residues at scenes of cocaine administration. Our results show that PSI-IMS is a simple, sensitive, rapid and economical method for in situ detection of this illicit drug, which could help governments to combat drug abuse.

Residue analysis of fipronil and difenoconazole in okra by liquid chromatography tandem mass spectrometry and their food safety evaluation.

PubMed

Hingmire, Sandip; Oulkar, Dasharath P; Utture, Sagar C; Ahammed Shabeer, T P; Banerjee, Kaushik

2015-06-01

A liquid chromatography tandem mass spectrometry (LC-MS/MS) based method is reported for simultaneous analysis of fipronil (plus its metabolites) and difenoconazole residues in okra. The sample preparation method involving extraction with ethyl acetate provided 80-107% recoveries for both the pesticides with precision RSD within 4-17% estimated at the limits of quantification (LOQ, fipronil=1ngg(-1), difenoconazole=5ngg(-1)) and higher fortification levels. In field, both the pesticides dissipated with half-life of 2.5days. The estimated pre-harvest intervals (PHI) for fipronil and difenoconazole were 15 and 19.5days, and 4 and 6.5days at single and double dose of field applications, respectively. Decontamination of incurred residues by washing and different cooking treatments was quite efficient in minimizing the residue load of both the chemicals. Okra samples harvested after the estimated PHIs were found safe for human consumption. Copyright © 2014 Elsevier Ltd. All rights reserved.

Nitrogen-to-Protein Conversion Factors for Crop Residues and Animal Manure Common in China.

PubMed

Chen, Xueli; Zhao, Guanglu; Zhang, Yang; Han, Lujia; Xiao, Weihua

2017-10-25

Accurately determining protein content is essential in exploiting biomass as feed and fuel. A survey of biomass samples in China indicated protein contents from 2.65 to 3.98% for crop residues and from 6.07 to 10.24% for animal manure of dry basis. Conversion factors based on amino acid nitrogen (k A ) ranged from 5.42 to 6.00 for the former and from 4.78 to 5.36 for the latter, indicating that the traditional factor of 6.25 is not suitable for biomass samples. On the other hand, conversion factors from Kjeldahl nitrogen (k P ) ranged from 3.97 to 4.57 and from 2.76 to 4.31 for crop residues and animal manure, respectively. Of note, conversion factors were strongly affected by amino acid composition and levels of nonprotein nitrogen. Thus, k P values of 4.23 for crop residues, 4.11 for livestock manure, and 3.11 for poultry manure are recommended to better estimate protein content from total nitrogen.

Caries-removal effectiveness of a papain-based chemo-mechanical agent: A quantitative micro-CT study.

PubMed

Neves, Aline A; Lourenço, Roseane A; Alves, Haimon D; Lopes, Ricardo T; Primo, Laura G

2015-01-01

The aim of this study was to access the effectiveness and specificity of a papain-based chemo-mechanical caries-removal agent in providing minimum residual caries after cavity preparation. In order to do it, extracted carious molars were selected and scanned in a micro-CT before and after caries-removal procedures with the papain-based gel. Similar parameters for acquisition and reconstruction of the image stacks were used between the scans. After classification of the dentin substrate based on mineral density intervals and establishment of a carious tissue threshold, volumetric parameters related to effectiveness (mineral density of removed dentin volume and residual dentin tissue) and specificity (relation between carious dentin in removed volume and initial caries) of this caries-removal agent were obtained. In general, removed dentin volume was similar or higher than the initial carious volume, indicating that the method was able to effectively remove dentin tissue. Samples with an almost perfect accuracy in carious dentin removal also showed an increased removal of caries-affected tissue. On the contrary, less or no affected dentin was removed in samples where some carious tissue was left in residual dentin. Mineral density values in residual dentin were always higher or similar to the threshold for mineral density values in carious dentin. In conclusion, the papain-based gel was effective in removing carious dentin up to a conservative in vitro threshold. Lesion characteristics, such as activity and morphology of enamel lesion, may also influence caries-removal properties of the method. © Wiley Periodicals, Inc.

Method for improve x-ray diffraction determinations of residual stress in nickel-base alloys

DOEpatents

Berman, Robert M.; Cohen, Isadore

1990-01-01

A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys which comprises covering part of a predetermined area of the surface of a nickel-base alloy with a dispersion, exposing the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample.

Intergranular stress study of TC11 titanium alloy after laser shock peening by synchrotron-based high-energy X-ray diffraction

NASA Astrophysics Data System (ADS)

Su, R.; Li, L.; Wang, Y. D.; Nie, Z. H.; Ren, Y.; Zhou, X.; Wang, J.

2018-05-01

The distribution of residual lattice strain as a function of depth were carefully investigated by synchrotron-based high energy X-ray diffraction (HEXRD) in TC11 titanium alloy after laser shock peening (LSP). The results presented big compressive residual lattice strains at surface and subsurface, then tensile residual lattice strains in deeper region, and finally close to zero lattice strains in further deep interior with no plastic deformation thereafter. These evolutions in residual lattice strains were attributed to the balance of direct load effect from laser shock wave and the derivative restriction force effect from surrounding material. Significant intergranular stress was evidenced in the processed sample. The intergranular stress exhibited the largest value at surface, and rapidly decreased with depth increase. The magnitude of intergranular stress was proportional to the severity of the plastic deformation caused by LSP. Two shocks generated larger intergranular stress than one shock.

Evaluation of pesticide residues of organochlorine in vegetables and fruits in Qatar: statistical analysis.

PubMed

Al-Shamary, Noora M; Al-Ghouti, Mohammad A; Al-Shaikh, Ismail; Al-Meer, Saeed H; Ahmad, Talaat A

2016-03-01

The study aimed to examine the residues of organochlorines pesticides (OCPs) in vegetables and fruits in Qatar. A total of 127 samples was studied. Ninety percent of the imported samples recorded residues above the maximum residue levels (MRLs). The most frequently detected OCP in the samples was heptachlor (found in 75 samples). In the comparisons between the washed and unwashed samples, no significant differences were observed (P > 0.05). However, the effect of washing process with tap water depended on the type of vegetables and fruits.

Determination of formetanate hydrochloride in fruit samples using liquid chromatography-mass selective detection or -tandem mass spectrometry.

PubMed

Podhorniak, Lynda V; Kamel, Alaa; Rains, Diane M

2010-05-26

A rapid multiresidue method that captures residues of the insecticide formetanate hydrochloride (FHCl) in selected fruits is described. The method was used to provide residue data for dietary exposure determinations of FHCl. Using an acetonitrile extraction with a dispersive cleanup based on AOAC International method 2007.01, also known as QuEChERS, which was further modified and streamlined, thousands of samples were successfully analyzed for FHCl residues. FHCl levels were determined both by liquid chromatography-single-stage mass spectrometry (LC-MS) and ultraperformance liquid chromatography (UPLC)-tandem mass spectrometry (LC-MS/MS). The target limit of detection (LOD) and the limit of quantitation (LOQ) achieved for FHCl were 3.33 and 10 ng/g, respectively, with LC-MS and 0.1 and 0.3 ng/g, respectively, with LC-MS/MS. Recoveries at these previously unpublished levels ranged from 95 to 109%. A set of 20-40 samples can be prepared in one working day by two chemists.

Characterization of organic gunshot residues in lead-free ammunition using a new sample collection device for liquid chromatography-quadrupole time-of-flight mass spectrometry.

PubMed

Benito, Sandra; Abrego, Zuriñe; Sánchez, Alicia; Unceta, Nora; Goicolea, M Aranzazu; Barrio, Ramón J

2015-01-01

The identification of characteristic organic gunshot residues (OGSR) provides conclusive evidence in the elucidation of elemental profiles when lead-free ammunition is fired. OGSR also prevents false negatives. Toward this aim, a quick and efficient method based on liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF) was developed to detect and identify 18 gunpowder additives in gunshot residues (GSR). The unequivocal identification of target analytes was assured by using MS/MS mode. Swabs were compared with home-modified tape lift supports covered with a PTFE layer to determine the better sampling technique. The modified tape lift provided better extraction recoveries and enabled the analysis of inorganic and organic GSR simultaneously. The developed method was applied to the analysis of GSR from four different lead-free ammunitions. Diphenylamine and its nitrated degradation products and centralites were identified in all samples, providing strong evidence of GSR. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Residual stresses in continuous graphite fiber Al metal matrix composites

NASA Technical Reports Server (NTRS)

Park, Hun Sub; Zong, Gui Sheng; Marcus, Harris L.

1988-01-01

The residual stresses in graphite fiber reinforced aluminum (Gr/Al) composites with various thermal histories are measured using X-ray diffraction (XRD) methods. The XRD stress analysis is based on the determination of lattice strains by precise measurements of the interplanar spacings in different directions of the sample. The sample is a plate consisting of two-ply P 100 Gr/Al 6061 precursor wires and Al 6061 overlayers. Prior to XRD measurement, the 6061 overlayers are electrochemically removed. In order to calibrate the relationship between stress magnitude and lattice spacing shift, samples of Al 6061 are loaded at varying stress levels in a three-point bend fixture, while the stresses are simultaneously determined by XRD and surface-attached strain gages. The stresses determined by XRD closely match those determined by the strain gages. Using these calibrations, the longitudinal residual stresses of P 100 Gr/Al 6061 composites are measured for various heat treatments, and the results are presented.

Characteristics of the LacTek test as applied to tissue samples: assessment of performance using incurred field samples.

PubMed

Mitchell, J M; McNab, W B; Yee, A J; Griffiths, M W; McEwen, S A; Spilsbury, L; Boison, J O

1998-08-01

The Lactek test, marketed for antimicrobial residue detection in milk, was validated for the detection of antimicrobial residues in tissues. A previous study found that the LacTek test could confidently identify tissue samples spiked with antimicrobial residues. However, the test could not reliably distinguish violative from nonviolative spiked samples relative to Canadian maximum residue limits (MRLs). The objectives of this study were to assess and compare the performance of the LacTek tests for beta-lactams, tetracyclines, gentamicin, and sulfamethazine on samples containing naturally incurred residues by running the test in parallel with the standard microbial inhibition test (MIT) presently used for the routine testing of tissues at our facility and to assess the agreement with high pressure liquid chromatographic (HPLC) determinative methods. Parallel testing with the official MIT found that the Lactek tests could be confidently used for testing tissue samples containing incurred residues. Among 1,008 MIT-positive samples, the LacTek test found that 90% contained beta-lactams and/or tetracyclines. A further 7.3% of violative residues could not be identified to an antimicrobial class. In addition, 9% of samples testing negative on the MIT were found to contain an antimicrobial residue by the LacTek tests. Comparative testing with HPLC methods found that there was very good agreement between the two tests and that most violations were due to penicillin G and oxytetracycline. Although the LacTek test cannot be used to distinguish violative from nonviolative residue levels, it does offer several advantages over the present MIT. These include speed, ease of use, the ability to identify residues to a specific class, and an improved sensitivity at the MRL level for the most commonly found antimicrobials in tissue.

Rapid analysis of pesticide residues in drinking water samples by dispersive solid-phase extraction based on multiwalled carbon nanotubes and pulse glow discharge ion source ion mobility spectrometry.

PubMed

Zou, Nan; Gu, Kejia; Liu, Shaowen; Hou, Yanbing; Zhang, Jialei; Xu, Xiang; Li, Xuesheng; Pan, Canping

2016-03-01

An analytical method based on dispersive solid-phase extraction with a multiwalled carbon nanotubes sorbent coupled with positive pulse glow discharge ion mobility spectrometry was developed for analysis of 30 pesticide residues in drinking water samples. Reduced ion mobilities and the mass-mobility correlation of 30 pesticides were measured. The pesticides were divided into five groups to verify the separation capability of pulse glow discharge in mobility spectrometry. The extraction conditions such as desorption solvent, ionic strength, conditions of adsorption and desorption, the amounts of multiwalled carbon nanotubes, and solution pH were optimized. The enrichment factors of pesticides were 5.4- to 48.7-fold (theoretical enrichment factor was 50-fold). The detection limits of pesticides were 0.01∼0.77 μg/kg. The linear range was 0.005-0.2 mg/L for pesticide standard solutions, with determination coefficients from 0.9616 to 0.9999. The method was applied for the analysis of practical and spiked drinking water samples. All results were confirmed by high-performance liquid chromatography with tandem mass spectrometry. The proposed method was proven to be a commendably rapid screening qualitative and semiquantitative technique for the analysis of pesticide residues in drinking water samples on site. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Determination of estrogen residues in drinking water by on-line solid phase extraction based on sol-gel technique coupled with high performance liquid chromatography].

PubMed

Li, Longfei; Su, Min; Shi, Xiaolei; Wang, Yana; Wang, Minmin; He, Jinxing

2014-02-01

A method for the determination of diethylstilbestrol (DES), hexestrol (HEX) and dienestrol (DS) residues in drinking water was established by on-line solid phase extraction (SPE) coupled with high performance liquid chromatography (HPLC). The material synthesized on the base of sol-gel technology was employed as adsorbent. This material was prepared using 3-aminopropyltriethoxysilane (APTES) as the functional monomer, tetraethoxysilane (TEOS) as the crosslinking agent, and acetic acid as the initiator. The synthesized adsorbent showed outstanding property for the estrogen extraction. The estrogen can be caught effectively from water samples and the extraction can be achieved rapidly. Some important parameters, such as pH of sample solution, eluent solvents, loading flow rate, which might influence extraction efficiency, were optimized. The results indicated that the limit of detection (S/N = 3) of the developed method could reach 0.07-0.13 microg/L under the conditions of pH 7.0 of sample solution, methanol and 1% (v/v) acetic acid aqueous solution as the eluent solvent and the loading flow rate of 2 mL/min. The recoveries of the three estrogens from the water samples at three spiked levels ranged from 82.31% to 99.43% with RSD of 1.61%-7.15%. The method was simple, rapid, and suitable to detect the trace residues of estrogens in drinking water.

Method development for the analysis of ionophore antimicrobials in dairy manure to assess removal within a membrane-based treatment system.

PubMed

Hurst, Jerod J; Wallace, Josh S; Aga, Diana S

2018-04-01

Ionophore antimicrobials are heavily used in the livestock industries, both for preventing animal infection by coccidia protozoa and for increasing feed efficiency. Ionophores are excreted mostly unmetabolized and are released into the environment when manure is land-applied to fertilize croplands. Here, an analytical method was optimized to study the occurrences of five ionophore residues (monensin, lasalocid, maduramycin, salinomycin, and narasin) in dairy manure after solid-liquid separation and further treatment of the liquid manure by a membrane-based treatment system. Ionophore residues from the separated solid manure (dewatered manure) and suspended solids of manure slurry samples were extracted using ultrasonication with methanol, followed by sample clean-up using solid phase extraction (SPE) and subsequent analysis via liquid chromatography-tandem mass spectrometry (LC-MS/MS). The use of an ethyl acetate and methanol (1:1 v:v) mixture as an SPE eluent resulted in higher recoveries and lower method quantitation limits (MQL), when compared to using methanol. Overall recoveries from separated solid manure ranged from 73 to 134%. Liquid manure fractions were diluted with Nanopure™ water and cleaned up using SPE, where recoveries ranged from 51 to 100%. The developed extraction and LC-MS/MS methods were applied to analyze dairy manure samples subjected to an advanced manure treatment process involving a membrane-based filtration step (reverse osmosis). Monensin and lasalocid were detected at higher concentrations in the suspended solid fractions (4.40-420 ng/g for lasalocid and 85-1950 ng/g for monensin) compared to the liquid fractions (

Systematic Review of Uit Parameters on Residual Stresses of Sensitized AA5456 and Field Based Residual Stress Measurements for Predicting and Mitigating Stress Corrosion Cracking

DTIC Science & Technology

2014-03-01

power, 4 mm pin size) at a position in or near the HAZ and a position in the base metal. The areas were electropolished using the “L1” solution as...quality of polish was assessed for each instance of electropolishing . 48 6 . Electrolytic Polishing The Proto Electrolytic Polisher Model 8818-V3...finish, followed by 0.05 μm colloidal silica. After metallography, the samples were electropolished using the Buehler Electromet 4 Electrolytic

A comparison of the efficacy and ecosystem impact of residual-based and topsoil-based amendments for restoring historic mine tailings in the Tri-State mining district.

PubMed

Brown, Sally; Mahoney, Michele; Sprenger, Mark

2014-07-01

A long-term research and demonstration site was established on Pb and Zn mine wastes in southwestern Missouri in 1999. Municipal biosolids and lime and composts were mixed into the wastes at different loading rates. The site was monitored intensively after establishment and again in 2012. A site restored with topsoil was also included in the 2012 sampling. Initial results including plant, earthworm and small mammal assays indicate that the bioaccessibility of metals had been significantly reduced as a result of amendment addition. The recent sampling showed that at higher loading rates, the residual mixtures have maintained a vegetative cover and are similar to the topsoil treatment based on nutrient availability and cycling and soil physical properties including bulk density and water holding capacity. The ecosystem implications of restoration with residuals versus mined topsoil were evaluated. Harvesting topsoil from nearby farms would require 1875 years to replace based on natural rates of soil formation. In contrast, diverting biosolids from combustion facilities (60% of biosolids generated in Missouri are incinerated) would result in greenhouse gas savings of close to 400 Mg CO2 per ha. Copyright © 2014 Elsevier B.V. All rights reserved.

Pharyngeal Residue Severity Rating Scales Based on Fiberoptic Endoscopic Evaluation of Swallowing: A Systematic Review.

PubMed

Neubauer, Paul D; Hersey, Denise P; Leder, Steven B

2016-06-01

Identification of pharyngeal residue severity located in the valleculae and pyriform sinuses has always been a primary goal during fiberoptic endoscopic evaluation of swallowing (FEES). Pharyngeal residue is a clinical sign of potential prandial aspiration making an accurate description of its severity an important but difficult challenge. A reliable, validated, and generalizable pharyngeal residue severity rating scale for FEES would be beneficial. A systematic review of the published English language literature since 1995 was conducted to determine the quality of existing pharyngeal residue severity rating scales based on FEES. Databases were searched using controlled vocabulary words and synonymous free text words for topics of interest (deglutition disorders, pharyngeal residue, endoscopy, videofluoroscopy, fiberoptic technology, aspiration, etc.) and outcomes of interest (scores, scales, grades, tests, FEES, etc.). Search strategies were adjusted for syntax appropriate for each database/platform. Data sources included MEDLINE (OvidSP 1946-April Week 3 2015), Embase (OvidSP 1974-2015 April 20), Scopus (Elsevier), and the unindexed material in PubMed (NLM/NIH) were searched for relevant articles. Supplementary efforts to identify studies included checking reference lists of articles retrieved. Scales were compared using qualitative properties (sample size, severity definitions, number of raters, and raters' experience and training) and psychometric analyses (randomization, intra- and inter-rater reliability, and construct validity). Seven articles describing pharyngeal residue severity rating scales met inclusion criteria. Six of seven scales had insufficient data to support their use as evidenced by methodological weaknesses with both qualitative properties and psychometric analyses. There is a need for qualitative and psychometrically reliable, validated, and generalizable pharyngeal residue severity rating scales that are anatomically specific, image-based, and easily learned by both novice and experienced clinicians. Only the Yale Pharyngeal Residue Severity Rating Scale, an anatomically defined and image-based tool, met all qualitative and psychometric criteria necessary for a valid, reliable, and generalizable vallecula and pyriform sinus severity rating scale based on FEES.

Determination and health risk assessment of enrofloxacin, flumequine and sulfamethoxazole in imported Pangasius catfish products in Thailand.

PubMed

Jansomboon, Worawat; Boontanon, Suwanna Kitpati; Boontanon, Narin; Polprasert, Chongrak

2018-02-01

The goals of this study were to determine the levels of three antibiotics - enrofloxacin, flumequine and sulfamethoxazole - in Pangasius catfish products imported into Thailand and to assess the health risks from consumption. To extract these antibiotic residues, acetonitrile, methanol and a small amount of formic acid were used as solvents. Determination of the antibiotics after extraction steps was carried out by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) technique. The results showed that 14 and 3 samples of Pangasius catfish products were contaminated with enrofloxacin and sulfamethoxazole, respectively. No flumequine residue was found. While the concentration levels of these antibiotics in most contaminated samples were lower than the European Union (EU) standard, one sample was found to contain sulfamethoxazole at 245.91 µg kg -1 , which was higher than the EU standard (100 µg kg -1 ), indicating the likelihood that some contaminated freshwater fish products are widely distributed in Thai markets. Notably, the concentration levels of enrofloxacin in samples of Pangasius catfish with skin were higher than in non-skin products, suggesting that products with skin might retain more antibiotic residues than non-skin products. Although the hazard quotient showed that consuming imported Pangasius catfish products, based on the current consumption rate, will not adversely affect consumer health, antibiotic residues in Pangasius catfish products imported into Thailand should be continually monitored.

Bioefficacy, residue dynamics and safety assessment of the combination fungicide trifloxystrobin 25% + tebuconazole 50%-75 WG in managing early blight of tomato (Lycopersicon esculentum Mill.).

PubMed

Saha, Sujoy; Purath, Ahammed Shabeer Thekkum; Jadhav, Manjusha R; Loganathan, M; Banerjee, Kaushik; Rai, A B

2014-01-01

This paper reports the in vitro and in vivo bioefficacy of a combination fungicide trifloxystrobin (25%) + tebuconazole (50%) against early blight disease of tomato (Lycopersicon esculentum Mill.) caused by Alternaria solani and their corresponding pre-harvest intervals (PHI) with reference to the maximum residue limits (European Union). Bioefficacy of the test fungicide combination revealed that in vitro conditions manifested the best control (75.1%) at 350 mg kg(-1) against 76.2% control under field conditions. A sample preparation method based on ethyl acetate extraction and estimation by LC-MS multiple reaction monitoring (MRM) was validated in tomato fruits at 0.01 mg/kg and dissipation studies were conducted in field at single and double doses. The residues of both the compounds on all the sampling days were below the European Union maximum residue limits (EU-MRLs) and the maximum permissible intakes (MPIs) were calculated on the basis of prescribed acceptable daily intake (ADI). The combined bioefficacy and residue dynamics information will support label-claim of this fungicide combination for the management of early blight in tomato.

Quantum-Dot-Based Lateral Flow Immunoassay for Detection of Neonicotinoid Residues in Tea Leaves.

PubMed

Wang, Shuangjie; Liu, Ying; Jiao, Shasha; Zhao, Ying; Guo, Yirong; Wang, Mengcen; Zhu, Guonian

2017-11-22

Neonicotinoid insecticides are commonly used for pest control on tea plantations as a result of their broad-spectrum activity. However, neonicotinoid residues released from tea leaves into tea infusions pose a dietary risk to consumers. Therefore, a rapid, sensitive, and reliable on-site detection method for neonicotinoids is needed. We developed a quantum-dot-based fluorescent lateral flow immunochromatographic strip (LFICS) combined with a broad-specific antibody for detection of typical neonicotinoids (imidacloprid, imidaclothiz, and clothianidin), with sensitivities [50% inhibitory concentration (IC 50 )] of 0.104-0.33 ng/mL and visual detection limits of 0.5-1 ng/mL. The strip assay could be completed in less than 30 min. Using the LFICS to analyze spiked tea samples (green tea, black tea, and oolong tea), the average recovery of the three neonicotinoids ranged between 71 and 111%, with the coefficient of variation below 12%. The results from the LFICS tests for field samples were consistent with results from ultraperformance liquid chromatography-tandem mass spectrometry. The newly developed strip is a useful tool for the on-site detection of neonicotinoid residues in tea.

Multilaboratory trial for determination of ceftiofur residues in bovine and swine kidney and muscle, and bovine milk.

PubMed

Hornish, Rex E; Hamlow, Philip J; Brown, Scott A

2003-01-01

A multilaboratory trial for determining ceftiofur-related residues in bovine and swine kidney and muscle, and bovine milk was conducted following regulatory guidelines of the U.S. Food and Drug Administration, Center for Veterinary Medicine. The methods convert all desfuroylceftiofur-related residues containing the intact beta-lactam ring to desfuroylceftiofur acetamide to establish ceftiofur residues in tissues. Four laboratories analyzed 5 sets of samples for each tissue. Each sample set consisted of a control/blank sample and 3 control samples fortified with ceftiofur at 0.5 Rm, Rm, and 2 Rm, respectively, where Rm is the U.S. tolerance assigned for ceftiofur residue in each tissue/matrix: 0.100 microg/mL for milk, 8.0 microg/g for kidney (both species), 1.0 microg/g for bovine muscle, and 2.0 microg/g for swine muscle. Each sample set also contained 2 samples of incurred-residue tissues (one > Rm and one < Rm) from animals treated with ceftiofur hydrochloride. All laboratories completed the method trial after a familiarization phase and test of system suitability in which they demonstrated > 80% recovery in pretrial fortified test samples. Results showed that the methods met all acceptable performance criteria for recovery, accuracy, and precision. Although sample preparation was easy, solid-phase extraction cartridge performance must be carefully evaluated before samples are processed. The liquid chromatography detection system was easily set up; however, the elution profile may require slight modifications. The procedures could clearly differentiate between violative (> Rm) and nonviolative (< Rm) ceftiofur residues. Participating laboratories found the procedures suitable for ceftiofur residue determination.

Analysis of veterinary drug residues in frog legs and other aquacultured species using liquid chromatography quadrupole time-of-flight mass spectrometry.

PubMed

Turnipseed, Sherri B; Clark, Susan B; Storey, Joseph M; Carr, Justin R

2012-05-09

A liquid chromatography quadrupole time-of-flight (Q-TOF) mass spectrometry method was developed to analyze veterinary drug residues in frog legs and other aquacultured species. Samples were extracted using a procedure based on a method developed for the analysis of fluoroquinolones (FQs) in fish. Briefly, the tissue was extracted with dilute acetic acid and acetonitrile with added sodium chloride. After centrifugation, the extracts were evaporated and reconstituted in mobile phase. A molecular weight cutoff filter was used to clean up the final extract. A set of target compounds, including trimethoprim, sulfamethoxazole, chloramphenicol, quinolones, and FQs, was used to validate the method. Screening of residues was accomplished by collecting TOF (MS¹) data and comparing the accurate mass and retention times of compounds to a database containing information for veterinary drugs. An evaluation of the MS data in fortified frog legs indicated that the target compounds could be consistently detected at the level of concern. The linearity and recoveries from matrix were evaluated for these analytes to estimate the amount of residue present. MS/MS data were also generated from precursor ions, and the mass accuracy of the product ions for each compound was compared to theoretical values. When the method was used to analyze imported frog legs, many of these residues were found in the samples, often in combination and at relatively high concentrations (>10 ng/g). The data from these samples were also evaluated for nontarget analytes such as residue metabolites and other chemotherapeutics.

Sampling and sample processing in pesticide residue analysis.

PubMed

Lehotay, Steven J; Cook, Jo Marie

2015-05-13

Proper sampling and sample processing in pesticide residue analysis of food and soil have always been essential to obtain accurate results, but the subject is becoming a greater concern as approximately 100 mg test portions are being analyzed with automated high-throughput analytical methods by agrochemical industry and contract laboratories. As global food trade and the importance of monitoring increase, the food industry and regulatory laboratories are also considering miniaturized high-throughput methods. In conjunction with a summary of the symposium "Residues in Food and Feed - Going from Macro to Micro: The Future of Sample Processing in Residue Analytical Methods" held at the 13th IUPAC International Congress of Pesticide Chemistry, this is an opportune time to review sampling theory and sample processing for pesticide residue analysis. If collected samples and test portions do not adequately represent the actual lot from which they came and provide meaningful results, then all costs, time, and efforts involved in implementing programs using sophisticated analytical instruments and techniques are wasted and can actually yield misleading results. This paper is designed to briefly review the often-neglected but crucial topic of sample collection and processing and put the issue into perspective for the future of pesticide residue analysis. It also emphasizes that analysts should demonstrate the validity of their sample processing approaches for the analytes/matrices of interest and encourages further studies on sampling and sample mass reduction to produce a test portion.

Plant protection product residues in white grapes and wines of "Malvasia Istriana" produced in Istria.

PubMed

Baša Česnik, Helena; Velikonja Bolta, Špela; Bavčar, Dejan; Radeka, Sanja; Lisjak, Klemen

2016-12-01

Monitorting of plant protection product residues was performed in 12 grape and 66 wine samples of "Malvasia Istriana" variety, produced in Istria winegrowing region of Croatia and Slovenia. The samples were analysed for the presence of 169 different active compounds using two multiresidual analytical methods: gas chromatography coupled with mass spectrometry and liquid chromatography coupled with tandem mass spectrometry. Residues were found in 58.3% of all the inspected grape samples and in 28.8% of all the inspected wine samples. Beside that contents of residues in grapes were below 10% of maximum residue level values and they should not represent any risk for "Malvasia Istriana" grape or wine consumers.

Trend-Residual Dual Modeling for Detection of Outliers in Low-Cost GPS Trajectories.

PubMed

Chen, Xiaojian; Cui, Tingting; Fu, Jianhong; Peng, Jianwei; Shan, Jie

2016-12-01

Low-cost GPS (receiver) has become a ubiquitous and integral part of our daily life. Despite noticeable advantages such as being cheap, small, light, and easy to use, its limited positioning accuracy devalues and hampers its wide applications for reliable mapping and analysis. Two conventional techniques to remove outliers in a GPS trajectory are thresholding and Kalman-based methods, which are difficult in selecting appropriate thresholds and modeling the trajectories. Moreover, they are insensitive to medium and small outliers, especially for low-sample-rate trajectories. This paper proposes a model-based GPS trajectory cleaner. Rather than examining speed and acceleration or assuming a pre-determined trajectory model, we first use cubic smooth spline to adaptively model the trend of the trajectory. The residuals, i.e., the differences between the trend and GPS measurements, are then further modeled by time series method. Outliers are detected by scoring the residuals at every GPS trajectory point. Comparing to the conventional procedures, the trend-residual dual modeling approach has the following features: (a) it is able to model trajectories and detect outliers adaptively; (b) only one critical value for outlier scores needs to be set; (c) it is able to robustly detect unapparent outliers; and (d) it is effective in cleaning outliers for GPS trajectories with low sample rates. Tests are carried out on three real-world GPS trajectories datasets. The evaluation demonstrates an average of 9.27 times better performance in outlier detection for GPS trajectories than thresholding and Kalman-based techniques.

Cooccurrence of Mycotoxins in Maize and Poultry Feeds from Brazil by Liquid Chromatography/Tandem Mass Spectrometry

PubMed Central

de Souza, Maria de Lourdes Mendes; Sulyok, Michael; Costa, Sônia Soares; Machinski Junior, Miguel; Sekiyama, Beatriz Leiko; Vargas, Eugenia Azevedo; Krska, Rudolf; Schuhmacher, Rainer

2013-01-01

The objective of this study was to quantitatively evaluate mycotoxins in samples of maize and poultry feed produced in Brazil. A multimycotoxin method based on HPLC-MS/MS was applied to investigate the occurrence of toxical fungal metabolites in 119 samples collected from poultry feed factory integrated poultry farms: maize grain (74), poultry feed (36), and feed factory residue (9). Twenty of 101 fungal metabolites investigated were detected and quantified in the samples: aflatoxins B1, B2, G1, and G2, fumonisins B1, B2, and B3, hydrolyzed fumonisin B1, zearalenone, agroclavine, chanoclavine, deoxynivalenol, and nivalenol, and enniatin A, A1, B, B1, beauvericin, kojic acid, and moniliformin. Most samples were contaminated with more than one mycotoxin. All samples were contaminated with fumonisins, with medians values of 1,840 μg/kg, 239 μg/kg, and 23,676 μg/kg for maize, feed, and factory residue samples, respectively. Surprisingly, beauvericin was detected in more than 90% of samples. The median contaminations of aflatoxin and trichothecenes were low, near LOD values. The factory residue presented highest contamination levels for all mycotoxins. This is the first study dealing with agroclavine, chanoclavine, enniatin A, A1, B, B1, beauvericin, and kojic acid contamination of maize and poultry feeds from Brazil. PMID:24348157

Evaluation of ecological risk to populations of a threatened plant from an invasive biocontrol insect

USGS Publications Warehouse

Louda, S.M.; Rand, T.A.; Arnett, A.E.; McClay, A.S.; McEachern, A.K.

2005-01-01

This study was conducted to determine the influence of residues of organochlorine pollutants on reproductive success in the brown pelican. A sample egg was taken from each of 93 marked nests in the nesting colony in South Carolina. Periodic visits were made to determine the fate of marked nests. Each sample egg was analysed for residues of organochlorine pollutants. Nest success in the brown pelican was related to residues of DDE and dieldrin in sample eggs. DDE seemed primarily responsible for nest failure; however, deleterious effects of this pollutant on nest success were not satisfactorily separated from those induced by dieldrin. Significant intercorrelation of all five organochlorine residues identified in the eggs complicated the relationship of residues to nest success. Maximum DDE residues in an egg from a successful nest were 2.37 ?g/g and 8.48 ?g/g in an egg from an unsuccessful nest. Comparable maximum residues for dieldrin in sample eggs were 0.54 ?g/g (successful) and 0.99 ?g/g (unsuccessful). Nineteen of the 26 eggs from unsuccessful nests contained DDE residues that exceeded 2.37 ?g/g, and 14 of these 26 eggs contained dieldrin residues that exceeded O.54 ?g/g. Residues of DDD, DDT or PCBs in sample eggs were not significantly related to nest success. Reproductive success in the brown pelican colony was subnormal in the years of study--1971 and 1972--but reproductive success was normal in those nests in which the sample egg contained either <2,5 ?g/g of DDE or 0.54 ?g/g of dieldrin.

Two States Mapping Based Time Series Neural Network Model for Compensation Prediction Residual Error

NASA Astrophysics Data System (ADS)

Jung, Insung; Koo, Lockjo; Wang, Gi-Nam

2008-11-01

The objective of this paper was to design a model of human bio signal data prediction system for decreasing of prediction error using two states mapping based time series neural network BP (back-propagation) model. Normally, a lot of the industry has been applied neural network model by training them in a supervised manner with the error back-propagation algorithm for time series prediction systems. However, it still has got a residual error between real value and prediction result. Therefore, we designed two states of neural network model for compensation residual error which is possible to use in the prevention of sudden death and metabolic syndrome disease such as hypertension disease and obesity. We determined that most of the simulation cases were satisfied by the two states mapping based time series prediction model. In particular, small sample size of times series were more accurate than the standard MLP model.

Detection of residues from explosive manipulation by near infrared hyperspectral imaging: a promising forensic tool.

PubMed

Fernández de la Ossa, Mª Ángeles; Amigo, José Manuel; García-Ruiz, Carmen

2014-09-01

In this study near infrared hyperspectral imaging (NIR-HSI) is used to provide a fast, non-contact, non-invasive and non-destructive method for the analysis of explosive residues on human handprints. Volunteers manipulated individually each of these explosives and after deposited their handprints on plastic sheets. For this purpose, classical explosives, potentially used as part of improvised explosive devices (IEDs) as ammonium nitrate, blackpowder, single- and double-base smokeless gunpowders and dynamite were studied. A partial-least squares discriminant analysis (PLS-DA) model was built to detect and classify the presence of explosive residues in handprints. High levels of sensitivity and specificity for the PLS-DA classification model created to identify ammonium nitrate, blackpowder, single- and double-base smokeless gunpowders and dynamite residues were obtained, allowing the development of a preliminary library and facilitating the direct and in situ detection of explosives by NIR-HSI. Consequently, this technique is showed as a promising forensic tool for the detection of explosive residues and other related samples. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

Identification of residual leukemic cells by flow cytometry in childhood B-cell precursor acute lymphoblastic leukemia: verification of leukemic state by flow-sorting and molecular/cytogenetic methods.

PubMed

Øbro, Nina F; Ryder, Lars P; Madsen, Hans O; Andersen, Mette K; Lausen, Birgitte; Hasle, Henrik; Schmiegelow, Kjeld; Marquart, Hanne V

2012-01-01

Reduction in minimal residual disease, measured by real-time quantitative PCR or flow cytometry, predicts prognosis in childhood B-cell precursor acute lymphoblastic leukemia. We explored whether cells reported as minimal residual disease by flow cytometry represent the malignant clone harboring clone-specific genomic markers (53 follow-up bone marrow samples from 28 children with B-cell precursor acute lymphoblastic leukemia). Cell populations (presumed leukemic and non-leukemic) were flow-sorted during standard flow cytometry-based minimal residual disease monitoring and explored by PCR and/or fluorescence in situ hybridization. We found good concordance between flow cytometry and genomic analyses in the individual flow-sorted leukemic (93% true positive) and normal (93% true negative) cell populations. Four cases with discrepant results had plausible explanations (e.g. partly informative immunophenotype and antigen modulation) that highlight important methodological pitfalls. These findings demonstrate that with sufficient experience, flow cytometry is reliable for minimal residual disease monitoring in B-cell precursor acute lymphoblastic leukemia, although rare cases require supplementary PCR-based monitoring.

Annotating Protein Functional Residues by Coupling High-Throughput Fitness Profile and Homologous-Structure Analysis.

PubMed

Du, Yushen; Wu, Nicholas C; Jiang, Lin; Zhang, Tianhao; Gong, Danyang; Shu, Sara; Wu, Ting-Ting; Sun, Ren

2016-11-01

Identification and annotation of functional residues are fundamental questions in protein sequence analysis. Sequence and structure conservation provides valuable information to tackle these questions. It is, however, limited by the incomplete sampling of sequence space in natural evolution. Moreover, proteins often have multiple functions, with overlapping sequences that present challenges to accurate annotation of the exact functions of individual residues by conservation-based methods. Using the influenza A virus PB1 protein as an example, we developed a method to systematically identify and annotate functional residues. We used saturation mutagenesis and high-throughput sequencing to measure the replication capacity of single nucleotide mutations across the entire PB1 protein. After predicting protein stability upon mutations, we identified functional PB1 residues that are essential for viral replication. To further annotate the functional residues important to the canonical or noncanonical functions of viral RNA-dependent RNA polymerase (vRdRp), we performed a homologous-structure analysis with 16 different vRdRp structures. We achieved high sensitivity in annotating the known canonical polymerase functional residues. Moreover, we identified a cluster of noncanonical functional residues located in the loop region of the PB1 β-ribbon. We further demonstrated that these residues were important for PB1 protein nuclear import through the interaction with Ran-binding protein 5. In summary, we developed a systematic and sensitive method to identify and annotate functional residues that are not restrained by sequence conservation. Importantly, this method is generally applicable to other proteins about which homologous-structure information is available. To fully comprehend the diverse functions of a protein, it is essential to understand the functionality of individual residues. Current methods are highly dependent on evolutionary sequence conservation, which is usually limited by sampling size. Sequence conservation-based methods are further confounded by structural constraints and multifunctionality of proteins. Here we present a method that can systematically identify and annotate functional residues of a given protein. We used a high-throughput functional profiling platform to identify essential residues. Coupling it with homologous-structure comparison, we were able to annotate multiple functions of proteins. We demonstrated the method with the PB1 protein of influenza A virus and identified novel functional residues in addition to its canonical function as an RNA-dependent RNA polymerase. Not limited to virology, this method is generally applicable to other proteins that can be functionally selected and about which homologous-structure information is available. Copyright © 2016 Du et al.

Suitability of the line intersect method for sampling hardwood logging residues

Treesearch

A. Jeff Martin

1976-01-01

The line intersect method of sampling logging residues was tested in Appalachian hardwoods and was found to provide unbiased estimates of the volume of residue in cubic feet per acre. Thirty-two chains of sample line were established on each of sixteen 1-acre plots on cutover areas in a variety of conditions. Estimates from these samples were then compared to actual...

DNA from fecal immunochemical test can replace stool for detection of colonic lesions using a microbiota-based model.

PubMed

Baxter, Nielson T; Koumpouras, Charles C; Rogers, Mary A M; Ruffin, Mack T; Schloss, Patrick D

2016-11-14

There is a significant demand for colorectal cancer (CRC) screening methods that are noninvasive, inexpensive, and capable of accurately detecting early stage tumors. It has been shown that models based on the gut microbiota can complement the fecal occult blood test and fecal immunochemical test (FIT). However, a barrier to microbiota-based screening is the need to collect and store a patient's stool sample. Using stool samples collected from 404 patients, we tested whether the residual buffer containing resuspended feces in FIT cartridges could be used in place of intact stool samples. We found that the bacterial DNA isolated from FIT cartridges largely recapitulated the community structure and membership of patients' stool microbiota and that the abundance of bacteria associated with CRC were conserved. We also found that models for detecting CRC that were generated using bacterial abundances from FIT cartridges were equally predictive as models generated using bacterial abundances from stool. These findings demonstrate the potential for using residual buffer from FIT cartridges in place of stool for microbiota-based screening for CRC. This may reduce the need to collect and process separate stool samples and may facilitate combining FIT and microbiota-based biomarkers into a single test. Additionally, FIT cartridges could constitute a novel data source for studying the role of the microbiome in cancer and other diseases.

Preliminary Evaluation of the Field and Laboratory Emission Cell (FLEC) for Sampling Attribution Signatures from Building Materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Harvey, Scott D.; He, Lijian; Wahl, Jon H.

2012-08-30

This study provides a preliminary evaluation of the Field and Laboratory Emission Cell (FLEC) for its suitability for sampling building materials for toxic compounds and their associated impurities and residues that might remain after a terrorist chemical attack. Chemical warfare (CW) agents and toxic industrial chemicals were represented by a range of test probes that included CW surrogates. The test probes encompassed the acid-base properties, volatilities, and polarities of the expected chemical agents and residual compounds. Results indicated that dissipation of the test probes depended heavily on the underlying material. Near complete dissipation of almost all test probes occurred frommore » galvanized stainless steel within 3.0 hrs, whereas far stronger retention with concomitant slower release was observed for vinyl composition floor tiles. The test probes displayed immediated permanence on Teflon. FLEC sampling was further evaluated by profiling residues remaining after the evaporation of 2-chloroethyl ethyl sulfide, a sulfur mustard simulant. This study lays the groundwork for the eventual goal of applying this sampling approach for collection of forensic attribution signatures that remain after a terrorist chemical attack.« less

The United States Polar Rock Repository: A geological resource for the Earth science community

USGS Publications Warehouse

Grunow, Annie M.; Elliot, David H.; Codispoti, Julie E.

2007-01-01

The United States Polar Rock Repository (USPRR) is a U. S. national facility designed for the permanent curatorial preservation of rock samples, along with associated materials such as field notes, annotated air photos and maps, raw analytic data, paleomagnetic cores, ground rock and mineral residues, thin sections, and microfossil mounts, microslides and residues from Polar areas. This facility was established by the Office of Polar Programs at the U. S. National Science Foundation (NSF) to minimize redundant sample collecting, and also because the extreme cold and hazardous field conditions make fieldwork costly and difficult. The repository provides, along with an on-line database of sample information, an essential resource for proposal preparation, pilot studies and other sample based research that should make fieldwork more efficient and effective. This latter aspect should reduce the environmental impact of conducting research in sensitive Polar Regions. The USPRR also provides samples for educational outreach. Rock samples may be borrowed for research or educational purposes as well as for museum exhibits.

77 FR 39895 - New Analytic Methods and Sampling Procedures for the United States National Residue Program for...

Federal Register 2010, 2011, 2012, 2013, 2014

2012-07-06

... Analytic Methods and Sampling Procedures for the United States National Residue Program for Meat, Poultry... implementing several multi-residue methods for analyzing samples of meat, poultry, and egg products for animal.... These modern, high-efficiency methods will conserve resources and provide useful and reliable results...

Pesticide residues in orange fruit from citrus orchards in Nuevo Leon State, Mexico.

PubMed

Suárez-Jacobo, Angela; Alcantar-Rosales, Victor Manuel; Alonso-Segura, Diana; Heras-Ramírez, Maria; Elizarragaz-De La Rosa, Dalau; Lugo-Melchor, Ofelia; Gaspar-Ramirez, Octavio

2017-09-01

Some international organisations established maximum residue limits (MRLs) in food to protect human health. Mexico lacks regulations in this matter, affecting national and international trade from agroindustry. The aim of this study was to diagnose pesticide residues in oranges from Nuevo Leon, México, in citrus orchards. In May 2014, 100 orange fruit samples were taken randomly from orchards and subjected to analysis for 93 pesticides at residual level by GC/QQQ-MS and LCQ-TOF-MS. Results showed the presence of 15 pesticide residues in the samples. The comparison of the residual levels of pesticides found in orange samples among the MRLs allowed by USA, EU and Japanese regulations demonstrated that all samples were below MRLs issued by USA and Japan. Some orange samples were above MRLs issued by the EU. This provides a basis to establish strategies in order to satisfy International Standards to protect human health and encourage Food Safety in Mexico.

Multi-residue analysis of pesticide residues in mangoes using solid-phase microextraction coupled to liquid chromatography and UV-Vis detection.

PubMed

Filho, Adalberto M; dos Santos, Fábio N; Pereira, Pedro A de Paula

2011-11-01

A sensitive and efficient solid-phase microextraction method, based on liquid chromatography and UV-Vis detection, was developed and validated as an alternative method for sample screening prior to LC-MS analysis. It enables the simultaneous determination of ten pesticides in mango fruits. The fiber used was polydimethylsiloxane while optimum SPME conditions employed have been developed and optimized in a previous work. The desorption process was performed in static mode, using acetonitrile as a solvent. The results indicate that the DI-SPME/HPLC/UV-Vis procedure resulted in good linear range, accuracy, precision and sensibility and is adequate for analyzing pesticide residues in mango fruits. The limits of detection (0.6-3.3 μg/kg) and quantification (2.0-10.0 μg/kg) were achieved with values lower than the maximum residue levels (MRLs) established by Brazilian legislation for all pesticides in this study. The average recovery rates obtained for each pesticide ranged from 71.6 to 104.3% at three fortification levels, with the relative standard deviation ranging from 4.3 to 18.6%. The proposed method was applied for the determination of the aforementioned compounds in commercial mango samples and residues of azoxystrobin, fenthion, permethrin, abamectin and bifenthrin were detected in the mango samples, although below the MRLs established by Brazilian legislation. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Assessing variability and trends in Arctic sea ice distribution using satellite data

USGS Publications Warehouse

Belchansky, G.I.; Mordvintsev, Ilia N.; Douglas, David C.

1996-01-01

A survey of organochlorine residues in woodcock wings was undertaken to determine whether these wings are suitable for showing regional differences in residues and to obtain a baseline in 1970-71 for later comparisons. Woodcock wings were obtained from the annual hunter's wing survey. Samples came from eight States (Louisiana, Maine, Michigan, New Hampshire, New Jersey, New York, Pennsylvania, and Wisconsin) and one tri-State area (North Carolina, South Carolina, and Georgia). Wings from the tri-State area contained significantly higher (P<0.01) concentrations of DDT (including DDT, DDD, and DDE) than those from other States. Concentrations of polychlorinated biphenyls (PCB's) also were significantly higher (P<0.05) in samples from these three States. Wings from Louisiana and the tri-State area had significantly higher (P<0.01) concentrations of dieldrin than wings from the other States, and those from Louisiana had significantly higher (P < 0.01) concentrations of mirex than those from other States. (Residues are on lipid base) The compounds detected and the ranges of residue means for all sampling areas were as follows: Total DDT (5.89--65.15 ppm); DDT (0.34 m--14.93 ppm); DDE (4.66--47.47 ppm); DDD (0.11--3.44 ppm); mirex (0.76--16.93 ppm); dieldrin (0.09--3.06 ppm); and PCB's (4.27--8.63 ppm). Woodcock wings appear to be suitable for determining regional differences in organochlorine residues in this species.

Good medicine for conservation biology: The intersection of epidemiology and conservation theory

USGS Publications Warehouse

Lafferty, Kevin D.; Gerber, Leah R.

2002-01-01

A survey of organochlorine residues in woodcock wings was undertaken to determine whether these wings are suitable for showing regional differences in residues and to obtain a baseline in 1970-71 for later comparisons. Woodcock wings were obtained from the annual hunter's wing survey. Samples came from eight States (Louisiana, Maine, Michigan, New Hampshire, New Jersey, New York, Pennsylvania, and Wisconsin) and one tri-State area (North Carolina, South Carolina, and Georgia). Wings from the tri-State area contained significantly higher (P<0.01) concentrations of DDT (including DDT, DDD, and DDE) than those from other States. Concentrations of polychlorinated biphenyls (PCB's) also were significantly higher (P<0.05) in samples from these three States. Wings from Louisiana and the tri-State area had significantly higher (P<0.01) concentrations of dieldrin than wings from the other States, and those from Louisiana had significantly higher (P < 0.01) concentrations of mirex than those from other States. (Residues are on lipid base) The compounds detected and the ranges of residue means for all sampling areas were as follows: Total DDT (5.89--65.15 ppm); DDT (0.34 m--14.93 ppm); DDE (4.66--47.47 ppm); DDD (0.11--3.44 ppm); mirex (0.76--16.93 ppm); dieldrin (0.09--3.06 ppm); and PCB's (4.27--8.63 ppm). Woodcock wings appear to be suitable for determining regional differences in organochlorine residues in this species.

An Image Segmentation Based on a Genetic Algorithm for Determining Soil Coverage by Crop Residues

PubMed Central

Ribeiro, Angela; Ranz, Juan; Burgos-Artizzu, Xavier P.; Pajares, Gonzalo; Sanchez del Arco, Maria J.; Navarrete, Luis

2011-01-01

Determination of the soil coverage by crop residues after ploughing is a fundamental element of Conservation Agriculture. This paper presents the application of genetic algorithms employed during the fine tuning of the segmentation process of a digital image with the aim of automatically quantifying the residue coverage. In other words, the objective is to achieve a segmentation that would permit the discrimination of the texture of the residue so that the output of the segmentation process is a binary image in which residue zones are isolated from the rest. The RGB images used come from a sample of images in which sections of terrain were photographed with a conventional camera positioned in zenith orientation atop a tripod. The images were taken outdoors under uncontrolled lighting conditions. Up to 92% similarity was achieved between the images obtained by the segmentation process proposed in this paper and the templates made by an elaborate manual tracing process. In addition to the proposed segmentation procedure and the fine tuning procedure that was developed, a global quantification of the soil coverage by residues for the sampled area was achieved that differed by only 0.85% from the quantification obtained using template images. Moreover, the proposed method does not depend on the type of residue present in the image. The study was conducted at the experimental farm “El Encín” in Alcalá de Henares (Madrid, Spain). PMID:22163966

Liquid paraffin as new dilution medium for the analysis of high boiling point residual solvents with static headspace-gas chromatography.

PubMed

D'Autry, Ward; Zheng, Chao; Bugalama, John; Wolfs, Kris; Hoogmartens, Jos; Adams, Erwin; Wang, Bochu; Van Schepdael, Ann

2011-07-15

Residual solvents are volatile organic compounds which can be present in pharmaceutical substances. A generic static headspace-gas chromatography analysis method for the identification and control of residual solvents is described in the European Pharmacopoeia. Although this method is proved to be suitable for the majority of samples and residual solvents, the method may lack sensitivity for high boiling point residual solvents such as N,N-dimethylformamide, N,N-dimethylacetamide, dimethyl sulfoxide and benzyl alcohol. In this study, liquid paraffin was investigated as new dilution medium for the analysis of these residual solvents. The headspace-gas chromatography method was developed and optimized taking the official Pharmacopoeia method as a starting point. The optimized method was validated according to ICH criteria. It was found that the detection limits were below 1μg/vial for each compound, indicating a drastically increased sensitivity compared to the Pharmacopoeia method, which failed to detect the compounds at their respective limit concentrations. Linearity was evaluated based on the R(2) values, which were above 0.997 for all compounds, and inspection of residual plots. Instrument and method precision were examined by calculating the relative standard deviations (RSD) of repeated analyses within the linearity and accuracy experiments, respectively. It was found that all RSD values were below 10%. Accuracy was checked by a recovery experiment at three different levels. Mean recovery values were all in the range 95-105%. Finally, the optimized method was applied to residual DMSO analysis in four different Kollicoat(®) sample batches. Copyright © 2011 Elsevier B.V. All rights reserved.

Long-Term Impacts Induced by Disposal of Contaminated River Sediments in Elliott Bay, Seattle, Washington

DTIC Science & Technology

1984-09-01

and these accompanied the sample residue through sieving to avoid sample mix- up . B. Field data sheets required logger’s initials on each page to A...ensure data completeness. C. Metal trays were placed to catch residue spillage during residue transfer from sieves to sample bottles. D. Sample bottles...methodologies were comparable for all sample e types and consisted of four sequential components: extraction, clean- up , gas chromatographic (GC) analysis, and

A heteroskedastic error covariance matrix estimator using a first-order conditional autoregressive Markov simulation for deriving asympotical efficient estimates from ecological sampled Anopheles arabiensis aquatic habitat covariates

PubMed Central

Jacob, Benjamin G; Griffith, Daniel A; Muturi, Ephantus J; Caamano, Erick X; Githure, John I; Novak, Robert J

2009-01-01

Background Autoregressive regression coefficients for Anopheles arabiensis aquatic habitat models are usually assessed using global error techniques and are reported as error covariance matrices. A global statistic, however, will summarize error estimates from multiple habitat locations. This makes it difficult to identify where there are clusters of An. arabiensis aquatic habitats of acceptable prediction. It is therefore useful to conduct some form of spatial error analysis to detect clusters of An. arabiensis aquatic habitats based on uncertainty residuals from individual sampled habitats. In this research, a method of error estimation for spatial simulation models was demonstrated using autocorrelation indices and eigenfunction spatial filters to distinguish among the effects of parameter uncertainty on a stochastic simulation of ecological sampled Anopheles aquatic habitat covariates. A test for diagnostic checking error residuals in an An. arabiensis aquatic habitat model may enable intervention efforts targeting productive habitats clusters, based on larval/pupal productivity, by using the asymptotic distribution of parameter estimates from a residual autocovariance matrix. The models considered in this research extends a normal regression analysis previously considered in the literature. Methods Field and remote-sampled data were collected during July 2006 to December 2007 in Karima rice-village complex in Mwea, Kenya. SAS 9.1.4® was used to explore univariate statistics, correlations, distributions, and to generate global autocorrelation statistics from the ecological sampled datasets. A local autocorrelation index was also generated using spatial covariance parameters (i.e., Moran's Indices) in a SAS/GIS® database. The Moran's statistic was decomposed into orthogonal and uncorrelated synthetic map pattern components using a Poisson model with a gamma-distributed mean (i.e. negative binomial regression). The eigenfunction values from the spatial configuration matrices were then used to define expectations for prior distributions using a Markov chain Monte Carlo (MCMC) algorithm. A set of posterior means were defined in WinBUGS 1.4.3®. After the model had converged, samples from the conditional distributions were used to summarize the posterior distribution of the parameters. Thereafter, a spatial residual trend analyses was used to evaluate variance uncertainty propagation in the model using an autocovariance error matrix. Results By specifying coefficient estimates in a Bayesian framework, the covariate number of tillers was found to be a significant predictor, positively associated with An. arabiensis aquatic habitats. The spatial filter models accounted for approximately 19% redundant locational information in the ecological sampled An. arabiensis aquatic habitat data. In the residual error estimation model there was significant positive autocorrelation (i.e., clustering of habitats in geographic space) based on log-transformed larval/pupal data and the sampled covariate depth of habitat. Conclusion An autocorrelation error covariance matrix and a spatial filter analyses can prioritize mosquito control strategies by providing a computationally attractive and feasible description of variance uncertainty estimates for correctly identifying clusters of prolific An. arabiensis aquatic habitats based on larval/pupal productivity. PMID:19772590

Method for improving x-ray diffraction determinations of residual stress in nickel-base alloys

DOEpatents

Berman, R.M.; Cohen, I.

1988-04-26

A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys is discussed. Part of a predetermined area of the surface of a nickel-base alloy is covered with a dispersion. This exposes the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose, since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample. 2 figs.

Pesticide residue determination in vegetables from western China applying gas chromatography with mass spectrometry.

PubMed

Qin, Guofu; Zou, Keting; Li, Yongbo; Chen, Yan; He, Fengrui; Ding, Guirong

2016-09-01

In this study,an effort has been made to evaluate the pesticide residues in vegetables from western China. Fifty-one pesticides, including organophosphorus, organochlorine, carbamate and pyrethroid, were detected in 369 commonly used vegetables by GC-MS. Concentrations of organophosphorus pesticides were detected ranging from 0.0008 to 18.8200 mg/kg, among which organophosphorus pesticide concentrations exceeded their maximum residue levels (MRLs) in five samples. Carbamate and organochlorine pesticides were determined to have concentrations in the range of 0.0012-0.7928 mg/kg. The residual concentrations of carbamate pesticides in six samples and organochlorine pesticides in four samples exceeded their MRLs. The residual concentrations of five pyrethroid pesticides were within the range of 0.0016-6.0827 mg/kg and the pyrethroid residues in two samples exceeded their MRLs. The results revealed that pesticide residues in 70.73% of the vegetables samples were not detected, while in the rest of vegetables there were one or more pesticide residues and some even exceeded their MRLs, which would threaten the health of consumers. Our work provides significant information for the food safety regulations to control the excessive use of some pesticides on those kinds of vegetables from western China. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Occurrence and spatial distribution of pesticide residues in butter and ghee (clarified butter fat) in Punjab (India).

PubMed

Bedi, J S; Gill, J P S; Aulakh, R S; Kaur, Prabhjit

2016-02-01

The present study was undertaken to monitor organochlorine, organophosphate, and synthetic pyrethroid pesticide residues in butter (n = 55) and ghee (n = 56) samples collected from three different regions of Punjab. The estimation of pesticide residues was done by multiple residue analytical technique using gas chromatography equipped with GC-ECD and GC-FTD. The confirmation of residues was done on gas chromatography mass spectrometry in both selective ion monitoring (SIM) and scan mode. Results indicated the presence of hexacholorocyclohexane (HCH) and p,p' DDE as predominant contaminant in both butter and ghee. Residues of HCH were detected in 25 and 23% samples of butter and ghee, respectively, while residues of p,p' DDE were recorded in 29 and 25% of butter and ghee samples, respectively. None of the butter and ghee sample violated the MRL values of 200 ng g(-1) for HCH and 1250 ng g(-1) for dichorodiphenyl tricholorethane (DDT). The presence of endosulfan, cypermethrin, fenvalerate, deltamethrin, and chlorpyrifos were observed in a few butter and ghee samples at traces. The spatial variation for comparative occurrence of pesticide residues indicated higher levels in the south-western region of Punjab. Additionally, the temporal variation indicated the significant reduction of HCH and DDT levels in butter and ghee in Punjab.

Evaluation of pesticide residues in fruits and vegetables from Algeria.

PubMed

Mebdoua, Samira; Lazali, Mohamed; Ounane, Sidi Mohamed; Tellah, Sihem; Nabi, Fahima; Ounane, Ghania

2017-06-01

A total of 160 samples of 13 types of fresh fruits and vegetables from domestic production and import were analysed to detect the presence of pesticide residues. Analysis was performed by multi-residual extraction followed by gas chromatography-mass spectrometry. In 42.5% of the tested samples, no residues were found and 12.5% of samples contained pesticide residues above maximum residue limits. Risk assessment for long-term exposure was done for all pesticides detected in this study. Except chlorpyrifos and lambda-cyhalothrin, exposure to pesticides from vegetables and fruits was below 1% of the acceptable daily intake. Short-term exposure assessment revealed that in seven pesticide/commodity combinations, including three pesticides (chlorpyrifos, deltamethrin and lambda-cyhalothrin), the acute reference dose had been exceeded.

Pesticide residue analysis of soil, water, and grain of IPM basmati rice.

PubMed

Arora, Sumitra; Mukherji, Irani; Kumar, Aman; Tanwar, R K

2014-12-01

The main aim of the present investigations was to compare the pesticide load in integrated pest management (IPM) with non-IPM crops of rice fields. The harvest samples of Basmati rice grain, soil, and irrigation water, from IPM and non-IPM field trials, at villages in northern India, were analyzed using multi-pesticide residue method. The field experiments were conducted for three consecutive years (2008-2011) for the successful validation of the modules, synthesized for Basmati rice, at these locations. Residues of tricyclazole, propiconazole, hexconazole, lambda cyhalothrin, pretilachlor chlorpyrifos, DDVP, carbendazim, and imidacloprid were analyzed from two locations, Dudhli village of Dehradun, Uttrakhand and Saboli and Aterna village of Sonepat, Haryana. The pesticide residues were observed below detectable limit (BDL) (<0.001-0.05 μg/g) in all 24 samples of rice grains and soil under IPM and non-IPM trials. Residues were below detection level (<0.001-0.05 μg/L) in irrigation water samples (2008-09). Residues of tricyclazole and carbendazim, analyzed from same locations, revealed pesticide residues as BDL (<0.001-0.05 μg/g) in all 40 samples of Basmati rice grains and soil. It was also observed as BDL (<0.001-0.05 μg/L) for 12 water samples (2009-2010). The residues of tricyclazole, propioconazole, chlorpyrifos, hexaconazole, pretilachlor, and λ-cyhalothrin were also found as BDL (<0.001-0.05 μg/g) in 40 samples of Basmati rice grains and soil and 12 water samples (<0.001-0.05 μg/L) (2010-2011).

Safe apples for baby-food production: survey of pesticide treatment regimes leaving minimum residues.

PubMed

Ticha, Jana; Hajslova, Jana; Kovalczuk, Tomas; Jech, Martin; Honzicek, Jiri; Kocourek, Vladimir; Lansky, Miroslav; Kloutvorova, Jana; Falta, Vladan

2007-06-01

A total of 19 pesticide preparations were used according to agricultural practice in six trials in apple orchards. Using gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS), premature Golden Delicious apples collected 64, 50, 36 days before harvest and mature fruit were examined for residues of active ingredients. No residues of triflumuron, triazamate, chlorpyrifos, etofenprox, fenoxycarb, kresoxim-methyl, cyprodinyl, difenoconazole or thiram were detected in the first sampling. Also, the levels of chlorpyrifos-methyl, penconazole, tebuconazole and tolylfluanid dropped during the pre-harvest interval. Detectable residues of pyridaben, thiacloprid, trifloxystrobin and tetraconazole in harvested fruits were below 0.01 mg kg(-1), which is the maximum concentration of residues acceptable by baby-food producers in any raw material. The only residues exceeding this concentration were captan and teflubenzuron. Based on the data, farmers can choose pesticides for optimal treatment of plants, while enabling growth of a safe crop suitable for baby-food production.

Highly sensitive MYD88L265P mutation detection by droplet digital PCR in Waldenström Macroglobulinemia.

PubMed

Drandi, Daniela; Genuardi, Elisa; Dogliotti, Irene; Ferrante, Martina; Jiménez, Cristina; Guerrini, Francesca; Lo Schirico, Mariella; Mantoan, Barbara; Muccio, Vittorio; Lia, Giuseppe; Zaccaria, Gian Maria; Omedè, Paola; Passera, Roberto; Orsucci, Lorella; Benevolo, Giulia; Cavallo, Federica; Galimberti, Sara; García-Sanz, Ramón; Boccadoro, Mario; Ladetto, Marco; Ferrero, Simone

2018-03-22

We here describe a novel method for MYD88 L265P mutation detection and minimal residual disease monitoring in Waldenström Macroglobulinemia, by droplet digital PCR, in bone marrow and peripheral blood cells, as well as in circulating cell free DNA. Our method shows a sensitivity of 5.00E-05, by far superior to the widely used allele-specific polymerase chain reaction (1.00E-03). Overall, 291 unsorted samples from 148 patients (133 Waldenstrom 11 IgG-lymphoplasmacytic lymphoma and 4 IgM-monoclonal gammopathy of undetermined significance), 194 baseline and 97 follow-up, were analyzed. 122/128 (95.3%) bone marrow and 47/66 (71.2%) baseline peripheral blood samples scored positive for MYD88 L265P Moreover, to investigate whether MYD88 L265P by droplet digital PCR could be used for minimal residual disease monitoring, mutation levels were compared with IGH-based minimal residual disease analysis in 10 patients, showing to be as informative as to the classical, standardized but not yet validated in Waldenström Macroglobulinemia, IGH-based minimal residual disease assay (r 2 =0.64). Finally, MYD88 L265P detection performed by droplet digital PCR on plasmatic circulating tumor DNA from 60 patients showed a good correlation with bone marrow (bone marrow median mutational value 1.92E-02, plasmatic circulating tumor DNA value: 1.4E-02, peripheral blood value: 1.03E-03). This study indicates that droplet digital PCR MYD88 L265P assay is a feasible and sensitive tool for mutational screening and minimal residual disease monitoring in Waldenström Macroglobulinemia. Both unsorted bone marrow and peripheral blood samples can be reliably tested, as well as circulating tumor DNA, that represents an attractive, less invasive alternative to bone marrow for MYD88 L265P detection. Copyright © 2018, Ferrata Storti Foundation.

Bee honey as an environmental bioindicator of pesticides' occurrence in six agricultural areas of Greece.

PubMed

Balayiannis, George; Balayiannis, Panos

2008-10-01

The pollution of six agricultural areas of Greece (north, central, south) by insecticides used in crop protection has been investigated utilizing, as a bioindicator, bee honey produced in those areas. Honey samples collected randomly from apiaries located in those areas were analyzed for pesticide residues with a multianalytical method, able to determine simultaneously up to 10 organophosphorous insecticides from the same honey extract. Findings concerning the acaricide coumaphos were also included, even though it is not used in crop protection. Coumaphos is used to control the mite Varroa destructor, an external parasite of the honeybee. The above areas are cultivated in large extent with citrus trees or cotton or sunflower crops, which are good forages for honeybees. The main pests of those crops are insects; hence, insecticides are used on a large scale for crop protection. The most contaminated samples originated from citrus groves; 16 out of 19 had pesticide residues: 4 samples had chlorfenvinphos (21.05%), 10 had chlorpyrifos (52.63%) and 2 had phorate (10.53%). Out of 17 samples from cotton fields, residues were found in 8, phorate in 6 (35.29%), chlorfenvinphos in 1 (5.88%), and chlorpyrifos in 1 (5.88%). Out of nine samples from fields of sunflower, four had phorate residues (44.44%). In brief, from the 50 analyzed samples, residues of chlorfenvinphos were detected in 5 samples (10%), residues of chlorpyrifos in 11 samples (22%), and residues of phorate in 12 samples (24%). Their levels ranged between 0.70 and 0.89 microg/kg. Coumaphos residues ranged from 0.10 up to 4.80 microg/kg and were derived exclusively from beehives treated with Perizin (the commercial formulation of coumaphos) for Varroa control. This study indicates that in agricultural areas with developed apiculture, useful information about the occurrence and the distribution of pesticide residues due to crop protection treatments can be derived from the analysis of randomly collected honey samples, used as bioindicators. It also shows that, very often, the chemicals used by apiculturists inside the hives in order to control disease are the main pollutants of the produced honey.

CO2CRC's Otway Residual Saturation and Dissolution Test: Using Reactive Ester Tracers to Determine Residual CO2 Saturation

NASA Astrophysics Data System (ADS)

Myers, M.; Stalker, L.; LaForce, T.; Pejcic, B.; Dyt, C.; Ho, K.; Ennis-King, J.

2013-12-01

Residual trapping, that is CO2 held in the rock pore space due to capillarity, is an important storage mechanism in geo-sequestration of over the short to medium term (up to 1000 years). As such residual CO2 saturation is a critical reservoir parameter for assessing the storage capacity and security of carbon capture and storage (CCS). As a component of the CO2CRC's Residual Gas Saturation and Dissolution Test at the CO2CRC Otway Project site in Victoria (Australia), we have recently tested a suite of reactive esters (triacetin, tripropionin and propylene glycol diacetate) in a single well chemical tracer test to determine residual CO2 saturation. The goal of this project was to assess and validate a suite of possible tests that could be implemented to determine residual CO2 saturation. For this test, the chemical tracers were injected with a saturated CO2/water mixture into the formation (that is already at residual CO2 saturation) where they were allowed to 'soak' for approximately 10 days allowing for the partial hydrolysis of the esters to their corresponding carboxylic acids and alcohols. Water containing the tracers was then produced from the well resulting in over 600 tracer samples over a period of 12 hours. A selection of these samples were analysed for tracer content and to establish tracer breakthrough curves. To understand the behaviour of these chemical tracers in the downhole environment containing residually trapped supercritical CO2 and formation water, it is necessary to determine the supercritical CO2/water partition coefficients. We have previously determined these in the laboratory (Myers et al., 2012) and they are used here to model the tracer behaviour and provide an estimate of the residual CO2 saturation. Two different computational simulators were used to analyse the tracer breakthrough profiles. The first is based on simple chromatographic retardation and has been used extensively in single well chemical tracer tests to determine residual oil saturation and the second is based on TOUGH2. The estimates of residual saturation given by these models were similar giving a very low residual CO2 saturation value. We suspect that this low value might be due to CO2 being inadvertently dissolved in the near wellbore region prior to this test. This possible dissolution of CO2 may be attributed to the complexity of the multi-test sequence (including other tracer tests prior to this particular test) used in the overall program at of the Residual Gas Saturation and Dissolution Test. References Myers, M., Stalker, L., Ross, A., Dyt, C., Ho, K.-B., 2012. Method for the determination of residual carbon dioxide saturation using reactive ester tracers. Applied Geochemistry 27, 2148-2156.

Progress toward the determination of correct classification rates in fire debris analysis.

PubMed

Waddell, Erin E; Song, Emma T; Rinke, Caitlin N; Williams, Mary R; Sigman, Michael E

2013-07-01

Principal components analysis (PCA), linear discriminant analysis (LDA), and quadratic discriminant analysis (QDA) were used to develop a multistep classification procedure for determining the presence of ignitable liquid residue in fire debris and assigning any ignitable liquid residue present into the classes defined under the American Society for Testing and Materials (ASTM) E 1618-10 standard method. A multistep classification procedure was tested by cross-validation based on model data sets comprised of the time-averaged mass spectra (also referred to as total ion spectra) of commercial ignitable liquids and pyrolysis products from common building materials and household furnishings (referred to simply as substrates). Fire debris samples from laboratory-scale and field test burns were also used to test the model. The optimal model's true-positive rate was 81.3% for cross-validation samples and 70.9% for fire debris samples. The false-positive rate was 9.9% for cross-validation samples and 8.9% for fire debris samples. © 2013 American Academy of Forensic Sciences.

Comparison of green sample preparation techniques in the analysis of pyrethrins and pyrethroids in baby food by liquid chromatography-tandem mass spectrometry.

PubMed

Petrarca, Mateus Henrique; Ccanccapa-Cartagena, Alexander; Masiá, Ana; Godoy, Helena Teixeira; Picó, Yolanda

2017-05-12

A new selective and sensitive liquid chromatography triple quadrupole mass spectrometry method was developed for simultaneous analysis of natural pyrethrins and synthetic pyrethroids residues in baby food. In this study, two sample preparation methods based on ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) and salting-out assisted liquid-liquid extraction (SALLE) were optimized, and then, compared regarding the performance criteria. Appropriate linearity in solvent and matrix-based calibrations, and suitable recoveries (75-120%) and precision (RSD values≤16%) were achieved for selected analytes by any of the sample preparation procedures. Both methods provided the analytical selectivity required for the monitoring of the insecticides in fruit-, cereal- and milk-based baby foods. SALLE, recognized by cost-effectiveness, and simple and fast execution, provided a lower enrichment factor, consequently, higher limits of quantification (LOQs) were obtained. Some of them too high to meet the strict legislation regarding baby food. Nonetheless, the combination of ultrasound and DLLME also resulted in a high sample throughput and environmental-friendly method, whose LOQs were lower than the default maximum residue limit (MRL) of 10μgkg -1 set by European Community for baby foods. In the commercial baby foods analyzed, cyhalothrin and etofenprox were detected in different samples, demonstrating the suitability of proposed method for baby food control. Copyright © 2017 Elsevier B.V. All rights reserved.

An Improved Sparse Representation over Learned Dictionary Method for Seizure Detection.

PubMed

Li, Junhui; Zhou, Weidong; Yuan, Shasha; Zhang, Yanli; Li, Chengcheng; Wu, Qi

2016-02-01

Automatic seizure detection has played an important role in the monitoring, diagnosis and treatment of epilepsy. In this paper, a patient specific method is proposed for seizure detection in the long-term intracranial electroencephalogram (EEG) recordings. This seizure detection method is based on sparse representation with online dictionary learning and elastic net constraint. The online learned dictionary could sparsely represent the testing samples more accurately, and the elastic net constraint which combines the 11-norm and 12-norm not only makes the coefficients sparse but also avoids over-fitting problem. First, the EEG signals are preprocessed using wavelet filtering and differential filtering, and the kernel function is applied to make the samples closer to linearly separable. Then the dictionaries of seizure and nonseizure are respectively learned from original ictal and interictal training samples with online dictionary optimization algorithm to compose the training dictionary. After that, the test samples are sparsely coded over the learned dictionary and the residuals associated with ictal and interictal sub-dictionary are calculated, respectively. Eventually, the test samples are classified as two distinct categories, seizure or nonseizure, by comparing the reconstructed residuals. The average segment-based sensitivity of 95.45%, specificity of 99.08%, and event-based sensitivity of 94.44% with false detection rate of 0.23/h and average latency of -5.14 s have been achieved with our proposed method.

Air Quality Inside Police Drug Safes and Drug Storage Areas.

PubMed

Doran, Gregory S; Deans, Ralph; De Filippis, Carlo; Kostakis, Chris; Howitt, Julia A

2018-06-01

Storage of drug-based evidence inside sealed safes may allow chemical vapors to accumulate, creating concerns of drug exposure by inhalation, or the possibility of cross-contamination of drug evidence. Air samples were taken from inside eight drug safes and one small storage room at nine city and country police stations, as well as a large centralized drug evidence storage vault, in New South Wales (NSW), Australia. Sorbent tubes containing charcoal were used to determine whether any drug residues could be detected in the air, and to identify the types of chemicals present. Carbon traps were extracted and analyzed by LC-MS-MS for a suite of 22 licit and illicit drug residues and 2 metabolites. Carbon traps and SPME fibers were also analyzed by GC-MS for general volatile organic compound (VOC) residues. No detectable drug residues, either as airborne dust or vapor, were found in the safes, the storage room or the large central repository vault. No drugs were detected in any of the 34 urine samples collected at 8 of the 10 sampling locations, while only one of the five hair samples was positive for cocaine (9 pg/mg) provided by police exhibit officers at 3 of the 10 sampling locations. VOC analysis identified a variety of solvents associated with drug manufacture, plasticisers, personal care products and volatiles associated with plants such as cannabis. The results indicate that strong chemical odours emanating from drug safes are unlikely to be drug residues due to low volatility of drugs, and are more likely VOCs associated with their manufacture or from plant growing operations. Consideration should be given to the quality of air flow in rooms in which safes are housed and the use of air filtering inside safes to reduce the likelihood of VOC accumulation, and therefore the risk of human exposure.

Research on identification and determination of mixed pesticides in apples using surface enhanced Raman spectroscopy

NASA Astrophysics Data System (ADS)

Zhai, Chen; Li, Yongyu; Peng, Yankun; Xu, Tianfeng; Dhakal, Sagar; Chao, Kuanglin; Qin, Jianwei

2015-05-01

Residual pesticides in fruits and vegetables have become one of the major food safety concerns around the world. At present, routine analytical methods used for the determination of pesticide residue on the surface of fruits and vegetables are destructive, complex, time-consuming, high cost and not environmentally friendly. In this study, a novel Surface Enhanced Raman Spectroscopy (SERS) method with silver colloid was developed for fast and sensitive nondestructive detection of residual pesticides in fruits and vegetables by using a self-developed Raman system. SERS technology is a combination of Raman spectroscopy and nanotechnology. SERS can greatly enhance the Raman signal intensity, achieve single-molecule detection, and has a simple sample pre-treatment characteristic of high sensitivity and no damage; in recent years it has begun to be used in food safety testing research. In this study a rapid and sensitive method was developed to identify and analyze mixed pesticides of chlorpyrifos, deltamethrin and acetamiprid in apple samples by SERS. Silver colloid was used for SERS measurement by hydroxylamine hydrochloride reduced. The advantages of this method are seen in its fast preparation at room temperature, good reproducibility and immediate applicability. Raman spectrum is highly interfered by noise signals and fluorescence background, which make it too complex to get good result. In this study the noise signals and fluorescence background were removed by Savitzky-Golay filter and min-max signal adaptive zooming method. Under optimal conditions, pesticide residues in apple samples can be detected by SERS at 0.005 μg/cm2 and 0.002 μg/cm2 for individual acetamiprid and thiram, respectively. When mixing the two pesticides at low concentrations, their characteristic peaks can still be identified from the SERS spectrum of the mixture. Based on the synthesized material and its application in SERS operation, the method represents an ultrasensitive SERS performance in apple samples detection without sample pre-treatment, which indicates that it could be served as a useful means in monitoring pesticide residues.

Internal Stress Distribution Measurement of TIG Welded SUS304 Samples Using Neutron Diffraction Technique

NASA Astrophysics Data System (ADS)

Muslih, M. Refai; Sumirat, I.; Sairun; Purwanta

2008-03-01

The distribution of residual stress of SUS304 samples that were undergone TIG welding process with four different electric currents has been measured. The welding has been done in the middle part of the samples that was previously grooved by milling machine. Before they were welded the samples were annealed at 650 degree Celsius for one hour. The annealing process was done to eliminate residual stress generated by grooving process so that the residual stress within the samples was merely produced from welding process. The calculation of distribution of residual stress was carried out by measuring the strains within crystal planes of Fe(220) SUS304. Strain, Young modulus, and Poisson ratio of Fe(220) SUS304 were measured using DN1-M neutron diffractometer. Young modulus and Poisson ratio of Fe(220) SUS304 sample were measured in-situ. The result of calculations showed that distribution of residual stress of SUS304 in the vicinity of welded area is influenced both by treatments given at the samples-making process and by the electric current used during welding process.

A web server for analysis, comparison and prediction of protein ligand binding sites.

PubMed

Singh, Harinder; Srivastava, Hemant Kumar; Raghava, Gajendra P S

2016-03-25

One of the major challenges in the field of system biology is to understand the interaction between a wide range of proteins and ligands. In the past, methods have been developed for predicting binding sites in a protein for a limited number of ligands. In order to address this problem, we developed a web server named 'LPIcom' to facilitate users in understanding protein-ligand interaction. Analysis, comparison and prediction modules are available in the "LPIcom' server to predict protein-ligand interacting residues for 824 ligands. Each ligand must have at least 30 protein binding sites in PDB. Analysis module of the server can identify residues preferred in interaction and binding motif for a given ligand; for example residues glycine, lysine and arginine are preferred in ATP binding sites. Comparison module of the server allows comparing protein-binding sites of multiple ligands to understand the similarity between ligands based on their binding site. This module indicates that ATP, ADP and GTP ligands are in the same cluster and thus their binding sites or interacting residues exhibit a high level of similarity. Propensity-based prediction module has been developed for predicting ligand-interacting residues in a protein for more than 800 ligands. In addition, a number of web-based tools have been integrated to facilitate users in creating web logo and two-sample between ligand interacting and non-interacting residues. In summary, this manuscript presents a web-server for analysis of ligand interacting residue. This server is available for public use from URL http://crdd.osdd.net/raghava/lpicom .

Resilience, Vulnerability and Residual Threat: An Assessment from Indian Sundarban

NASA Astrophysics Data System (ADS)

Ghosh, T.

2016-12-01

The estuarine islands within Indian Sundarban are extremely vulnerable due to climate change, erosion, flooding and increasing population pressure. Around 4.6 million people are living under constant threat of climatic shocks, affecting their farm based economy and dependency on forest resources for their livelihood. This paper attempts to focus on the dynamics of system's resilience in the backdrop of higher level of vulnerability. Globally the assessment of island vulnerability is generally more focused towards the climate change impacts, rather than taking into account other determining drivers with proper weightage. Three estuarine islands namely Sagar, Ghoramara and Mousani at the western part of Indian Sundarban Delta (ISD) have been chosen for this study to derive the indicator based scoring method using the household survey data from twenty seven (27) sampled `Mouza' (lowest administrative boundary; village) with cluster random sampling. Vulnerability and resilience of these islands have been calculated using the indicators like housing condition, electrification, population density, accretion, adult secondary education level, percentage of people `Below Poverty Line' (BPL) based on per capita income. Residual threats for these islands have been obtained by subtracting the score of resilience and vulnerability of the system. Result suggests that all these islands are in less resilient condition to combat the negative impact of the influencing factors. Sapkhali, Ghoramara, Bankimnagar, Shibpur and Baliara are becoming sensitive from excess residual threats. This study is an initiation for identifying the thrust areas need to address with effective policy adaptation, necessary to minimize the existing vulnerable conditions in these islands. Key words: Vulnerability, Resilience, Residual threat, Indian Sundarban

Trend-Residual Dual Modeling for Detection of Outliers in Low-Cost GPS Trajectories

PubMed Central

Chen, Xiaojian; Cui, Tingting; Fu, Jianhong; Peng, Jianwei; Shan, Jie

2016-01-01

Low-cost GPS (receiver) has become a ubiquitous and integral part of our daily life. Despite noticeable advantages such as being cheap, small, light, and easy to use, its limited positioning accuracy devalues and hampers its wide applications for reliable mapping and analysis. Two conventional techniques to remove outliers in a GPS trajectory are thresholding and Kalman-based methods, which are difficult in selecting appropriate thresholds and modeling the trajectories. Moreover, they are insensitive to medium and small outliers, especially for low-sample-rate trajectories. This paper proposes a model-based GPS trajectory cleaner. Rather than examining speed and acceleration or assuming a pre-determined trajectory model, we first use cubic smooth spline to adaptively model the trend of the trajectory. The residuals, i.e., the differences between the trend and GPS measurements, are then further modeled by time series method. Outliers are detected by scoring the residuals at every GPS trajectory point. Comparing to the conventional procedures, the trend-residual dual modeling approach has the following features: (a) it is able to model trajectories and detect outliers adaptively; (b) only one critical value for outlier scores needs to be set; (c) it is able to robustly detect unapparent outliers; and (d) it is effective in cleaning outliers for GPS trajectories with low sample rates. Tests are carried out on three real-world GPS trajectories datasets. The evaluation demonstrates an average of 9.27 times better performance in outlier detection for GPS trajectories than thresholding and Kalman-based techniques. PMID:27916944

The impact of seasonal variation on organochlorine pesticide residues in buffalo and cow milk of selected dairy farms from Faisalabad region.

PubMed

Sajid, Muhammad Wasim; Shamoon, Muhammad; Randhawa, Muhammad Atif; Asim, Muhammad; Chaudhry, Abdul Shakoor

2016-10-01

Two hundred milk samples from 20 randomly selected dairy farms were screened for the incidence of organochlorine pesticide residues to evaluate the safety of milk in Faisalabad region. The results revealed that overall buffalo milk samples in winter (85 %) and in summer (78 %) were more contaminated as compared to cow milk samples 83 and 75 % in respective seasons. The residues of cyhalothrin were found only in summer season in milk of both species. Permethrin residues were detected at higher levels than perfinofos while DDT and methamedophos were found undetectable. The mean levels of permethrin were 0.042 and 0.033 mg kg -1 in buffalo milk samples and 0.045 and 0.043 mg kg -1 in cow milk in winter and summer season, respectively. Perfinofos residues were found to be the least contaminated pesticides with mean values of 0.0006 and 0.0013 mg kg -1 , respectively in winter season, and 0.004 and 0.0025 mg kg -1 in summer season. All analysed pesticide residues in milk samples in both seasons were below the maximum residual limit (MRL) values as described by European Union (EU) but milk samples contaminated with α, β-endosulfan and endosulphate exceeded their respective Food and Agriculture Organization's (FAO) established MRLs both in winter and summer.

Advances in biosensor development for the screening of antibiotic residues in food products of animal origin - A comprehensive review.

PubMed

Gaudin, Valérie

2017-04-15

Antibiotic residues may be found in food of animal origin, since veterinary drugs are used for preventive and curative purposes to treat animals. The control of veterinary drug residues in food is necessary to ensure consumer safety. Screening methods are the first step in the control of antibiotic residues in food of animal origin. Conventional screening methods are based on different technologies, microbiological methods, immunological methods or physico-chemical methods (e.g. thin-layer chromatography, HPLC, LC-MS/MS). Screening methods should be simple, quick, inexpensive and specific, with low detection limits and high sample throughput. Biosensors can meet some of these requirements. Therefore, the development of biosensors for the screening of antibiotic residues has been increasing since the 1980s. The present review provides extensive and up-to-date findings on biosensors for the screening of antibiotic residues in food products of animal origin. Biosensors are constituted of a bioreceptor and a transducer. In the detection of antibiotic residues, even though antibodies were the first bioreceptors to be used, new kinds of bioreceptors are being developed more and more (enzymes, aptamers, MIPs); their advantages and drawbacks are discussed in this review. The different categories of transducers (electrochemical, mass-based biosensors, optical and thermal) and their potential applications for the screening of antibiotic residues in food are presented. Moreover, the advantages and drawbacks of the different types of transducers are discussed. Lastly, outlook and the future development of biosensors for the control of antibiotic residues in food are highlighted. Copyright © 2016. Published by Elsevier B.V.

FastRNABindR: Fast and Accurate Prediction of Protein-RNA Interface Residues.

PubMed

El-Manzalawy, Yasser; Abbas, Mostafa; Malluhi, Qutaibah; Honavar, Vasant

2016-01-01

A wide range of biological processes, including regulation of gene expression, protein synthesis, and replication and assembly of many viruses are mediated by RNA-protein interactions. However, experimental determination of the structures of protein-RNA complexes is expensive and technically challenging. Hence, a number of computational tools have been developed for predicting protein-RNA interfaces. Some of the state-of-the-art protein-RNA interface predictors rely on position-specific scoring matrix (PSSM)-based encoding of the protein sequences. The computational efforts needed for generating PSSMs severely limits the practical utility of protein-RNA interface prediction servers. In this work, we experiment with two approaches, random sampling and sequence similarity reduction, for extracting a representative reference database of protein sequences from more than 50 million protein sequences in UniRef100. Our results suggest that random sampled databases produce better PSSM profiles (in terms of the number of hits used to generate the profile and the distance of the generated profile to the corresponding profile generated using the entire UniRef100 data as well as the accuracy of the machine learning classifier trained using these profiles). Based on our results, we developed FastRNABindR, an improved version of RNABindR for predicting protein-RNA interface residues using PSSM profiles generated using 1% of the UniRef100 sequences sampled uniformly at random. To the best of our knowledge, FastRNABindR is the only protein-RNA interface residue prediction online server that requires generation of PSSM profiles for query sequences and accepts hundreds of protein sequences per submission. Our approach for determining the optimal BLAST database for a protein-RNA interface residue classification task has the potential of substantially speeding up, and hence increasing the practical utility of, other amino acid sequence based predictors of protein-protein and protein-DNA interfaces.

Comparison of different agar diffusion methods for the detection of residues in the kidneys of pigs treated with antimicrobial drugs.

PubMed

Korkeala, H; Sorvettula, O; Mäki-Petäys, O; Hirn, J

1983-01-01

Residue analyses of the kidneys of twenty-six pigs treated with various antimicrobial drugs 20 h before slaughter and of eleven untreated pigs were performed. The effects of storage temperature of the kidneys, and of sampling location, on the residue analysis were also studied. No method alone was sufficient for the detection of residues. Oxytetracycline residues could be detected at pH 6, dihydrostreptomycin residues at pH 8, and sulphonamide residues if trimethoprim was present in the medium. Chloramphenicol, penicillin G procaine, tylosin and lincomycin residues were not detectable with the methods used. The concentration of ampicillin decreased during the storage of samples at +4°C. Most methods also yielded zones of inhibition for the frozen kidneys from untreated pigs. It seems necessary to use agar media of two different pH values: the addition of trimethoprim to the medium is also needed. The use of fresh pig kidneys, and samples containing both kidney medulla and kidney cortex, is recommended in residue analysis. Copyright © 1983. Published by Elsevier Ltd.

Chemical characterization of some aqueous leachates from crop residues in 'CELSS'

NASA Technical Reports Server (NTRS)

Madsen, Brooks C.

1992-01-01

Aqueous leachate samples prepared from crop residues that are produced as a component of the Controlled Ecological Life Support System program designed to support long duration space missions have been compared and general chemical characterization has been accomplished. Solid phase extraction and high performance liquid chromatography were used to accomplish comparisons based on chromatographic and ultraviolet absorption properties of the components that are present. Specific compounds were not identified, however, general composition related to the presence of phenol-like compounds was explored.

Surface electrochemical properties of red mud (bauxite residue): zeta potential and surface charge density.

PubMed

Liu, Yanju; Naidu, Ravendra; Ming, Hui

2013-03-15

The surface electrochemical properties of red mud (bauxite residue) from different alumina refineries in Australia and China were studied by electrophoresis and measuring surface charge density obtained from acid/base potentiometric titrations. The electrophoretic properties were measured from zeta potentials obtained in the presence of 0.01 and 0.001 M KNO(3) over a wide pH range (3.5-10) by titration. The isoelectric point (IEP) values were found to vary from 6.35 to 8.70 for the red mud samples. Further investigation into the surface charge density of one sample (RRM) by acid/base potentiometric titration showed similar results for pH(PZC) with pH(IEP) obtained from electrokinetic measurements. The pH(IEP) determined from zeta potential measurements can be used as a characteristic property of red mud. The minerals contained in red mud contributed to the different values of pH(IEP) of samples obtained from different refineries. Different relationships of pH(IEP) with Al/Fe and Al/Si ratios (molar basis) were also found for different red mud samples. Copyright © 2012 Elsevier Inc. All rights reserved.

Assessment of oxytetracycline and tetracycline antibiotics in manure samples in different cities of Khuzestan Province, Iran.

PubMed

Alavi, Nadali; Babaei, Ali Akbar; Shirmardi, Mohammad; Naimabadi, Abolfazl; Goudarzi, Gholamreza

2015-11-01

Tetracyclines (TCs), a class of antibiotics with a broad spectrum, are the most frequently used antibiotics in animal production. The major concern is that the widespread use of the antibiotics may lead to the emergence of new strains of bacteria that are resistant to these antibiotics. The objective of this study was to determine the residual levels of oxytetracycline and tetracycline in 80 animal manure samples that were collected from the livestock and poultry feedlots in Khuzestan Province. The residual levels of the antibiotics in the samples were extracted by using solid-phase extraction (SPE) method and subsequently were measured by liquid chromatography. Recoveries from the spiked poultry manure samples ranged from 65 to 113% for tetracycline and 86 to 132% for oxytetracycline. Relative standard deviations of the recoveries were less than 5.7% within the same day. Method detection limit (MDL) measured for oxytetracycline and tetracycline in the manure were 0.011 and 0.01 mg/kg, respectively. Analysis of the collected 50 chickens and 30 cow manure samples showed that the highest concentration of tetracycline was related to Behbahan City (5.36 mg/kg) and the lowest concentration was detected for Ramhormoz (0.05 mg/kg). The highest and lowest concentrations of oxytetracycline were respectively observed for Behbahan (13.77 mg/kg) and Ramhormoz (0.047 mg/kg). Based on the results, in chicken manure, there was significant statistical difference between the residual TC concentrations among five cities (p(value) < 0.05). However, no significant relationship was observed between oxytetracyclin (OTC) residual concentrations among five cities (p(value) > 0.05).

STATISTICAL ANALYSIS OF TANK 18F FLOOR SAMPLE RESULTS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Harris, S.

2010-09-02

Representative sampling has been completed for characterization of the residual material on the floor of Tank 18F as per the statistical sampling plan developed by Shine [1]. Samples from eight locations have been obtained from the tank floor and two of the samples were archived as a contingency. Six samples, referred to in this report as the current scrape samples, have been submitted to and analyzed by SRNL [2]. This report contains the statistical analysis of the floor sample analytical results to determine if further data are needed to reduce uncertainty. Included are comparisons with the prior Mantis samples resultsmore » [3] to determine if they can be pooled with the current scrape samples to estimate the upper 95% confidence limits (UCL{sub 95%}) for concentration. Statistical analysis revealed that the Mantis and current scrape sample results are not compatible. Therefore, the Mantis sample results were not used to support the quantification of analytes in the residual material. Significant spatial variability among the current sample results was not found. Constituent concentrations were similar between the North and South hemispheres as well as between the inner and outer regions of the tank floor. The current scrape sample results from all six samples fall within their 3-sigma limits. In view of the results from numerous statistical tests, the data were pooled from all six current scrape samples. As such, an adequate sample size was provided for quantification of the residual material on the floor of Tank 18F. The uncertainty is quantified in this report by an upper 95% confidence limit (UCL{sub 95%}) on each analyte concentration. The uncertainty in analyte concentration was calculated as a function of the number of samples, the average, and the standard deviation of the analytical results. The UCL{sub 95%} was based entirely on the six current scrape sample results (each averaged across three analytical determinations).« less

STATISTICAL ANALYSIS OF TANK 19F FLOOR SAMPLE RESULTS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Harris, S.

2010-09-02

Representative sampling has been completed for characterization of the residual material on the floor of Tank 19F as per the statistical sampling plan developed by Harris and Shine. Samples from eight locations have been obtained from the tank floor and two of the samples were archived as a contingency. Six samples, referred to in this report as the current scrape samples, have been submitted to and analyzed by SRNL. This report contains the statistical analysis of the floor sample analytical results to determine if further data are needed to reduce uncertainty. Included are comparisons with the prior Mantis samples resultsmore » to determine if they can be pooled with the current scrape samples to estimate the upper 95% confidence limits (UCL95%) for concentration. Statistical analysis revealed that the Mantis and current scrape sample results are not compatible. Therefore, the Mantis sample results were not used to support the quantification of analytes in the residual material. Significant spatial variability among the current scrape sample results was not found. Constituent concentrations were similar between the North and South hemispheres as well as between the inner and outer regions of the tank floor. The current scrape sample results from all six samples fall within their 3-sigma limits. In view of the results from numerous statistical tests, the data were pooled from all six current scrape samples. As such, an adequate sample size was provided for quantification of the residual material on the floor of Tank 19F. The uncertainty is quantified in this report by an UCL95% on each analyte concentration. The uncertainty in analyte concentration was calculated as a function of the number of samples, the average, and the standard deviation of the analytical results. The UCL95% was based entirely on the six current scrape sample results (each averaged across three analytical determinations).« less

XAFS SPECTROSCOPY RESULTS FOR PM SAMPLES FROM RESIDUAL FUEL OIL

EPA Science Inventory

X-ray absorption fine structure (XAFS spectroscopy data were obtained from particulate samples produced by the combustion of residual fuel oil in a 732-kW fire-tube boiler at EPA's National Risk Management Research Laboratory in North Carolina. Residual oil flyash (ROFA) from fo...

Pesticide Residues in Honey from the Major Honey Producing Forest Belts in Ghana.

PubMed

Darko, Godfred; Addai Tabi, Jonah; Adjaloo, Michael Kodwo; Borquaye, Lawrence Sheringham

2017-01-01

Concentrations of pesticides residues in honey sampled from the major honey producing forest belts in Ghana were determined. Samples were purposively collected and extracted using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method and analysed for synthetic pyrethroids, organochlorine, and organophosphate pesticide residues. Aldrin, γ -HCH, β -HCH, ∑endosulfan, cyfluthrin, cypermethrin, deltamethrin, permethrin methoxychlor, ∑DDT, chlorpyrifos, fenvalerate, malathion, dimethoate, and diazinon were all detected at the concentration of 0.01 mg/kg, while cyfluthrin and permethrin were detected at mean concentrations of 0.02 and 0.04 mg/kg, respectively. All the pesticide residues detected were very low and below their respective maximum residue limits set by the European Union. Hence, pesticide residues in honey samples analyzed do not pose any health risk to consumers.

Baseline toxicity of a chlorobenzene mixture and total body residues measured and estimated with solid-phase microextraction.

PubMed

Leslie, Heather A; Hermens, Joop L M; Kraak, Michiel H S

2004-08-01

Body residues of compounds with a narcotic mode of action that exceed critical levels result in baseline toxicity in organisms. Previous studies have shown that internal concentrations in organisms also can be estimated by way of passive sampling. In this experiment, solid-phase microextraction (SPME) fibers were used as a tool to estimate the body residues, which were then compared to measured levels. Past application of SPME fibers in the assessment of toxicity risk of samples has focused on separate exposure of fibers and organisms, often necessitated by the amount of agitation needed in order to achieve steady state in the fibers within a convenient time period. Uptake kinetic studies have shown that in SPME fibers with thin coatings, equilibrium concentrations can be reached without agitation within the time frame of a toxicity test. In contrast to toxicity experiments to date, the SPME fibers in the current study were exposed concomitantly to the test water with the organisms, ensuring an exposure under the exact same conditions. Fibers and two aquatic invertebrate species were exposed to a mixture of four chlorobenzenes with a narcotic mode of action. The total body residue of these compounds in the organisms was determined, as was the acute toxicity resulting from the accumulation. The total body residues of both species were correlated to the total concentrations in SPME fibers. It was concluded that toxicity could be predicted based on total body residue (TBR) estimates from fiber concentrations.

Presence and biological activity of antibiotics used in fuel ethanol and corn co-product production.

PubMed

Compart, D M Paulus; Carlson, A M; Crawford, G I; Fink, R C; Diez-Gonzalez, F; Dicostanzo, A; Shurson, G C

2013-05-01

Antibiotics are used in ethanol production to control bacteria from competing with yeast for nutrients during starch fermentation. However, there is no published scientific information on whether antibiotic residues are present in distillers grains (DG), co-products from ethanol production, or whether they retain their biological activity. Therefore, the objectives of this study were to quantify concentrations of various antibiotic residues in DG and determine whether residues were biologically active. Twenty distillers wet grains and 20 distillers dried grains samples were collected quarterly from 9 states and 43 ethanol plants in the United States. Samples were analyzed for DM, CP, NDF, crude fat, S, P, and pH to describe the nutritional characteristics of the samples evaluated. Samples were also analyzed for the presence of erythromycin, penicillin G, tetracycline, tylosin, and virginiamycin M1, using liquid chromatography and mass spectrometry. Additionally, virginiamycin residues were determined, using a U.S. Food and Drug Administration-approved bioassay method. Samples were extracted and further analyzed for biological activity by exposing the sample extracts to 10(4) to 10(7) CFU/mL concentrations of sentinel bacterial strains Escherichia coli ATCC 8739 and Listeria monocytogenes ATCC 19115. Extracts that inhibited bacterial growth were considered to have biological activity. Physiochemical characteristics varied among samples but were consistent with previous findings. Thirteen percent of all samples contained low (≤1.12 mg/kg) antibiotic concentrations. Only 1 sample extract inhibited growth of Escherichia coli at 10(4) CFU/mL, but this sample contained no detectable concentrations of antibiotic residues. No extracts inhibited Listeria monocytogenes growth. These data indicate that the likelihood of detectable concentrations of antibiotic residues in DG is low; and if detected, they are found in very low concentrations. The inhibition in only 1 DG sample by sentinel bacteria suggests that antibiotic residues in DG were inactivated during the production process or are present in sublethal concentrations.

Residue analysis and persistence evaluation of fipronil and its metabolites in cotton using high-performance liquid chromatography-tandem mass spectrometry.

PubMed

Wu, Xiaohu; Yu, Yang; Xu, Jun; Dong, Fengshou; Liu, Xingang; Du, Pengqiang; Wei, Dongmei; Zheng, Yongquan

2017-01-01

A simple residue analytical method based on the QuEChERS approach and high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) detection was developed for the analysis of fipronil and its three metabolites in cottonseed, cotton plant and soil. The average recoveries of four test compounds from all three matrices were 78.6-108.9% at the level of 0.005 to 0.5 mg/kg, with an RSD in the range of 0.6 to 13.7%. The limit of quantification (LOQ) of the four test compounds ranged from 0.005 to 0.01 mg/kg. The results of the residual dynamics experiments showed that fipronil dissipated rapidly in cotton plants and soil and that oxidation and photolysis were the main degradation pathways. Moreover, the bi-exponential models demonstrated a good fit of the measured data for fipronil in cotton plants and soil, with R2 in the range of 0.8989 to 0.9989. Furthermore, a total of 40 samples of cottonseed from Shandong Province were analyzed, and all of the samples were free from the four test compound residues.

Residue analysis and persistence evaluation of fipronil and its metabolites in cotton using high-performance liquid chromatography-tandem mass spectrometry

PubMed Central

Wu, Xiaohu; Yu, Yang; Xu, Jun; Dong, Fengshou; Liu, Xingang; Du, Pengqiang; Wei, Dongmei; Zheng, Yongquan

2017-01-01

A simple residue analytical method based on the QuEChERS approach and high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) detection was developed for the analysis of fipronil and its three metabolites in cottonseed, cotton plant and soil. The average recoveries of four test compounds from all three matrices were 78.6–108.9% at the level of 0.005 to 0.5 mg/kg, with an RSD in the range of 0.6 to 13.7%. The limit of quantification (LOQ) of the four test compounds ranged from 0.005 to 0.01 mg/kg. The results of the residual dynamics experiments showed that fipronil dissipated rapidly in cotton plants and soil and that oxidation and photolysis were the main degradation pathways. Moreover, the bi-exponential models demonstrated a good fit of the measured data for fipronil in cotton plants and soil, with R2 in the range of 0.8989 to 0.9989. Furthermore, a total of 40 samples of cottonseed from Shandong Province were analyzed, and all of the samples were free from the four test compound residues. PMID:28291815

Path length dependent neutron diffraction peak shifts observed during residual strain measurements in U–8 wt% Mo castings

DOE PAGES

Steiner, M. A.; Bunn, J. R.; Einhorn, J. R.; ...

2017-05-16

This study reports an angular diffraction peak shift that scales linearly with the neutron beam path length traveled through a diffracting sample. This shift was observed in the context of mapping the residual stress state of a large U–8 wt% Mo casting, as well as during complementary measurements on a smaller casting of the same material. If uncorrected, this peak shift implies a non-physical level of residual stress. A hypothesis for the origin of this shift is presented, based upon non-ideal focusing of the neutron monochromator in combination with changes to the wavelength distribution reaching the detector due to factorsmore » such as attenuation. The magnitude of the shift is observed to vary linearly with the width of the diffraction peak reaching the detector. Consideration of this shift will be important for strain measurements requiring long path lengths through samples with significant attenuation. This effect can probably be reduced by selecting smaller voxel slit widths.« less

Colling Wipe Samples for VX Analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Koester, C; Hoppes, W G

2010-02-11

This standard operating procedure (SOP) provides uniform procedures for the collection of wipe samples of VX residues from surfaces. Personnel may use this procedure to collect and handle wipe samples in the field. Various surfaces, including building materials (wood, metal, tile, vinyl, etc.) and equipment, may be sampled based on this procedure. The purpose of such sampling is to determine whether or not the relevant surfaces are contaminated, to determine the extent of their contamination, to evaluate the effectiveness of decontamination procedures, and to determine the amount of contaminant that might present as a contact hazard.

Evaluation of oriented lysozyme immobilized with monoclonal antibody

NASA Astrophysics Data System (ADS)

Aoyagi, Satoka; Okada, Keigo; Shigyo, Ayako; Man, Naoki; Karen, Akiya

2008-12-01

The orientation of a lysozyme immobilized with a monoclonal antibody was evaluated based on determination of the uppermost surface structure using time-of-flight secondary ion mass spectrometry (TOF-SIMS). Specific peaks of the oriented lysozyme immobilized with monoclonal anti-lysozyme antibody were obtained in comparison with reference samples, non-oriented immobilized lysozyme and immobilized anti-lysozyme antibody. All samples were freeze-dried before TOF-SIMS measurement, and then each sample was measured using TOF-SIMS with a bismuth cluster ion source. TOF-SIMS spectra were analyzed to select peaks specific to the oriented immobilized lysozyme as well as to identify their chemical formula and ensemble of amino acids. The possible chemical formulae of the lysozyme fragments were then investigated with an element matching program and a residue matching program. The results from TOF-SIMS spectra analysis were compared to the amino acid sequence of the lysozyme and its three-dimensional structure registered in the protein data bank. Finally, the fragment-ion-generating regions of the oriented immobilized lysozyme were determined based on the suggested residues and the three-dimensional structure.

Occurrence of pesticide residues in fruiting vegetables from production farms in south-eastern region of Poland

PubMed

Słowik-Borowiec, Magdalena; Szpyrka, Ewa; Rupar, Julian; Podbielska, Magdalena; Matyaszek, Aneta

Considering the fact that pesticides are commonly used in agriculture, continuous monitoring of these substances in food products is of great significance. Residues of these substances can be present in crops after harvest. The aim of this study was to evaluate presence of pesticide residues in fruiting vegetables from production farms in south-eastern region of Poland in 2012–2015. 138 samples were tested using accredited test methods. The monitoring programme covered determination of 242 pesticides. The tests covered tomato, cucumber and pepper crops. The test results were interpreted in accordance with criteria included in the European Commission recommendations published in the document SANCO/12571/2013 (now superseded by Document SANTE 2015), as well as on a basis of the maximum residue levels in force in the EU Member States. Pesticide residues were found in 47 samples, representing 34% of all tested samples. 17 active substances were found, belonging to fungicides and insecticides. Azoxystrobin (38%), boscalid (28%) and chlorothalonil (21%) were most commonly found in fruiting vegetables testing samples. Non-compliances related to use of plant protection product not authorized for protection of a given crop were observed in 6% of analysed samples. However, pesticide residues of fruiting vegetables in quantities that exceed the maximum residue levels (NDP, ang. MRLs), as well as substances which use for plant protection is forbidden were no found. Crops monitoring is used to determine to what extent such products are contaminated with pesticide residues, and ensures protection of customer health.

Short communication: Macrocyclic lactone residues in butter from Brazilian markets.

PubMed

Macedo, Fabio; Marsico, Eliane Teixeira; Conte-Júnior, Carlos Adam; de Almeida Furtado, Leonardo; Brasil, Taila Figueredo; Pereira Netto, Annibal Duarte

2015-06-01

Macrocyclic lactones (ML) are commonly used in drug formulations for the treatment of parasites in cattle. In Brazil, except for drugs (or formulations) with long-term (half-life) effects, ML are registered for use in bovines. Indiscriminate use of ML may result in the presence of residues in milk and dairy products due to their lipophilic properties and thermal stability. This study applied a method of liquid chromatography with fluorimetric detection, recently developed and validated for the determination of residues of abamectin, doramectin, ivermectin, and moxidectin in butter. The method was applied to 38 samples of commercial butter purchased in the metropolitan area of Rio de Janeiro, Brazil, between June and September 2013, analyzed in triplicate. Ivermectin was detected in 89.5% of the samples, with concentrations between 0.3 and 119.4 µg/kg; 76.3% of the samples contained doramectin (0.6 to 64.7 µg/kg) and 55.2% contained abamectin (0.7 to 4.5 µg/kg). Most butter samples (76.3%) contained residues of more than 1 ML; however, no residues of moxidectin were detected. The results showed a high incidence of the presence of avermectins in butter samples. Butter is not included in the Brazilian National Plan for Control of Residues and Contaminants in Animal Products. As ML residues concentrate in lipophilic compounds, butter and other fatty dairy products should be screened for the presence of ML residues. Copyright © 2015 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Determination of residual solvents in bulk pharmaceuticals by thermal desorption/gas chromatography/mass spectrometry.

PubMed

Urakami, K; Saito, Y; Fujiwara, Y; Watanabe, C; Umemoto, K; Godo, M; Hashimoto, K

2000-12-01

Thermal desorption (TD) techniques followed by capillary GC/MS were applied for the analysis of residual solvents in bulk pharmaceuticals. Solvents desorbed from samples by heating were cryofocused at the head of a capillary column prior to GC/MS analysis. This method requires a very small amount of sample and no sample pretreatment. Desorption temperature was set at the point about 20 degrees C higher than the melting point of each sample individually. The relative standard deviations of this method tested by performing six consecutive analyses of 8 different samples were 1.1 to 3.1%, and analytical results of residual solvents were in agreement with those obtained by direct injection of N,N-dimethylformamide solution of the samples into the GC. This novel TD/GC/MS method was demonstrated to be very useful for the identification and quantification of residual solvents in bulk pharmaceuticals.

DDT-based indoor residual spraying suboptimal for visceral leishmaniasis elimination in India

PubMed Central

Coleman, Michael; Foster, Geraldine M.; Deb, Rinki; Pratap Singh, Rudra; Ismail, Hanafy M.; Shivam, Pushkar; Ghosh, Ayan Kumar; Dunkley, Sophie; Kumar, Vijay; Coleman, Marlize; Hemingway, Janet; Paine, Mark J. I.; Das, Pradeep

2015-01-01

Indoor residual spraying (IRS) is used to control visceral leishmaniasis (VL) in India, but it is poorly quality assured. Quality assurance was performed in eight VL endemic districts in Bihar State, India, in 2014. Residual dichlorodiphenyltrichloroethane (DDT) was sampled from walls using Bostik tape discs, and DDT concentrations [grams of active ingredient per square meter (g ai/m2)] were determined using HPLC. Pre-IRS surveys were performed in three districts, and post-IRS surveys were performed in eight districts. A 20% threshold above and below the target spray of 1.0 g ai/m2 was defined as “in range.” The entomological assessments were made in four districts in IRS and non-IRS villages. Vector densities were measured: pre-IRS and 1 and 3 mo post-IRS. Insecticide susceptibility to 4% DDT and 0.05% deltamethrin WHO-impregnated papers was determined with wild-caught sand flies. The majority (329 of 360, 91.3%) of pre-IRS samples had residual DDT concentrations of <0.1 g ai/m2. The mean residual concentration of DDT post-IRS was 0.37 g ai/m2; 84.9% of walls were undersprayed, 7.4% were sprayed in range, and 7.6% were oversprayed. The abundance of sand flies in IRS and non-IRS villages was significantly different at 1 mo post-IRS only. Sand flies were highly resistant to DDT but susceptible to deltamethrin. The Stockholm Convention, ratified by India in 2006, calls for the complete phasing out of DDT as soon as practical, with limited use in the interim where no viable IRS alternatives exist. Given the poor quality of the DDT-based IRS, ready availability of pyrethroids, and susceptibility profile of Indian sand flies, the continued use of DDT in this IRS program is questionable. PMID:26124110

DDT-based indoor residual spraying suboptimal for visceral leishmaniasis elimination in India.

PubMed

Coleman, Michael; Foster, Geraldine M; Deb, Rinki; Pratap Singh, Rudra; Ismail, Hanafy M; Shivam, Pushkar; Ghosh, Ayan Kumar; Dunkley, Sophie; Kumar, Vijay; Coleman, Marlize; Hemingway, Janet; Paine, Mark J I; Das, Pradeep

2015-07-14

Indoor residual spraying (IRS) is used to control visceral leishmaniasis (VL) in India, but it is poorly quality assured. Quality assurance was performed in eight VL endemic districts in Bihar State, India, in 2014. Residual dichlorodiphenyltrichloroethane (DDT) was sampled from walls using Bostik tape discs, and DDT concentrations [grams of active ingredient per square meter (g ai/m(2))] were determined using HPLC. Pre-IRS surveys were performed in three districts, and post-IRS surveys were performed in eight districts. A 20% threshold above and below the target spray of 1.0 g ai/m(2) was defined as "in range." The entomological assessments were made in four districts in IRS and non-IRS villages. Vector densities were measured: pre-IRS and 1 and 3 mo post-IRS. Insecticide susceptibility to 4% DDT and 0.05% deltamethrin WHO-impregnated papers was determined with wild-caught sand flies. The majority (329 of 360, 91.3%) of pre-IRS samples had residual DDT concentrations of <0.1 g ai/m(2). The mean residual concentration of DDT post-IRS was 0.37 g ai/m(2); 84.9% of walls were undersprayed, 7.4% were sprayed in range, and 7.6% were oversprayed. The abundance of sand flies in IRS and non-IRS villages was significantly different at 1 mo post-IRS only. Sand flies were highly resistant to DDT but susceptible to deltamethrin. The Stockholm Convention, ratified by India in 2006, calls for the complete phasing out of DDT as soon as practical, with limited use in the interim where no viable IRS alternatives exist. Given the poor quality of the DDT-based IRS, ready availability of pyrethroids, and susceptibility profile of Indian sand flies, the continued use of DDT in this IRS program is questionable.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Negrete, Oscar A.; Branda, Catherine; Hardesty, Jasper O. E.

In the response to and recovery from a critical homeland security event involving deliberate or accidental release of biological agents, initial decontamination efforts are necessarily followed by tests for the presence of residual live virus or bacteria. Such 'clearance sampling' should be rapid and accurate, to inform decision makers as they take appropriate action to ensure the safety of the public and of operational personnel. However, the current protocol for clearance sampling is extremely time-intensive and costly, and requires significant amounts of laboratory space and capacity. Detection of residual live virus is particularly problematic and time-consuming, as it requires evaluationmore » of replication potential within a eukaryotic host such as chicken embryos. The intention of this project was to develop a new method for clearance sampling, by leveraging Sandia's expertise in the biological and material sciences in order to create a C. elegans-based foam that could be applied directly to the entire contaminated area for quick and accurate detection of any and all residual live virus by means of a fluorescent signal. Such a novel technology for rapid, on-site detection of live virus would greatly interest the DHS, DoD, and EPA, and hold broad commercial potential, especially with regard to the transportation industry.« less

Properties of Soil Pore Space Regulate Pathways of Plant Residue Decomposition and Community Structure of Associated Bacteria

PubMed Central

Negassa, Wakene C.; Guber, Andrey K.; Kravchenko, Alexandra N.; Marsh, Terence L.; Hildebrandt, Britton; Rivers, Mark L.

2015-01-01

Physical protection of soil carbon (C) is one of the important components of C storage. However, its exact mechanisms are still not sufficiently lucid. The goal of this study was to explore the influence of soil structure, that is, soil pore spatial arrangements, with and without presence of plant residue on (i) decomposition of added plant residue, (ii) CO2 emission from soil, and (iii) structure of soil bacterial communities. The study consisted of several soil incubation experiments with samples of contrasting pore characteristics with/without plant residue, accompanied by X-ray micro-tomographic analyses of soil pores and by microbial community analysis of amplified 16S–18S rRNA genes via pyrosequencing. We observed that in the samples with substantial presence of air-filled well-connected large (>30 µm) pores, 75–80% of the added plant residue was decomposed, cumulative CO2 emission constituted 1,200 µm C g-1 soil, and movement of C from decomposing plant residue into adjacent soil was insignificant. In the samples with greater abundance of water-filled small pores, 60% of the added plant residue was decomposed, cumulative CO2 emission constituted 2,000 µm C g-1 soil, and the movement of residue C into adjacent soil was substantial. In the absence of plant residue the influence of pore characteristics on CO2 emission, that is on decomposition of the native soil organic C, was negligible. The microbial communities on the plant residue in the samples with large pores had more microbial groups known to be cellulose decomposers, that is, Bacteroidetes, Proteobacteria, Actinobacteria, and Firmicutes, while a number of oligotrophic Acidobacteria groups were more abundant on the plant residue from the samples with small pores. This study provides the first experimental evidence that characteristics of soil pores and their air/water flow status determine the phylogenetic composition of the local microbial community and directions and magnitudes of soil C decomposition processes. PMID:25909444

Properties of soil pore space regulate pathways of plant residue decomposition and community structure of associated bacteria

DOE PAGES

Negassa, Wakene C.; Guber, Andrey K.; Kravchenko, Alexandra N.; ...

2015-07-01

Physical protection of soil carbon (C) is one of the important components of C storage. However, its exact mechanisms are still not sufficiently lucid. The goal of this study was to explore the influence of soil structure, that is, soil pore spatial arrangements, with and without presence of plant residue on (i) decomposition of added plant residue, (ii) CO₂ emission from soil, and (iii) structure of soil bacterial communities. The study consisted of several soil incubation experiments with samples of contrasting pore characteristics with/without plant residue, accompanied by X-ray micro-tomographic analyses of soil pores and by microbial community analysis ofmore » amplified 16S–18S rRNA genes via pyrosequencing. We observed that in the samples with substantial presence of air-filled well-connected large (>30 µm) pores, 75–80% of the added plant residue was decomposed, cumulative CO₂ emission constituted 1,200 µm C g⁻¹ soil, and movement of C from decomposing plant residue into adjacent soil was insignificant. In the samples with greater abundance of water-filled small pores, 60% of the added plant residue was decomposed, cumulative CO₂ emission constituted 2,000 µm C g⁻¹ soil, and the movement of residue C into adjacent soil was substantial. In the absence of plant residue the influence of pore characteristics on CO₂ emission, that is on decomposition of the native soil organic C, was negligible. The microbial communities on the plant residue in the samples with large pores had more microbial groups known to be cellulose decomposers, that is, Bacteroidetes, Proteobacteria, Actinobacteria, and Firmicutes, while a number of oligotrophic Acidobacteria groups were more abundant on the plant residue from the samples with small pores. This study provides the first experimental evidence that characteristics of soil pores and their air/water flow status determine the phylogenetic composition of the local microbial community and directions and magnitudes of soil C decomposition processes.« less

Properties of soil pore space regulate pathways of plant residue decomposition and community structure of associated bacteria.

PubMed

Negassa, Wakene C; Guber, Andrey K; Kravchenko, Alexandra N; Marsh, Terence L; Hildebrandt, Britton; Rivers, Mark L

2015-01-01

Physical protection of soil carbon (C) is one of the important components of C storage. However, its exact mechanisms are still not sufficiently lucid. The goal of this study was to explore the influence of soil structure, that is, soil pore spatial arrangements, with and without presence of plant residue on (i) decomposition of added plant residue, (ii) CO2 emission from soil, and (iii) structure of soil bacterial communities. The study consisted of several soil incubation experiments with samples of contrasting pore characteristics with/without plant residue, accompanied by X-ray micro-tomographic analyses of soil pores and by microbial community analysis of amplified 16S-18S rRNA genes via pyrosequencing. We observed that in the samples with substantial presence of air-filled well-connected large (>30 µm) pores, 75-80% of the added plant residue was decomposed, cumulative CO2 emission constituted 1,200 µm C g(-1) soil, and movement of C from decomposing plant residue into adjacent soil was insignificant. In the samples with greater abundance of water-filled small pores, 60% of the added plant residue was decomposed, cumulative CO2 emission constituted 2,000 µm C g(-1) soil, and the movement of residue C into adjacent soil was substantial. In the absence of plant residue the influence of pore characteristics on CO2 emission, that is on decomposition of the native soil organic C, was negligible. The microbial communities on the plant residue in the samples with large pores had more microbial groups known to be cellulose decomposers, that is, Bacteroidetes, Proteobacteria, Actinobacteria, and Firmicutes, while a number of oligotrophic Acidobacteria groups were more abundant on the plant residue from the samples with small pores. This study provides the first experimental evidence that characteristics of soil pores and their air/water flow status determine the phylogenetic composition of the local microbial community and directions and magnitudes of soil C decomposition processes.

Properties of soil pore space regulate pathways of plant residue decomposition and community structure of associated bacteria

DOE Office of Scientific and Technical Information (OSTI.GOV)

Negassa, Wakene C.; Guber, Andrey K.; Kravchenko, Alexandra N.

Physical protection of soil carbon (C) is one of the important components of C storage. However, its exact mechanisms are still not sufficiently lucid. The goal of this study was to explore the influence of soil structure, that is, soil pore spatial arrangements, with and without presence of plant residue on (i) decomposition of added plant residue, (ii) CO₂ emission from soil, and (iii) structure of soil bacterial communities. The study consisted of several soil incubation experiments with samples of contrasting pore characteristics with/without plant residue, accompanied by X-ray micro-tomographic analyses of soil pores and by microbial community analysis ofmore » amplified 16S–18S rRNA genes via pyrosequencing. We observed that in the samples with substantial presence of air-filled well-connected large (>30 µm) pores, 75–80% of the added plant residue was decomposed, cumulative CO₂ emission constituted 1,200 µm C g⁻¹ soil, and movement of C from decomposing plant residue into adjacent soil was insignificant. In the samples with greater abundance of water-filled small pores, 60% of the added plant residue was decomposed, cumulative CO₂ emission constituted 2,000 µm C g⁻¹ soil, and the movement of residue C into adjacent soil was substantial. In the absence of plant residue the influence of pore characteristics on CO₂ emission, that is on decomposition of the native soil organic C, was negligible. The microbial communities on the plant residue in the samples with large pores had more microbial groups known to be cellulose decomposers, that is, Bacteroidetes, Proteobacteria, Actinobacteria, and Firmicutes, while a number of oligotrophic Acidobacteria groups were more abundant on the plant residue from the samples with small pores. This study provides the first experimental evidence that characteristics of soil pores and their air/water flow status determine the phylogenetic composition of the local microbial community and directions and magnitudes of soil C decomposition processes.« less

Quantitative expression of protein heterogeneity: Response of amino acid side chains to their local environment.

PubMed

Bandyopadhyay, Debashree; Mehler, Ernest L

2008-08-01

A general method has been developed to characterize the hydrophobicity or hydrophilicity of the microenvironment (MENV), in which a given amino acid side chain is immersed, by calculating a quantitative property descriptor (QPD) based on the relative (to water) hydrophobicity of the MENV. Values of the QPD were calculated for a test set of 733 proteins to analyze the modulating effects on amino acid residue properties by the MENV in which they are imbedded. The QPD values and solvent accessibility were used to derive a partitioning of residues based on the MENV hydrophobicities. From this partitioning, a new hydrophobicity scale was developed, entirely in the context of protein structure, where amino acid residues are immersed in one or more "MENVpockets." Thus, the partitioning is based on the residues "sampling" a large number of "solvents" (MENVs) that represent a very large range of hydrophobicity values. It was found that the hydrophobicity of around 80% of amino acid side chains and their MENV are complementary to each other, but for about 20%, the MENV and their imbedded residue can be considered as mismatched. Many of these mismatches could be rationalized in terms of the structural stability of the protein and/or the involvement of the imbedded residue in function. The analysis also indicated a remarkable conservation of local environments around highly conserved active site residues that have similar functions across protein families, but where members have relatively low sequence homology. Thus, quantitative evaluation of this QPD is suggested, here, as a tool for structure-function prediction, analysis, and parameter development for the calculation of properties in proteins. (c) 2008 Wiley-Liss, Inc.

Micaceous Soil Strength And Permeability Improvement Induced By Microbacteria From Vegetable Waste

NASA Astrophysics Data System (ADS)

Omar, R. C.; Roslan, R.; Baharuddin, I. N. Z.; Hanafiah, M. I. M.

2016-11-01

Green technology method using vegetable waste are introduced in this paper for improvement of phyllite residual soil from UNITEN, Campus. Residual soil from phyllite are known as micaceous soils and it give problem in managing the stability of the slope especially in wet and extensively dry seasons. Micaceous soil are collected using tube sampler technique and mixed with liquid contain microorganism from fermented vegetable waste name as vege-grout to form remolded sample. The remolded sample are classify as 15.0%, 17.5%, 20.00% and 22.5% based on different incremental percentages of vege-grout. The curing time for the sample are 7, 14, 21, 28, and 35 days before the tests were conducted. Observation of the effect of treatment shows 20.0% of liquid contain Bacillus pasteurii and Bacillus Subtilis with 21 days curing time is the optimum value in strengthening the soil and improve the permeability.

Identification of residues of sulfosulfuron and its metabolites in subsoil-dissipation kinetics and factors influencing the stability and degradation of residues from topsoil to subsoil under predominant cropping conditions.

PubMed

Atmakuru, Ramesh; Perumal Elumalai, Thirugnanam; Sivanandam, Sathiyanarayanan

2007-07-01

Long term stability of sulfosulfuron was investigated in subsoil under the natural wheat cropping conditions. Experiments were conducted by applying a commercial formulation of sulfosulfuron on soil at 50 g/ha and 100 g/ha. To understand the factors influencing the persistence of residues two different experiments were conducted. In one experiment wheat crop was cultivated once at the beginning of the two years study period and subsequently the plots were kept undisturbed for the remaining period. In another experiment cultivation of subsequent crops were continued during the study period. In both the cases sulfosulfuron was applied only once at the beginning of the study. Representative soil samples were collected from the depths viz., 0-5, 15, 30, 45, 60 and 90 cm on different pre determined sampling occasions 50, 100, 200, 300, 400, 500 and 600 days after the application of the herbicide. The collected soil samples were analyzed for the residues of sulfosulfuron. Under the influence of continuous cropping conditions residues of sulfosulfuron were found to be relatively low when compared with the soil samples collected from the agriculture plots maintained without any cultivation. The residues detected are in the range 0.001 to 0.017 microg/g. Samples collected from the depth, at 30 to 45 cm showed higher residual concentrations. Soil samples were also showed the presence of break down products. The data has been confirmed by LC-MS/MS. The relation between residue content of sulfosulfuron and the factors contributing the stability of herbicide concentration were also studied.

Hazardous properties of paint residues from the furniture industry.

PubMed

Vaajasaari, Kati; Kulovaara, Maaret; Joutti, Anneli; Schultz, Eija; Soljamo, Kari

2004-01-30

The objective of this study was to screen nine excess paint residues for environmental hazard and to evaluate their disposability in a non-hazardous or hazardous-waste landfill. These residues were produced in the process of spray-painting furniture. Residues were classified according to their leaching and ecotoxicological properties. Leaching properties were determined with the European standard SFS-EN 12457-2 leaching-test. The toxicity of the leaching-test eluates was measured with plant-, bacteria- and enzyme-inhibition bioassays. Total organic carbon, formaldehyde and solvent concentrations in the solid wastes and in the leaching-test eluates were analysed. It seemed likely that leached formaldehyde caused very high acute toxicity in leaching-test eluates of the dry-booth residues. This hypothesis was based on the fact that the formaldehyde concentrations in the leaching-test eluates of the dry-booth residues were 62-75 times higher than the EC50 value reported in the literature for formaldehyde. The results of the water-curtain booth residues showed that the samples with the highest TOC and aromatic solvent concentrations were also the most toxic. The studied excess paint residues were complex organic mixtures and contained large amounts of compounds not identifiable from chemical data. Therefore, the evaluation of the hazard based solely on available chemical data is unlikely to be sufficient, as evidenced by our study. Our results show that harmful compounds remain in the solid waste and the toxicity results of their leaching-test eluates show that toxicity may leach from residues in contact with water at landfill sites. They also confirm the benefit of combining chemical and ecotoxicological assays in assessing the potential environmental hazard of complex organic mixtures found in wastes. Copyright 2003 Elsevier B.V.

Use of airborne hyperspectral data to estimate residual heavy metal contamination and acidification potential in the Guadiamar floodplain Andalusia, Spain after the Aznacollar mining accident

NASA Astrophysics Data System (ADS)

Kemper, Thomas; Sommer, Stefan

2004-10-01

Field and airborne hyperspectral data was used to map residual contamination after a mining accident, by applying spectral mixture modelling. Test case was the Aznalcollar Mine (Southern Spain) accident, where heavy metal bearing sludge from a tailings pond was distributed over large areas of the Guadiamar flood plain. Although the sludge and the contaminated topsoils have been removed mechanically in the whole affected area, still high abundance of pyritic material remained on the ground. During dedicated field campaigns in two subsequent years soil samples were collected for geochemical and spectral laboratory analysis and spectral field measurements were carried out in parallel to data acquisition with the HyMap sensor. A Variable Multiple Endmember Spectral Mixture Analysis (VMESMA) tool was used providing possibilities of multiple endmember unmixing, aiming to estimate the quantities and distribution of the remaining tailings material. A spectrally based zonal partition of the area was introduced to allow the application of different submodels to the selected areas. Based on an iterative feedback process, the unmixing performance could be improved in each stage until an optimum level was reached. The sludge abundances obtained by unmixing the hyperspectral spectral data were confirmed by the field observations and chemical measurements of samples taken in the area. The semi-quantitative sludge abundances of residual pyritic material could be transformed into quantitative information for an assessment of acidification risk and distribution of residual heavy metal contamination based on an artificial mixture experiment. The unmixing of the second year images allowed identification of secondary minerals of pyrite as indicators of pyrite oxidation and associated acidification.

Measures of precision for dissimilarity-based multivariate analysis of ecological communities

PubMed Central

Anderson, Marti J; Santana-Garcon, Julia

2015-01-01

Ecological studies require key decisions regarding the appropriate size and number of sampling units. No methods currently exist to measure precision for multivariate assemblage data when dissimilarity-based analyses are intended to follow. Here, we propose a pseudo multivariate dissimilarity-based standard error (MultSE) as a useful quantity for assessing sample-size adequacy in studies of ecological communities. Based on sums of squared dissimilarities, MultSE measures variability in the position of the centroid in the space of a chosen dissimilarity measure under repeated sampling for a given sample size. We describe a novel double resampling method to quantify uncertainty in MultSE values with increasing sample size. For more complex designs, values of MultSE can be calculated from the pseudo residual mean square of a permanova model, with the double resampling done within appropriate cells in the design. R code functions for implementing these techniques, along with ecological examples, are provided. PMID:25438826

Screening blood samples to estimate when oxytetverycline residues exceed regulatory tolerances in poultry muscle

USDA-ARS?s Scientific Manuscript database

The presence of antibiotic residues in edible animal products is a human food safety concern. To address this potential problem, the government samples edible tissues, such as muscle, to monitor for residues. Due to loss of valuable product and analytical difficulties only a small percentage of po...

Chemometric comparison of polychlorinated biphenyl residues and toxicologically active polychlorinated biphenyl congeners in the eggs of Forster's Terns (Sterna fosteri)

USGS Publications Warehouse

Schwartz, Ted R.; Stalling, David L.

1991-01-01

The separation and characterization of complex mixtures of polychlorinated biphenyls (PCBs) is approached from the perspective of a problem in chemometrics. A technique for quantitative determination of PCB congeners is described as well as an enrichment technique designed to isolate only those congener residues which induce mixed aryl hydrocarbon hydroxylase enzyme activity. A congener-specific procedure is utilized for the determination of PCBs in whichn-alkyl trichloroacetates are used as retention index marker compounds. Retention indices are reproducible in the range of ±0.05 to ±0.7 depending on the specific congener. A laboratory data base system developed to aid in the editing and quantitation of data generated from capillary gas chromatography was employed to quantitate chromatographic data. Data base management was provided by computer programs written in VAX-DSM (Digital Standard MUMPS) for the VAX-DEC (Digital Equipment Corp.) family of computers.In the chemometric evaluation of these complex chromatographic profiles, data are viewed from a single analysis as a point in multi-dimensional space. Principal Components Analysis was used to obtain a representation of the data in a lower dimensional space. Two-and three-dimensional proections based on sample scores from the principal components models were used to visualize the behavior of Aroclor® mixtures. These models can be used to determine if new sample profiles may be represented by Aroclor profiles. Concentrations of individual congeners of a given chlorine substitution may be summed to form homologue concentration. However, the use of homologue concentrations in classification studies with environmental samples can lead to erroneous conclusions about sample similarity. Chemometric applications are discussed for evaluation of Aroclor mixture analysis and compositional description of environmental residues of PCBs in eggs of Forster's terns (Sterna fosteri) collected from colonies near Lake Poygan and Green Bay, Wisconsin. The application of chemometrics is extended to the comparison of: a) Aroclors and PCB-containing environmental samples; to b) fractions of Aroclors and of environmental samples that have been enriched in congeners which induce mixed aryl hydrocarbon hydroxylase enzyme activity.

Determination of chloramphenicol residues in meat, seafood, egg, honey, milk, plasma and urine with liquid chromatography-tandem mass spectrometry, and the validation of the method based on 2002/657/EC.

PubMed

Rønning, Helene Thorsen; Einarsen, Kristin; Asp, Tone Normann

2006-06-23

A simple and rapid method for the determination and confirmation of chloramphenicol in several food matrices with LC-MS/MS was developed. Following addition of d5-chloramphenicol as internal standard, meat, seafood, egg, honey and milk samples were extracted with acetonitrile. Chloroform was then added to remove water. After evaporation, the residues were reconstituted in methanol/water (3+4) before injection. The urine and plasma samples were after addition of internal standard applied to a Chem Elut extraction cartridge, eluted with ethyl acetate, and hexane washed. Also these samples were reconstituted in methanol/water (3+4) after evaporation. By using an MRM acquisition method in negative ionization mode, the transitions 321-->152, 321-->194 and 326-->157 were used for quantification, confirmation and internal standard, respectively. Quantification of chloramphenicol positive samples regardless of matrix could be achieved with a common water based calibration curve. The validation of the method was based on EU-decision 2002/657 and different ways of calculating CCalpha and CCbeta were evaluated. The common CCalpha and CCbeta for all matrices were 0.02 and 0.04 microg/kg for the 321-->152 ion transition, and 0.02 and 0.03 microg/kg for the 321-->194 ion transition. At fortification level 0.1 microg/kg the within-laboratory reproducibility is below 25%.

Minimization of Residual Stress in an Al-Cu Alloy Forged Plate by Different Heat Treatments

NASA Astrophysics Data System (ADS)

Dong, Ya-Bo; Shao, Wen-Zhu; Jiang, Jian-Tang; Zhang, Bao-You; Zhen, Liang

2015-06-01

In order to improve the balance of mechanical properties and residual stress, various quenching and aging treatments were applied to Al-Cu alloy forged plate. Residual stresses determined by the x-ray diffraction method and slitting method were compared. The surface residual stress measured by x-ray diffraction method was consistent with that measured by slitting method. The residual stress distribution of samples quenched in water with different temperatures (20, 60, 80, and 100 °C) was measured, and the results showed that the boiling water quenching results in a 91.4% reduction in residual stress magnitudes compared with cold water quenching (20 °C), but the tensile properties of samples quenched in boiling water were unacceptably low. Quenching in 80 °C water results in 75% reduction of residual stress, and the reduction of yield strength is 12.7%. The residual stress and yield strength level are considerable for the dimensional stability of aluminum alloy. Quenching samples into 30% polyalkylene glycol quenchants produced 52.2% reduction in the maximum compressive residual stress, and the reduction in yield strength is 19.7%. Moreover, the effects of uphill quenching and thermal-cold cycling on the residual stress were also investigated. Uphill quenching and thermal-cold cycling produced approximately 25-40% reduction in residual stress, while the effect on tensile properties is quite slight.

Residue profiles of brodifacoum in coastal marine species following an island rodent eradication.

PubMed

Masuda, Bryce M; Fisher, Penny; Beaven, Brent

2015-03-01

The second-generation anticoagulant rodenticide brodifacoum is an effective tool for the eradication of invasive rodents from islands and fenced sanctuaries, for biodiversity restoration. However, broadcast application of brodifacoum bait on islands may expose non-target wildlife in coastal marine environments to brodifacoum, with subsequent secondary exposure risk for humans if such marine wildlife is harvested for consumption. We report a case study of monitoring selected marine species following aerial application of brodifacoum bait in August 2011 to eradicate Norway rats (Rattus norvegicus) from Ulva Island, New Zealand. Residual concentrations of brodifacoum were detected in 3 of 10 species of coastal fish or shellfish sampled 43-176d after bait application commenced. Residual brodifacoum concentrations were found in liver, but not muscle tissue, of 2 of 24 samples of blue cod (0.026 and 0.092 µg/g; Parapercis colias) captured live then euthanized for tissue sampling. Residual brodifacoum concentrations were also found in whole-body samples of 4 of 24 mussels (range=0.001-0.022 µg/g, n=4; Mytilus edulis) and 4 of 24 limpets (range=0.001-0.016 µg/g, n=4; Cellana ornata). Measured residue concentrations in all three species were assessed as unlikely to have eventually caused mortality of the sampled individuals. We also conducted a literature review and determined that in eleven previous accounts of residue examination of coastal marine species following aerial applications of brodifacoum bait, including our results from Ulva Island, the overall rate of residue detection was 5.6% for marine invertebrates (11 of 196 samples tested) and 3.1% for fish (2 of 65 samples tested). Furthermore, our results from Ulva Island are the first known detection of brodifacoum residue in fish liver following an aerial application of brodifacoum bait. Although our findings confirm the potential for coastal marine wildlife to be exposed to brodifacoum following island rodent eradications using aerial bait application, the risk of mortality to exposed individual fish or shellfish appears very low. There is also a very low risk of adverse effects on humans that consume fish or shellfish containing residual concentrations in the ranges reported here. Furthermore, any brodifacoum residues that occur in marine wildlife decline to below detectable concentrations over a period of weeks. Thus potential human exposure to brodifacoum through consumption of marine wildlife containing residual brodifacoum could be minimized by defining 'no take' periods for harvest following bait application and regular monitoring to confirm the absence of detectable residues in relevant marine wildlife. Copyright © 2014 Elsevier Inc. All rights reserved.

Sample and data processing considerations for the NIST quantitative infrared database

NASA Astrophysics Data System (ADS)

Chu, Pamela M.; Guenther, Franklin R.; Rhoderick, George C.; Lafferty, Walter J.; Phillips, William

1999-02-01

Fourier-transform infrared (FT-IR) spectrometry has become a useful real-time in situ analytical technique for quantitative gas phase measurements. In fact, the U.S. Environmental Protection Agency (EPA) has recently approved open-path FT-IR monitoring for the determination of hazardous air pollutants (HAP) identified in EPA's Clean Air Act of 1990. To support infrared based sensing technologies, the National Institute of Standards and Technology (NIST) is currently developing a standard quantitative spectral database of the HAPs based on gravimetrically prepared standard samples. The procedures developed to ensure the quantitative accuracy of the reference data are discussed, including sample preparation, residual sample contaminants, data processing considerations, and estimates of error.

Cytotoxic drug residues in urine of dogs receiving anticancer chemotherapy.

PubMed

Knobloch, A; Mohring, S A I; Eberle, N; Nolte, I; Hamscher, G; Simon, D

2010-01-01

The presence of cytotoxic drug residues in urine of dogs may represent an exposure risk for pet owners and other people as well as a potential environmental contaminant. However, studies on cytotoxic drug residues in excretions of clinical patients are lacking in veterinary oncology. Variable concentrations of cytotoxic residues are present in urine samples, depending on sampling time and substance. Client-owned dogs with lymphoma or mast cell tumors treated with standard chemotherapy protocols. Urine samples were collected before, directly after, and on days after administration of chemotherapy. Measurement of vincristine, vinblastine, cyclophosphamide, and doxorubicin residues in canine urine was performed by a quantitative liquid chromatography tandem mass spectrometry (LC/MS/MS) method. Median cyclophosphamide residue concentration was 398.2 microg/L directly after treatment (d0) and was below the level of detection on days 1-3 (d1, d2, d3). Median vincristine residue concentration was 53.8 microg/L directly after treatment and was 20.2, 11.4, and 6.6 microg/L on days 1, 2, and 3. Median vinblastine residues were 144.9 (d0), 70.8 (d1), 35.6 (d2), and 18.7 microg/L (d3) with low concentrations detectable for 7 days after treatment. Median urine doxorubicin concentrations were 354.0 (d0), 165.6 (d1), 156.9 (d2), and 158.2 microg/L (d3). Low concentrations of doxorubicin were measurable up to 21 days after administration. Variable concentrations of chemotherapeutics were measured in urine samples, depending on sampling time point and drug. Findings may inform current chemoprotection guidelines and help minimize exposure risks.

A quantitative method for residues of macrolide antibiotics in porcine kidney by liquid chromatography/tandem mass spectrometry.

PubMed

Dickson, Leslie C; O'Byrne, Collin; Chan, Wayne

2012-01-01

An LC/MS/MS-based multiresidue quantitative method was developed for the macrolides erythromycin A, neospiramycin I, oleandomycin, spiramycin I, tilmicosin, and tylosin A in porcine kidney tissues. The Canadian Food Inspection Agency (CFIA) had as part of its analytical scope an LC/UV method for quantification of residues of two macrolide antibiotics, tilmicosin and tylosin A, in the kidney, liver, and muscle of cattle, swine, and poultry. The method could not reliably detect concentrations below 10 microg/kg. To increase the scope of the CFIA's analytical capabilities, a sensitive multiresidue quantitative method for macrolide residues in food animal tissues was required. Porcine kidney samples were extracted with acetonitrile and alkaline buffer and cleaned-up using silica-based C18 SPE cartridges. Sample extracts were analyzed using LC/MS/MS with positive electrospray ionization. Fitness for purpose was verified in a single-laboratory validation study using a second analyst. The working analytical range was 5 to 50 microg/kg. LOD and LOQ were 0.5 to 0.6 microg/kg and 1.5 to 3.0 microg/kg, respectively. Limits of identification were 0.5 to 2.0 microg/kg. Relative intermediate precisions were 8 to 17%. Average absolute recoveries were 68 to 76%.

Detection of kanamycin and gentamicin residues in animal-derived food using IgY antibody based ic-ELISA and FPIA.

PubMed

Li, Cui; Zhang, Yaoyao; Eremin, Sergei A; Yakup, Omar; Yao, Gang; Zhang, Xiaoying

2017-07-15

Our aim in this study is to show that IgY antibody based immunoassays could be used to detect antibiotic residues in animal-derived food. Briefly, full antigens of gentamicin (Gent) and kanamycin (Kana) were used to immunize the laying chickens to prepare IgY antibodies. Then, these antibodies were evaluated by FPIA and ic-ELISA to detect Gent/Kana in animal-derived samples. The IC 50 of FPIA and ic-ELISA based anti-Gent IgY were 7.70±0.6μg/mL and 0.32±0.06μg/mL, respectively. The IC 50 of FPIA and ic-ELISA based anti-Kana IgY were 7.97±0.9μg/mL and 0.15±0.01μg/mL. The limits of detection (LOD, IC 10 ) for FPIA based anti-Gent/Kana IgY were 0.17 and 0.007μg/mL, respectively. The LOD for ic-ELISA were both 0.001μg/mL. These results indicated that the ic-ELISA might more suitable for antibiotic residues detection than FPIA. Copyright © 2017 Elsevier Ltd. All rights reserved.

Distribution and weathering of crude oil residues on shorelines 18 years after the Exxon Valdez spill.

PubMed

Boehm, Paul D; Page, David S; Brown, John S; Neff, Jerry M; Bragg, James R; Atlas, Ronald M

2008-12-15

In 2007, a systematic study was conducted to evaluate the form and location of residues of oil buried on Prince William Sound (PWS) shorelines, 18 years after the 1989 Exxon Valdez Oil Spill (EVOS). We took 678 sediment samples from 22 sites that were most heavily oiled in 1989 and known to contain the heaviest subsurface oil (SSO) deposits based on multiple studies conducted since 2001. An additional 66 samples were taken from two sites, both heavily oiled in 1989 and known to be active otter foraging sites. All samples were analyzed for total extractable hydrocarbons (TEH), and 25% were also analyzed for saturated and aromatic hydrocarbon weathering parameters. Over 90% of the samples from all sites contained light or no SSO at all. Of samples containing SSO, 81% showed total polycyclic aromatic hydrocarbon (TPAH) losses greater than 70%, relative to cargo oil, with most having >80% loss. Samples with SSO were observed in isolated patches sequestered by surface boulder and cobble armoring. Samples showing lowest TPAH loss correlated strongly with higher elevations in the intertidal zones. Of the 17 atypical, less-weathered samples having less than 70% loss of TPAH (>30% remaining), only two were found sequestered in the lower intertidal zone, both at a single site. Most of the EVOS oil in PWS has been eliminated due to natural weathering. Some isolated SSO residues remain because they are sequestered and only slowly affected by natural weathering processes that normally would bring about their rapid removal. Even where SSO patches remain, most are highly weathered, sporadically distributed at a small number of sites, and widely separated from biologically productive lower intertidal zones where most foraging by wildlife occurs.

Thin layer chromatography residue applicator sampler

DOEpatents

Nunes, Peter J [Danville, CA; Kelly, Fredrick R [Modesto, CA; Haas, Jeffrey S [San Ramon, CA; Andresen, Brian D [Livermore, CA

2007-07-24

A thin layer chromatograph residue applicator sampler. The residue applicator sampler provides for rapid analysis of samples containing high explosives, chemical warfare, and other analyses of interest under field conditions. This satisfied the need for a field-deployable, small, hand-held, all-in-one device for efficient sampling, sample dissolution, and sample application to an analytical technique. The residue applicator sampler includes a sampling sponge that is resistant to most chemicals and is fastened via a plastic handle in a hermetically sealed tube containing a known amount of solvent. Upon use, the wetted sponge is removed from the sealed tube and used as a swiping device across an environmental sample. The sponge is then replaced in the hermetically sealed tube where the sample remains contained and dissolved in the solvent. A small pipette tip is removably contained in the hermetically sealed tube. The sponge is removed and placed into the pipette tip where a squeezing-out of the dissolved sample from the sponge into the pipette tip results in a droplet captured in a vial for later instrumental analysis, or applied directly to a thin layer chromatography plate for immediate analysis.

Influences of metal ions crosslinked alginate based coatings on thermal stability and fire resistance of cotton fabrics.

PubMed

Pan, Ying; Wang, Wei; Liu, Longxiang; Ge, Hua; Song, Lei; Hu, Yuan

2017-08-15

Bio-based and phosphorus-free coating was fabricated by layer-by-layer assembly method to obtain the flame retardant cotton fabric. For the first time, the modified cotton fabrics were prepared by utilizing positively charged polyethylenimine and negatively charged alginate together with subsequent crosslinking of barium, nickel and cobalt ions. Scanning electron microscopy and energy-dispersive X-ray demonstrated that the metal ions crosslinked coating was successfully constructed on the substrate. The thermal stability and flame retardancy were investigated by thermogravimetric analysis (TGA) and horizontal flame tests. TGA results showed that the degradation of the coated cotton fabrics were retarded at high temperature and the char residue of the cotton fabrics were improved after covered with the barium, nickel and cobalt ions crosslinked coatings. Furthermore, the fire resistance of cotton-Ba sample was enhanced significantly compared with the untreated sample, as evidenced by the obvious reduction (28%) of flame spread rate and complete char residue. Finally, the washing durability of coating on the fabric was enhanced after metal ions crosslinked with alginate based coating. Copyright © 2017. Published by Elsevier Ltd.

Detection of quinolones in commercial eggs obtained from farms in the Espaíllat Province in the Dominican Republic.

PubMed

Moscoso, S; de los Santos, F Solís; Andino, A G; Diaz-Sanchez, Sandra; Hanning, I

2015-01-01

Previously, we reported the use of quinolones in broiler chickens resulted in residues in retail poultry meat obtained from nine districts in the Santiago Province of the Dominican Republic. Residues in poultry products are a concern due to consumer allergies and the potential to develop antibiotic-resistant bacteria. Given the use of quinolones in poultry production and our previous findings in poultry meat, the objective of this study was to evaluate the presence of quinolone residues in eggs. Samples were collected from 48 different farms located in three of the four municipalities (Moca, Cayetano Germosén, and Jamao) of the Espaíllat Province. Each farm was sampled three times between July and September for a total of 144 samples. Samples were evaluated qualitatively and quantitatively for quinolone residues using the Equinox test. Operation systems (cage or floor), seasonality, and location were considered along with egg-producer sizes that were defined as small scale, <30,000 eggs per day; medium scale, 30,000 to 60,000 eggs per day; or large scale, >60,000 eggs per day. From small-, medium-, and large-scale producers, 69, 50, and 40% of samples were positive for quinolone residues, respectively. A greater number of samples were positive (61%) in floor-laying hen producers compared with those using cages (40%). In the Jamao municipality, 67% of the samples were positive compared with Moca and Cayetano Germosén, where 56 and 25% of samples were positive, respectively. Sampling time had an effect on percent positives: samples collected in July, August, and September were 71, 19, and 63% positive, respectively. Overall, 51% of the samples obtained from eggs produced in the province of Espaíllat were positive for quinolone residues at levels higher than the maximum limits for edible tissue established by the regulatory agencies, including the European Union and U.S. Department of Agriculture. The results obtained from this research confirmed the presence of quinolone residue in eggs, which may present a health risk to some consumers.

Determination of organophosphorus pesticide residues in vegetables by an enzyme inhibition method using α-naphthyl acetate esterase extracted from wheat flour*

PubMed Central

Wang, Jun-liang; Xia, Qing; Zhang, An-ping; Hu, Xiao-yan; Lin, Chun-mian

2012-01-01

The widespread use of organophosphorus pesticides (OPs) poses a great threat to human health and has made the detection of OP residues in food an important task, especially in view of the fact that easy and rapid detection methods are needed. Because OPs have inhibitory effects on the activity of α-naphthyl acetate esterase (ANAE) in plants, in this work we evaluated the possibility of detecting OPs in vegetables with ANAE extracted from commercial flour. The limits of detection (LODs) obtained for methamidophos, dichlorvos, phoxim, dimethoate, and malathion in lettuce samples with crude ANAE were 0.17, 0.11, 0.11, 0.96, and 1.70 mg/kg, respectively. Based on the maximum residue limits (MRLs) for OPs in food stipulated by Chinese laws which are 0.05, 0.20, 0.05, 1.00, and 8.00 mg/kg for methamidophos, dichlorvos, phoxim, dimethoate, and malathion, respectively, the esterase inhibition method with crude ANAE had sufficient sensitivity to detect the residues of dichlorvos, dimethoate, and malathion in lettuce, but it could not be used to guarantee the safety of the same samples if methamidophos or phoxim residue was present. The sensitivity of the method was improved by the use of esterase purified by ammonium sulfate salting-out. The LODs obtained for methamidophos and phoxim with purified esterase were lower than the MRLs for these OPs in food. This is a very promising method for the detection of OP residues in vegetables using crude or purified esterase because of its cheapness, sensitivity, and convenience. PMID:22467368

Fatty Acid Structure and Degradation Analysis in Fingerprint Residues

NASA Astrophysics Data System (ADS)

Pleik, Stefanie; Spengler, Bernhard; Schäfer, Thomas; Urbach, Dieter; Luhn, Steven; Kirsch, Dieter

2016-09-01

GC-MS investigations were carried out to elucidate the aging behavior of unsaturated fatty acids in fingerprint residues and to identify their degradation products in aged samples. For this purpose, a new sample preparation technique for fingerprint residues was developed that allows producing N-methyl- N-trimethylsilyl-trifluoroacetamide (MSTFA) derivatives of the analyzed unsaturated fatty acids and their degradation products. MSTFA derivatization catalyzed by iodotrimethylsilane enables the reliable identification of aldehydes and oxoacids as characteristic MSTFA derivatives in GCMS. The obtained results elucidate the degradation pathway of unsaturated fatty acids. Our study of aged fingerprint residues reveals that decanal is the main degradation product of the observed unsaturated fatty acids. Furthermore, oxoacids with different chain lengths are detected as specific degradation products of the unsaturated fatty acids. The detection of the degradation products and their chain length is a simple and effective method to determine the double bond position in unsaturated compounds. We can show that the hexadecenoic and octadecenoic acids found in fingerprint residues are not the pervasive fatty acids Δ9-hexadecenoic (palmitoleic acid) and Δ9-octadecenoic (oleic acid) acid but Δ6-hexadecenoic acid (sapienic acid) and Δ8-octadecenoic acid. The present study focuses on the structure identification of human sebum-specific unsaturated fatty acids in fingerprint residues based on the identification of their degradation products. These results are discussed for further investigations and method developments for age determination of fingerprints, which is still a tremendous challenge because of several factors affecting the aging behavior of individual compounds in fingerprints.

Fatty Acid Structure and Degradation Analysis in Fingerprint Residues.

PubMed

Pleik, Stefanie; Spengler, Bernhard; Schäfer, Thomas; Urbach, Dieter; Luhn, Steven; Kirsch, Dieter

2016-09-01

GC-MS investigations were carried out to elucidate the aging behavior of unsaturated fatty acids in fingerprint residues and to identify their degradation products in aged samples. For this purpose, a new sample preparation technique for fingerprint residues was developed that allows producing N-methyl-N-trimethylsilyl-trifluoroacetamide (MSTFA) derivatives of the analyzed unsaturated fatty acids and their degradation products. MSTFA derivatization catalyzed by iodotrimethylsilane enables the reliable identification of aldehydes and oxoacids as characteristic MSTFA derivatives in GCMS. The obtained results elucidate the degradation pathway of unsaturated fatty acids. Our study of aged fingerprint residues reveals that decanal is the main degradation product of the observed unsaturated fatty acids. Furthermore, oxoacids with different chain lengths are detected as specific degradation products of the unsaturated fatty acids. The detection of the degradation products and their chain length is a simple and effective method to determine the double bond position in unsaturated compounds. We can show that the hexadecenoic and octadecenoic acids found in fingerprint residues are not the pervasive fatty acids Δ9-hexadecenoic (palmitoleic acid) and Δ9-octadecenoic (oleic acid) acid but Δ6-hexadecenoic acid (sapienic acid) and Δ8-octadecenoic acid. The present study focuses on the structure identification of human sebum-specific unsaturated fatty acids in fingerprint residues based on the identification of their degradation products. These results are discussed for further investigations and method developments for age determination of fingerprints, which is still a tremendous challenge because of several factors affecting the aging behavior of individual compounds in fingerprints. Graphical Abstract ᅟ.

A prospective gating method to acquire a diverse set of free-breathing CT images for model-based 4DCT

NASA Astrophysics Data System (ADS)

O'Connell, D.; Ruan, D.; Thomas, D. H.; Dou, T. H.; Lewis, J. H.; Santhanam, A.; Lee, P.; Low, D. A.

2018-02-01

Breathing motion modeling requires observation of tissues at sufficiently distinct respiratory states for proper 4D characterization. This work proposes a method to improve sampling of the breathing cycle with limited imaging dose. We designed and tested a prospective free-breathing acquisition protocol with a simulation using datasets from five patients imaged with a model-based 4DCT technique. Each dataset contained 25 free-breathing fast helical CT scans with simultaneous breathing surrogate measurements. Tissue displacements were measured using deformable image registration. A correspondence model related tissue displacement to the surrogate. Model residual was computed by comparing predicted displacements to image registration results. To determine a stopping criteria for the prospective protocol, i.e. when the breathing cycle had been sufficiently sampled, subsets of N scans where 5  ⩽  N  ⩽  9 were used to fit reduced models for each patient. A previously published metric was employed to describe the phase coverage, or ‘spread’, of the respiratory trajectories of each subset. Minimum phase coverage necessary to achieve mean model residual within 0.5 mm of the full 25-scan model was determined and used as the stopping criteria. Using the patient breathing traces, a prospective acquisition protocol was simulated. In all patients, phase coverage greater than the threshold necessary for model accuracy within 0.5 mm of the 25 scan model was achieved in six or fewer scans. The prospectively selected respiratory trajectories ranked in the (97.5  ±  4.2)th percentile among subsets of the originally sampled scans on average. Simulation results suggest that the proposed prospective method provides an effective means to sample the breathing cycle with limited free-breathing scans. One application of the method is to reduce the imaging dose of a previously published model-based 4DCT protocol to 25% of its original value while achieving mean model residual within 0.5 mm.

Valid internal standard technique for arson detection based on gas chromatography-mass spectrometry.

PubMed

Salgueiro, Pedro A S; Borges, Carlos M F; Bettencourt da Silva, Ricardo J N

2012-09-28

The most popular procedures for the detection of residues of accelerants in fire debris are the ones published by the American Society for Testing and Materials (ASTM E1412-07 and E1618-10). The most critical stages of these tests are the conservation of fire debris from the sampling to the laboratory, the extraction of residues of accelerants from the debris to the activated charcoal strips (ACS) and from those to the final solvent, as well as the analysis of sample extract by gas chromatography-mass spectrometry (GC-MS) and the interpretation of the instrumental signal. This work proposes a strategy for checking the quality of the sample conservation, the accelerant residues transference to final solvent and GC-MS analysis, using internal standard additions. It is used internal standards ranging from a highly volatile compound for checking debris conservation to low volatile compound for checking GC-MS repeatability. The developed quality control (QC) parameters are not affected by GC-MS sensitivity variation and, specifically, the GC-MS performance control is not affected by ACS adsorption saturation that may mask test performance deviations. The proposed QC procedure proved to be adequate to check GC-MS repeatability, ACS extraction and sample conservation since: (1) standard additions are affected by negligible uncertainty and (2) observed dispersion of QC parameters are fit for its intended use. Copyright © 2012 Elsevier B.V. All rights reserved.

The comparison of solid phase microextraction-GC and static headspace-GC for determination of solvent residues in vegetable oils.

PubMed

Ligor, Magdalena; Buszewski, Bogusław

2008-02-01

The objective of these investigations has been the determination of volatile organic compounds including residue solvents present in vegetable oil samples. Some olive oil, rape oil, sunflower oil, soy-bean oil, pumpkin oil, grape oil, rice oil as well as hazel-nut oil samples were analysed. Among residue solvents the following compounds have been mentioned: acetone, n-hexane, benzene, and toluene. Some experiments for the solid phase microextraction (SPME)-GC-flame ionisation detection (FID) were performed to examine extraction conditions such as fiber exposure time, temperature of extraction, and temperature of desorption. Various SPME fibers such as polydimethylsiloxane, Carboxen/polydimethylsiloxane and polydimethylsiloxane/divinylbenzene coatings were used for the isolation of tested compounds from vegetable oil samples. After optimisation of SPME, real vegetable oil samples were examined using SPME-GC/MS. Based on preliminary experiments the qualitative and quantitative analyses for the determination of acetone, n-hexane, benzene and toluene were performed by SPME-GC-FID and static head-space (SHS)-GC-FID methods. The regression coefficients for calibration curves for the examined compounds were R(2) > or = 0.992. This shows that the used method is linear in the examined concentration range (0.005-0.119 mg/kg for SPME-GC-FID and 0.003-0.728 mg/kg for SHS-GC-FID). Chemical properties of analysed vegetable oils have been characterised by chemometric procedure (cluster analysis).

Occurrence of glyphosate and AMPA residues in soy-based infant formula sold in Brazil.

PubMed

Rodrigues, Nadia Regina; de Souza, Ana Paula Ferreira

2018-04-01

Glyphosate is an herbicide widely used in the world, being applied in several crops, among them soybeans. Recently, glyphosate and its metabolite aminomethylphosphonic acid (AMPA) have been identified as possible contributors to the emergence of various diseases such as autism, Parkinson's and Alzheimer's diseases, as well as cancer. The child population-consuming cereal-based foods is the most exposed to the effects of pesticides because of their developmental phase and they have a higher food intake per kilogram of body weight than adults. The presence of glyphosate and AMPA residues in soy-based infant formulas was evaluated during the years 2012-2017, totalising 105 analyses carried out on 10 commercial brands from different batches. Glyphosate and AMPA were determined by liquid chromatography with fluorescence detection after derivatisation reaction. The method was validated and showed accuracy and precision with a limit of quantification (LOQ) of 0.02 mg kg -1 . Among those samples that contained levels above the LOQ, the variation of glyphosate residues was from 0.03 mg kg -1 to 1.08 mg kg -1 and for AMPA residues was from 0.02 mg kg -1 to 0.17 mg kg -1 . This is the first scientific communication about glyphosate and AMPA contamination in soy-based infant formula in Brazil, The study was conducted under good laboratory practice (GLP) and supported by good scientific practice.

Optimization of sol-gel medium for entrapment of acetylcholinesterase enzyme in biosensor for pesticide detection

NASA Astrophysics Data System (ADS)

Wijayanti, S. D.; Rahayu, F. S.; Widyaningsih, T. D.

2018-03-01

Pesticides are chemical substances used to kill and control pests or diseases that can damage crops. The use of pesticides should be done precisely because the accumulation of chemicals contained in pesticides can cause various health effects. Therefore, detection of pesticide residues on plants is important to reduce the risk of poisoning due to pesticide residues. Some of the conventional methods that have been done to detect pesticide residues have weaknesses among expensive tools, takes a long time, and are generally performed by trained laboratory technicians. Biosensors are analytical devices that can measure the quantitative or semi-quantitative targets of analyte by utilizing a bioreceptor such as enzyme. Several studies have shown that enzyme-based acetylcholinesterase-based biosensors can be used to detect pesticide residues in vegetable samples. The objective of this research was to get a proper silica based sol-gel formulation with molar ratio of H2O:TEOS and NaOH concentration as immobilization medium of acetylcholinesterase enzyme for biosensor application. Response Surface Methodology (RSM) was used in order to determine the interaction between the parameters studied and resulting responses which were amount and activity of acetylcholinesterase enzyme. Based on the research, the best result for immobilized enzyme activity was shown by molar ratio (H2O: TEOS) 1: 8 and 4 mM NaOH treatment.

The influence of baking fuel on residues of polycyclic aromatic hydrocarbons and heavy metals in bread.

PubMed

Ahmed, M T; Abdel Hadi el-S; el-Samahy, S; Youssof, K

2000-12-30

The influence of fuel type used to bake bread on the spectrum and concentrations of some polycyclic aromatic hydrocarbons and heavy metals in baked bread was assessed. Bread samples were collected from different bakeries operated by either electricity, solar, mazot or solid waste and their residue content of PAHs and heavy metals was assessed. The total concentration of PAHs detected in mazot, solar, solid waste and electricity operated bakeries had an average of 320.6, 158.4, 317.3 and 25.5 microgkg(-1), respectively. Samples collected from mazot, solar and solid waste operated bakeries have had a wide spectrum of PAHs, in comparison to that detected in bread samples collected from electricity operated bakeries. Lead had the highest concentrations in the four groups of bread samples, followed by nickel, while the concentrations of zinc and cadmium were the least. The concentration of lead detected in bread samples produced from mazot, solar, solid waste and electricity fueled bakeries were 1375.5, 1114, 1234, and 257.3 microgkg(-1), respectively. Estimated daily intake of PAHs based on bread consumption were 48.2, 28.5, 80. 1, and 4.8 microg per person per day for bread produced in bakeries using mazot, solar, solid waste and electricity, respectively. Meanwhile, the estimated daily intake of benzo (a) pyrene were 3.69, 2.65, 8.1, and 0.81 microg per person per day for bread sample baked with mazot, solar, solid waste and electricity, respectively. The daily intake of lead, based on bread consumption was 291, 200.5, 222, and 46.31 microg per person per day for bread sample baked with mazot, solar, solid waste and electricity, respectively. The present work has indicated the comparatively high level of daily intake of benzo (a) pyrene and lead in comparison to levels reported from many other countries and those recommended by international regulatory bodies. It is probable that residues detected in bread samples are partially cereal-borne but there is strong evidence that the process of baking and the gases emitted are responsible for most of the contamination load.

Comparison of veterinary drug residue results in animal tissues by ultrahigh-performance liquid chromatography coupled to triple quadrupole or quadrupole-time-of-flight tandem mass spectrometry after different sample preparation methods, including use of a commercial lipid removal product.

PubMed

Anumol, Tarun; Lehotay, Steven J; Stevens, Joan; Zweigenbaum, Jerry

2017-04-01

Veterinary drug residues in animal-derived foods must be monitored to ensure food safety, verify proper veterinary practices, enforce legal limits in domestic and imported foods, and for other purposes. A common goal in drug residue analysis in foods is to achieve acceptable monitoring results for as many analytes as possible, with higher priority given to the drugs of most concern, in an efficient and robust manner. The U.S. Department of Agriculture has implemented a multiclass, multi-residue method based on sample preparation using dispersive solid phase extraction (d-SPE) for cleanup and ultrahigh-performance liquid chromatography-tandem quadrupole mass spectrometry (UHPLC-QQQ) for analysis of >120 drugs at regulatory levels of concern in animal tissues. Recently, a new cleanup product called "enhanced matrix removal for lipids" (EMR-L) was commercially introduced that used a unique chemical mechanism to remove lipids from extracts. Furthermore, high-resolution quadrupole-time-of-flight (Q/TOF) for (U)HPLC detection often yields higher selectivity than targeted QQQ analyzers while allowing retroactive processing of samples for other contaminants. In this study, the use of both d-SPE and EMR-L sample preparation and UHPLC-QQQ and UHPLC-Q/TOF analysis methods for shared spiked samples of bovine muscle, kidney, and liver was compared. The results showed that the EMR-L method provided cleaner extracts overall and improved results for several anthelmintics and tranquilizers compared to the d-SPE method, but the EMR-L method gave lower recoveries for certain β-lactam antibiotics. QQQ vs. Q/TOF detection showed similar mixed performance advantages depending on analytes and matrix interferences, with an advantage to Q/TOF for greater possible analytical scope and non-targeted data collection. Either combination of approaches may be used to meet monitoring purposes, with an edge in efficiency to d-SPE, but greater instrument robustness and less matrix effects when analyzing EMR-L extracts. Graphical abstract Comparison of cleanup methods in the analysis of veterinary drug residues in bovine tissues.

An evaluation of remote sensing technologies for the detection of residual contamination at ready-for-anticipated use sites

USGS Publications Warehouse

Slonecker, E. Terrence; Fisher, Gary B.

2014-01-01

Operational problems with site access and information, XRF instrument operation, and imagery collections hampered the effective data collection and analysis process. Of the 24 sites imaged and analyzed, 17 appeared to be relatively clean with no discernible metal contamination, hydrocarbons, or asbestos in the soil. None of the samples for the sites in Louisiana had any result exceeding the appropriate industrial or residential standard for arsenic or lead. One site in South Carolina (North Street Dump) had two samples that exceeded the residential standard for lead. One site in Texas (Cadiz Street), and four sites in Florida (210 North 12th Street, Encore Retail Site, Clearwater Auto, and 22nd Street Mixed Use) were found to have some level of residual metal contamination above the applicable residential or commercial Risk-Based Concentration (RBC) standard. Three of the Florida sites showing metal contamination also showed a pattern of vegetation stress based on standard vegetation analysis techniques.

Using ATR-FT/IR molecular spectroscopy to detect effects of blend DDGS inclusion level on the molecular structure spectral and metabolic characteristics of the proteins in hulless barley

NASA Astrophysics Data System (ADS)

Zhang, Xuewei; Yu, Peiqiang

2012-09-01

The objectives of this study were to investigate the effects of inclusion of a bioethanol co-product of blend DDGS (wheat:corn = 70%:30%) on protein molecular structure spectral and metabolic characteristics in hulless barley-based feed using ATR-FT/IR molecular spectroscopy. Hulless barley grain with the blend DDGS were mixed in the five ratios. The results showed that when blend DDGS was included at an increased ratio, predicted truly absorbed protein supply was highly and linearly increased (P < 0.05) from 98 to 245 g kg-1 DM and degraded protein balance was increased (P < 0.05) from -1 to 75 g kg-1 DM. The ratio of amide I to II peak area was increased (P < 0.05) in the original combination samples but decreased (P < 0.05) in the in situ 48 h residue samples. The ratio of α-helix to β-sheet peak height was quadratically changed with increasing inclusion rate of blend DDGS in the original samples, but no difference among the in situ 48 h residue samples, indicating completion of protein degradation. No correlation was found between protein 2nd structures and protein nutrient profiles not only for the original combination samples (except NPN) but also for in situ 48 h residue samples. This study may provide information on how protein molecular structure and metabolic characteristic changes after feed combination and how more effectively utilize hulless barley and blend co-products for dairy and beef cattle.

Are polychlorinated biphenyl residues adequately describe by aroclor mixture equivalents. Isomer-specific principal components analysis of such residues in fish and turtles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schwartz, T.R.; Stalling, D.L.; Rice, C.L.

1987-01-01

Polychlorinated biphenyl (PCB) residues from fish and turtles were analyzed with SIMCA (Soft Independent Modeling of Class Analogy), a principal components analysis technique. A series of technical Aroclors were also analyzed to provide a reference data set for pattern recognition. Environmental PCB residues are often expressed in terms of relative Aroclor composition. In this work, we assessed the similarity of Aroclors to class models derived for fish and turtles to ascertain if the PCB residues in the samples could be described by an Aroclor or Aroclor mixture. Using PCA, we found that these samples could not be described by anmore » Aroclor or Aroclor mixture and that it would be inappropriate to report these samples as such. 18 references, 3 figures, 3 tables.« less

Iodide Residues in Milk Vary between Iodine-Based Teat Disinfectants.

PubMed

French, Elizabeth A; Mukai, Motoko; Zurakowski, Michael; Rauch, Bradley; Gioia, Gloria; Hillebrandt, Joseph R; Henderson, Mark; Schukken, Ynte H; Hemling, Thomas C

2016-07-01

Majority of iodine found in dairy milk comes from the diet and teat disinfection products used during milking process. The objective of this study was to evaluate the effects of 4 iodine-based teat dips on milk iodide concentrations varying in iodine level (0.25% vs. 0.5%, w/w), normal low viscosity dip versus barrier dip, and application method (dip vs. spray) to ensure safe iodine levels in dairy milk when these products are used. The iodine exposure study was performed during a 2-wk period. The trial farm was purged of all iodine-based disinfection products for 21 d during a prestudy "washout period," which resulted in baseline milk iodide range of 145 to 182 ppb. During the experiment, iodine-based teat dips were used as post-milking teat disinfectants and compared to a non-iodine control disinfectant. Milk iodide residue levels for each treatment was evaluated from composited group samples. Introduction of different iodine-based teat disinfectants increased iodide residue content in milk relative to the control by between 8 and 29 μg/L when averaged across the full trial period. However, residues levels for any treatment remained well below the consumable limit of 500 μg/L. The 0.5% iodine disinfectant increased milk iodide levels by 20 μg/L more compared to the 0.25% iodine. Compared to dip-cup application, spray application significantly increased milk iodide residue by 21 μg/L and utilized approximately 23% more teat dip. This carefully controlled study demonstrated an increase in milk iodide concentrations from iodine disinfectants, but increases were small and within acceptable limits. © 2016 Institute of Food Technologists®

Evaluating organochlorine pesticide residues in the aquatic environment of the Lake Naivasha River basin using passive sampling techniques.

PubMed

Abbasi, Yasser; Mannaerts, Chris M

2018-05-18

Passive sampling techniques can improve the discovery of low concentrations by continuous collecting the contaminants, which usually go undetected with classic and once-off time-point grab sampling. The aim of this study was to evaluate organochlorine pesticide (OCP) residues in the aquatic environment of the Lake Naivasha river basin (Kenya) using passive sampling techniques. Silicone rubber sheet and Speedisk samplers were used to detect residues of α-HCH, β-HCH, γ-HCH, δ-HCH, heptachlor, aldrin, heptachlor epoxide, pp-DDE, endrin, dieldrin, α-endosulfan, β-endosulfan, pp-DDD, endrin aldehyde, pp-DDT, endosulfan sulfate, and methoxychlor in the Malewa River and Lake Naivasha. After solvent extraction from the sampling media, the residues were analyzed using gas chromatography electron capture detection (GC-ECD) for the OCPs and gas chromatography-mass spectrometry (GC-MS) for the PCB reference compounds. Measuring the OCP residues using the silicone rubber samplers revealed the highest concentration of residues (∑OCPs of 81 (± 18.9 SD) μg/L) to be at the Lake site, being the ultimate accumulation environment for surficial hydrological, chemical, and sediment transport through the river basin. The total OCP residue sums changed to 71.5 (± 11.3 SD) μg/L for the Middle Malewa and 59 (± 12.5 SD) μg/L for the Upper Malewa River sampling sites. The concentration sums of OCPs detected using the Speedisk samplers at the Upper Malewa, Middle Malewa, and the Lake Naivasha sites were 28.2 (± 4.2 SD), 31.3 (± 1.8 SD), and 34.2 (± 6.4 SD) μg/L, respectively. An evaluation of the different pesticide compound variations identified at the three sites revealed that endosulfan sulfate, α-HCH, methoxychlor, and endrin aldehyde residues were still found at all sampling sites. However, the statistical analysis of one-way ANOVA for testing the differences of ∑OCPs between the sampling sites for both the silicone rubber sheet and Speedisk samplers showed that there was no significant difference from the Upper Malewa to the Lake site (P < 0.05). Finally, the finding of this study indicated that continued monitoring of pesticides residues in the catchment remains highly recommended.

A sampling-based method for ranking protein structural models by integrating multiple scores and features.

PubMed

Shi, Xiaohu; Zhang, Jingfen; He, Zhiquan; Shang, Yi; Xu, Dong

2011-09-01

One of the major challenges in protein tertiary structure prediction is structure quality assessment. In many cases, protein structure prediction tools generate good structural models, but fail to select the best models from a huge number of candidates as the final output. In this study, we developed a sampling-based machine-learning method to rank protein structural models by integrating multiple scores and features. First, features such as predicted secondary structure, solvent accessibility and residue-residue contact information are integrated by two Radial Basis Function (RBF) models trained from different datasets. Then, the two RBF scores and five selected scoring functions developed by others, i.e., Opus-CA, Opus-PSP, DFIRE, RAPDF, and Cheng Score are synthesized by a sampling method. At last, another integrated RBF model ranks the structural models according to the features of sampling distribution. We tested the proposed method by using two different datasets, including the CASP server prediction models of all CASP8 targets and a set of models generated by our in-house software MUFOLD. The test result shows that our method outperforms any individual scoring function on both best model selection, and overall correlation between the predicted ranking and the actual ranking of structural quality.

Diagnosis of neonatal group B Streptococcus sepsis by nested-PCR of residual urine samples

PubMed Central

Cezarino, Bruno Nicolino; Yamamoto, Lidia; Del Negro, Gilda Maria Barbaro; Rocha, Daisy; Okay, Thelma Suely

2008-01-01

Group B streptococcus (GBS) remains the most common cause of early-onset sepsis in newborns. Laboratory gold-standard, broth culture methods are highly specific, but lack sensitivity. The aim of this study was to validate a nested-PCR and to determine whether residue volumes of urine samples obtained by non invasive, non sterile methods could be used to confirm neonatal GBS sepsis. The nested-PCR was performed with primers of the major GBS surface antigen. Unavailability of biological samples to perform life supporting exams, as well as others to elucidate the etiology of infections is a frequent problem concerning newborn patients. Nevertheless, we decided to include cases according to strict criteria: newborns had to present with signs and symptoms compatible with GBS infection; at least one of the following biological samples had to be sent for culture: blood, urine, or cerebrospinal fluid; availability of residue volumes of the samples sent for cultures, or of others collected on the day of hospitalization, prior to antibiotic therapy prescription, to be analyzed by PCR; favorable outcome after GBS empiric treatment. In only one newborn GBS infection was confirmed by cultures, while infection was only presumptive in the other three patients (they fulfilled inclusion criteria but were GBS-culture negative). From a total of 12 biological samples (5 blood, 3 CSF and 4 urine specimen), eight were tested by culture methods (2/8 were positive), and 8 were tested by PCR (7/8 were positive), and only 4 samples were simultaneously tested by both methods (1 positive by culture and 3 by PCR). In conclusion, although based on a restricted number of neonates and samples, our results suggest that the proposed nested-PCR might be used to diagnose GBS sepsis as it has successfully amplified the three types of biological samples analyzed (blood, urine and cerebrospinal fluid), and was more sensitive than culture methods as PCR in urine confirmed diagnosis in all four patients. Moreover, PCR has enabled us to use residue volumes of urine samples collected by non invasive, non sterile methods, what is technically adequate as GBS is not part of the normal urine flora, thus avoiding invasive procedures such as suprapubic bladder punction or transurethral catheterization. At the same time, the use of urine instead of blood samples could help preventing newborns blood spoliation. PMID:24031170

Residual antibacterial activity of chlorhexidine digluconate and camphorated p-monochlorophenol in calcium hydroxide-based root canal dressings.

PubMed

Soares, Janir Alves; Leonardo, Mario Roberto; Tanomaru Filho, Mário; Silva, Léa Assed Bezerra da; Ito, Izabel Yoko

2007-01-01

The purpose of this study was to evaluate the residual antibacterial activity of several calcium hydroxide [Ca(OH)2]-based pastes, placed in root canals of dogs' teeth with induced chronic periapical lesions. Root canals were instrumented with the ProFile rotary system and filled with 4 pastes: G1 (n=16): Ca(OH)2 paste + anesthetic solution; G2 (n=20): Calen paste + camphorated p-monochlorophenol (CMCP); G3 (n=18): Calen; and G4 (n=18): Ca(OH)2 paste + 2% chlorhexidine digluconate. After 21 days, the pastes were removed with size 60 K-files and placed on Petri plates with agar inoculated with Micrococcus luteus ATCC 9341. Pastes that were not placed into root canals served as control. After pre-diffusion, incubation and optimization, the inhibition zones of bacterial growth were measured and analyzed by Mann-Whitney U test at 5% significance level. All pastes showed residual antibacterial activity. The control samples had larger halos (p<0.05). The mean residual antibacterial activity halos in G1, G2, G3 and G4 were 7.6; 10.4; 17.7 and 21.4 mm, respectively. The zones of bacterial growth of G4 were significantly larger than those of G1 and G2 (p<0.05). In conclusion, regardless of the vehicle and antiseptic, all Ca(OH)2-based pastes showed different degrees of measurable residual antibacterial activity. Furthermore, unlike CMCP, chlorhexidine increased significantly the antibacterial activity of Ca(OH)2.

Residues of organochlorine and synthetic pyrethroid pesticides in honey, an indicator of ambient environment, a pilot study.

PubMed

Malhat, Farag M; Haggag, Mohamed N; Loutfy, Naglaa M; Osman, Mohamed A M; Ahmed, Mohamed Tawfic

2015-02-01

Samples of honey were screened to monitor residues of organochlorine and pyrethroid pesticides. The study meant to examine the quality of honey, and to use honey as a bioindicator of environmental contamination. Residue levels were determined by gas chromatography (GC-μECD). Samples had a wide spectrum of organochlorine and synthetic pyrethroids pesticides, with hexachlorobenzene (HCB) as the most frequently detected organochlorine, followed by permethrin, heptachlor epoxide. Only one sample had a concentration of γ-HCH higher than maximum residue limit of honey (0.01 mg kg(-1)). Residues of organochlorines detected, indicate the presence of some fresh supplies, despite the ban imposed on their use. The study confirmed that honey bee and beehive matrices could be used as gauge for monitoring environment contamination. From public health point of view, the observed levels of pesticide residues in honey do not pose a serious health risk to the consumers, but raises questions of the source of organochlorines. Copyright © 2014 Elsevier Ltd. All rights reserved.

Persistence and bioaccumulation of oxyfluorfen residues in onion.

PubMed

Sondhia, Shobha

2010-03-01

A field study was conducted to determine persistence and bioaccumulation of oxyflorfen residues in onion crop at two growth stages. Oxyfluorfen (23.5% EC) was sprayed at 250 and 500 g ai/ha on the crop (variety, N53). Mature onion and soil samples were collected at harvest. Green onion were collected at 55 days from each treated and control plot and analyzed for oxyfluorfen residues by a validated high-performance liquid chromatography method with an accepted recovery of 78-92% at the minimum detectable concentration of 0.003 microg g(-1). Analysis showed 0.015 and 0.005 microg g(-1) residues of oxyfluorfen at 250 g a.i. ha(-1) rate in green and mature onion samples, respectively; however, at 500 g a.i.ha(-1) rates, 0.025 and 0.011 microg g(-1) of oxyfluorfen residues were detected in green and mature onion samples, respectively. Soil samples collected at harvest showed 0.003 and 0.003 microg g(-1) of oxyfluorfen residues at the doses 250 and 500 g a.i. ha(-1), respectively. From the study, a pre-harvest interval of 118 days for onion crop after the herbicide application is suggested.

Overview of pesticide residues in stored pollen and their potential effect on bee colony (Apis mellifera) losses in Spain.

PubMed

Bernal, J; Garrido-Bailón, E; Del Nozal, M J; González-Porto, A V; Martín-Hernández, R; Diego, J C; Jiménez, J J; Bernal, J L; Higes, M

2010-12-01

In the last decade, an increase in honey bee (Apis mellifera L.) colony losses has been reported in several countries. The causes of this decline are still not clear. This study was set out to evaluate the pesticide residues in stored pollen from honey bee colonies and their possible impact on honey bee losses in Spain. In total, 1,021 professional apiaries were randomly selected. All pollen samples were subjected to multiresidue analysis by gas chromatography-mass spectrometry (MS) and liquid chromatography-MS; moreover, specific methods were applied for neonicotinoids and fipronil. A palynological analysis also was carried out to confirm the type of foraging crop. Pesticide residues were detected in 42% of samples collected in spring, and only in 31% of samples collected in autumn. Fluvalinate and chlorfenvinphos were the most frequently detected pesticides in the analyzed samples. Fipronil was detected in 3.7% of all the spring samples but never in autumn samples, and neonicotinoid residues were not detected. More than 47.8% of stored pollen samples belonged to wild vegetation, and sunflower (Heliantus spp.) pollen was only detected in 10.4% of the samples. A direct relation between pesticide residues found in stored pollen samples and colony losses was not evident accordingly to the obtained results. Further studies are necessary to determine the possible role of the most frequent and abundant pesticides (such as acaricides) and the synergism among them and with other pathogens more prevalent in Spain.

Food safety in Thailand 2: Pesticide residues found in Chinese kale (Brassica oleracea), a commonly consumed vegetable in Asian countries.

PubMed

Wanwimolruk, Sompon; Kanchanamayoon, Onnicha; Phopin, Kamonrat; Prachayasittikul, Virapong

2015-11-01

There is increasing public concern over human health risks associated with extensive use of pesticides in agriculture. Regulation of pesticide maximum residue limits (MRLs) in food commodities is established in many developed countries. For Thailand, this regulation exists in law but is not fully enforced. Therefore, pesticide residues in vegetables and fruits have not been well monitored. This study investigated the pesticide residues in Chinese kale, a commonly eaten vegetable among Asians. The Chinese kale samples (N = 117) were purchased from markets in Nakhon Pathom Province, Thailand, and analyzed for the content of 28 pesticides. Analysis was performed by the multiresidual extraction followed by GC-MS/MS. Of pesticides investigated, 12 pesticides were detected in 85% of the Chinese kale samples. Although carbaryl, deltamethrin, diazinon, fenvalerate and malathion were found in some samples, their levels were lower than their MRLs. However, in 34 samples tested, either carbofuran, chlorpyrifos, chlorothalonil, cypermethrin, dimethoate, metalaxyl or profenofos was detected exceeding their MRLs. This represents a 29% rate of pesticide detection above the MRL; a rate much higher than in developed countries. Washing vegetables under running water significantly reduced (p < 0.05) profenofos residues by 55%. The running water method did not significantly decrease cypermethrin residues in the samples but washing with vinegar did. Our research suggests that routine monitoring of pesticide residues is necessary to reduce the public health risks associated with eating contaminated vegetables. Washing vegetables before consumption is advisable as this helps to reduce the level of pesticide residues in our daily intake. Copyright © 2015 Elsevier B.V. All rights reserved.

Organophosphorous residue in Liza aurata and Cyprinus carpio

PubMed Central

Shayeghi, Mansoreh; Khoobdel, Mehdi; Bagheri, Fatemeh; Abtahi, Mohammad; Zeraati, Hojjatollah

2012-01-01

Objective To determine the amount of azinphos methyl and diazinon residues in two river fishes, Liza aurata and Cyprinus carpio, in the north of Iran. Methods This study was done during 2006-2007. In this survey, 152 water and fish samples from Gorgan and Qarasu rivers, north of Iran, were investigated. Sampling was done in three predetermined stations along each river. Organophosphorus compounds (OPs) were extracted from the fishes and the water of rivers. After extraction, purification and concentration processes, the amount and type of insecticides in water and fish samples were determined by high performance thin layer chromatography (HPTLC). Results There was a significant difference in the residue of the insecticides in the water and fish samples between summer and other seasons in the two rivers. The highest amount of insecticides residue was seen during summer. In both rivers, the amount of diazinon and azinphos methyl residues in the two fishes was more than 2 000 mg/L in summer. There was no significant difference in insecticides residue between the fishes in two rivers. The diazinon residue was higher than the standard limits in both rivers during the spring and the summer, but the residual amount of azinphos methyl was higher than the standard limits only during the summer and only in Qarasu River. Conclusions It can be concluded that the amount of OPs in the water and the two fishes, Liza aurata and Cyprinus carpio, is higher than the permitted levels. PMID:23569972

Microbiological quality and antibiotic residues in informally marketed raw cow milk within the coastal savannah zone of Ghana.

PubMed

Addo, K K; Mensah, G I; Aning, K G; Nartey, N; Nipah, G K; Bonsu, C; Akyeh, M L; Smits, H L

2011-02-01

To investigate the microbiological quality and the presence of antibiotic residues in raw cow milk and in some indigenous milk products produced and marketed by the informal sector in the coastal savannah zone of Ghana. Milk samples were aseptically collected from 224 kraals and samples of 26 indigenous milk products were purchased from processors and retailers. Total plate counts, total coliform counts and the presence of Escherichia coli and E. coli O157:H7 were determined in all 250 samples. Milk samples were also tested for antibiotic residues. Total plate counts exceeded 10⁵ CFU/ml in 45.2% of the samples while coliforms exceeded 10³ CFU/ml in 66.0% and E. coli was detected in 11.2%. E. coli was present in raw cow milk but not in the indigenous products and all E. coli isolates were negative for E. coli O157:H7. Antibiotic residues were detected in 3.1% of the raw cow milk samples. Bulk milk contains unacceptable levels of hygiene indicators and antibiotic residues and is a potential source of milk-borne infections. The detection of E. coli and antibiotic residues raises public health concerns about the safety of fresh unpasteurized cow milk in the coastal savannah zone of Ghana and calls for improved farm hygiene, the need for milk pasteurization and the sensible use of antibiotics in the milk industry. © 2010 Blackwell Publishing Ltd.

Development of QuEChERS-based extraction and liquid chromatography-tandem mass spectrometry method for quantifying flumethasone residues in beef muscle.

PubMed

Park, Ki Hun; Choi, Jeong-Heui; Abd El-Aty, A M; Cho, Soon-Kil; Park, Jong-Hyouk; Kwon, Ki Sung; Park, Hee Ra; Kim, Hyung Soo; Shin, Ho-Chul; Kim, Mi Ra; Shim, Jae-Han

2012-12-01

A rapid, specific, and sensitive method based on liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM) was developed and validated to quantify flumethasone residues in beef muscle. Methods were compared between the original as well as the EN quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based extraction. Good linearity was achieved at concentration levels of 5-30 μg/kg. Estimated recovery rates at spiking levels of 5 and 10 μg/kg ranged from 72.1 to 84.6%, with relative standard deviations (RSDs)<7%. The results of the inter-day study, which was performed by fortifying beef muscle samples (n=18) on 3 separate days, showed an accuracy of 93.4-94.4%. The precision (expressed as relative standard deviation values) for the inter-day variation at two levels of fortification (10 and 20 μg/kg) was 1.9-5.2%. The limit of detection (LOD) and limit of quantitation (LOQ) were 1.7 and 5 μg/kg, at signal-to-noise ratios (S/Ns) of 3 and 10, respectively. The method was successfully applied to analyze real samples obtained from large markets throughout the Korean Peninsula. The method proved to be sensitive and reliable and, thus, rendered an appropriate means for residue analysis studies. Copyright © 2012 Elsevier Ltd. All rights reserved.

Monitoring of pesticide residues of five notable vegetables at Agbogbloshie market in Accra, Ghana.

PubMed

Osei-Fosu, P; Donkor, A K; Nyarko, S; Nazzah, N K; Asante, I K; Kingsford-Adabo, R; Arkorful, N A

2014-11-01

The study monitored the concentrations of pesticide residues in vegetables arriving at Agbogbloshie, a central market in the Accra Metropolis from different parts of Ghana and beyond. A total of 810 samples of 5 different vegetables from Central, Volta, Greater Accra, Ashanti, Eastern Regions, and neighboring country (Togo) were collected from January 2009 through to December 2011. In all, 18 % of the samples had no detectable residues, 62 % were below the maximum residue limits (MRLs), and 20 % also exceeded the EU (MRLs) adopted values. Overall, lettuce contained the highest number of residues above their MRLs besides cucumber and cabbage. The pesticide residues were mainly organophosphates and synthetic pyrethroids. The results demonstrate the need for continuous monitoring of pesticide residues in vegetables arriving at the various major markets in Ghana.

Leaching characteristics of fly ash from thermal power plants of Soma and Tuncbilek, Turkey.

PubMed

Baba, Alper; Kaya, Abidin

2004-02-01

Use of lignite in power generation has led to increasing environmental problems associated not only with gaseous emissions but also with the disposal of ash residues. In particular, use of low quality coal with high ash content results in huge quantities of fly ash to be disposed of. The main problem related to fly ash disposal is the heavy metal content of the residue. In this regard, experimental results of numerous studies indicate that toxic trace metals may leach when fly ash contacts water. In this study, fly ash samples obtained from thermal power plants, namely Soma and Tunçbilek, located at the west part of Turkey, were subjected to toxicity tests such as European Committee for standardization (CEN) and toxicity characteristic leaching (TCLP) procedures of the U.S. Environmental Protection Agency (U.S. EPA). The geochemical composition of the tested ash samples from the power plant show variations depending on the coal burned in the plants. Furthermore, the CEN and TCLP extraction results showed variations such that the ash samples were classified as 'toxic waste' based on TCLP result whereas they were classified as 'non-toxic' wastes based on CEN results, indicating test results are pH dependent.

A High-Throughput Enzyme Assay for Organophosphate Residues in Milk

PubMed Central

Mishra, Rupesh K.; Deshpande, Kanchanmala; Bhand, Sunil

2010-01-01

A rapid, high-sensitivity, chemiluminescence (CL) enzyme assay for the determination of organophosphate (OP) residues in milk is presented. The assay for quantification of OP residues in milk is based on the inhibition of enzyme butyrylcholinesterase (BuChE). BuChE was stabilized and preloaded in 384 well plates at 30 °C. The assay permits rapid determination of OPs in milk within 12 min including an incubation step. The enzyme assay was tested for individual and mixtures of OPs such as methyl paraoxon (MPOx), methyl parathion (MP) and malathion (MT) in milk to evaluate their synergistic effect on BuChE inhibition. Good linearity was obtained in the range 0.005–50 μg·L−1 for MPOx and 0.5–1,000 μg·L−1 for MP as well as MT in milk. Mean recovery of 93.2%–98.6% was obtained for MPOx spiked milk samples with 0.99%–1.67% reproducibility (RSD). The proposed method facilitated rapid screening of milk samples in 384 well plate formats with further miniaturization presented in 1,536 well plates. PMID:22163525

Multi-pesticides residue analysis of grains using modified magnetic nanoparticle adsorbent for facile and efficient cleanup.

PubMed

Liu, Zhenzhen; Qi, Peipei; Wang, Xiangyun; Wang, Zhiwei; Xu, Xiahong; Chen, Wenxue; Wu, Liyu; Zhang, Hu; Wang, Qiang; Wang, Xinquan

2017-09-01

A facile, rapid sample pretreatment method was developed based on magnetic nanoparticles for multi-pesticides residue analysis of grains. Magnetite (Fe 3 O 4 ) nanoparticles modified with 3-(N,N-diethylamino)propyltrimethoxysilane (Fe 3 O 4 -PSA) and commercial C18 were selected as the cleanup adsorbents to remove the target interferences of the matrix, such as fatty acids and non-polar compounds. Rice was used as the representative grain sample for method optimization. The amount of Fe 3 O 4 -PSA and C18 were systematically investigated for selecting the suitable purification conditions, and the simultaneous determination of 50 pesticides and 8 related metabolites in rice was established by liquid chromatography-tandem mass spectrometry. Under the optimal conditions, the method validation was performed including linearity, sensitivity, matrix effect, recovery and precision, which all satisfy the requirement for pesticides residue analysis. Compared to the conventional QuEChERS method with non-magnetic material as cleanup adsorbent, the present method can save 30% of the pretreatment time, giving the high throughput analysis possible. Copyright © 2017 Elsevier Ltd. All rights reserved.

Molecularly imprinted solid-phase extraction for the determination of ten macrolide drugs residues in animal muscles by liquid chromatography-tandem mass spectrometry.

PubMed

Song, Xuqin; Zhou, Tong; Liu, Qingying; Zhang, Meiyu; Meng, Chenying; Li, Jiufeng; He, Limin

2016-10-01

A simple and sensitive method based on molecularly imprinted solid-phase extraction coupled with liquid chromatography-tandem mass spectrometry was developed for the determination of the residues of ten macrolide drugs in swine, cattle and chicken muscles samples. The molecularly imprinted polymers (MIPs) were synthesized using tylosin as a template and methacrylic acid as a functional monomer. Samples were extracted with sodium borate buffer solution and ethyl acetate, and purified by the MIP cartridge. The results showed that the cartridge exhibited good recognition performance for macrolides, and better purification effect than the traditional solid-phase extraction cartridges. Recoveries of analytes at three spiking levels 1, 5 and 20μgkg(-1) ranged from 60.7% to 100.3% with the relative standard deviations less than 14%. The limits of detection of the method were between 0.1 and 0.4μgkg(-1). The method is useful for the routine monitoring of the residues of macrolide drugs in animal muscles. Copyright © 2016 Elsevier Ltd. All rights reserved.

Determination of ethephon residues in water by gas chromatography with cubic mass spectrometry after ion-exchange purification and derivatisation with N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide.

PubMed

Royer, A; Laporte, F; Bouchonnet, S; Communal, P-Y

2006-03-03

An analytical method has been developed for the determination of residues of ethephon (2-chloroethyl phosphonic acid) in drinking and surface water. The procedure is based on de-ionisation with an anion/cation-exchange resin, solid phase extraction by means of anion-exchange polystyrene-divinylbenzene extraction disks, elution with a mixture of methanol and 10 M hydrochloric acid (98/2, v/v), redisolution into acetonitrile after evaporation and silylation with N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA). Quantification is performed by gas chromatography with ion-trap cubic mass spectrometric detection in the electron impact mode (GC-EI-MS3). Method validation was conducted using samples of mineral, tap, and river water that were fortified with ethephon at concentration levels ranging from 0.1 to 1.0 microg/L. The mean recovery from all the fortified samples (n = 36) amounted to 88% with a relative standard deviation of 17%. The method, therefore, was shown to allow accurate determination of ethephon residues in drinking and surface water with a limit of quantification of 0.1 microg/L.

Monitoring of pesticide residues in vegetarian diet.

PubMed

Kumari, Beena; Kathpal, T S

2009-04-01

Samples (28) of complete vegetarian diet consumed from morning till night i.e. tea, milk, breakfast, lunch, snacks, dinner, sweet dish etc. were collected from homes, hostels and hotels periodically from Hisar and analysed for detecting the residues of organochlorine, synthetic pyrethriod, organophosphate and carbamate insecticides. The estimation was carried out by using multi-residue analytical technique employing gas chromatograph (GC)-electron capture detector and GC-nitrogen phosphorous detector systems equipped with capillary columns. The whole diet sample was macerated in a mixer grinder and a representative sample in duplicate was analyzed for residues keeping the average daily diet of an adult to be 1,300 g. On comparing the data, it was found that actual daily intake (microgram/person/day) of lindane in two and endosulfan in four samples exceeded the acceptable daily intake. Residues of other pesticides in all the diet samples were lower than the acceptable daily intake (ADI) of the respective pesticides. The study concluded that although all the diet samples were found contaminated with one or the other pesticide, the actual daily intake of only a few pesticides was higher than their respective ADI. More extensive study covering other localities of Haryana has been suggested to know the overall scenario of contamination of vegetarian diet.

Detecting spatial structures in throughfall data: the effect of extent, sample size, sampling design, and variogram estimation method

NASA Astrophysics Data System (ADS)

Voss, Sebastian; Zimmermann, Beate; Zimmermann, Alexander

2016-04-01

In the last three decades, an increasing number of studies analyzed spatial patterns in throughfall to investigate the consequences of rainfall redistribution for biogeochemical and hydrological processes in forests. In the majority of cases, variograms were used to characterize the spatial properties of the throughfall data. The estimation of the variogram from sample data requires an appropriate sampling scheme: most importantly, a large sample and an appropriate layout of sampling locations that often has to serve both variogram estimation and geostatistical prediction. While some recommendations on these aspects exist, they focus on Gaussian data and high ratios of the variogram range to the extent of the study area. However, many hydrological data, and throughfall data in particular, do not follow a Gaussian distribution. In this study, we examined the effect of extent, sample size, sampling design, and calculation methods on variogram estimation of throughfall data. For our investigation, we first generated non-Gaussian random fields based on throughfall data with heavy outliers. Subsequently, we sampled the fields with three extents (plots with edge lengths of 25 m, 50 m, and 100 m), four common sampling designs (two grid-based layouts, transect and random sampling), and five sample sizes (50, 100, 150, 200, 400). We then estimated the variogram parameters by method-of-moments and residual maximum likelihood. Our key findings are threefold. First, the choice of the extent has a substantial influence on the estimation of the variogram. A comparatively small ratio of the extent to the correlation length is beneficial for variogram estimation. Second, a combination of a minimum sample size of 150, a design that ensures the sampling of small distances and variogram estimation by residual maximum likelihood offers a good compromise between accuracy and efficiency. Third, studies relying on method-of-moments based variogram estimation may have to employ at least 200 sampling points for reliable variogram estimates. These suggested sample sizes exceed the numbers recommended by studies dealing with Gaussian data by up to 100 %. Given that most previous throughfall studies relied on method-of-moments variogram estimation and sample sizes << 200, our current knowledge about throughfall spatial variability stands on shaky ground.

Detecting spatial structures in throughfall data: The effect of extent, sample size, sampling design, and variogram estimation method

NASA Astrophysics Data System (ADS)

Voss, Sebastian; Zimmermann, Beate; Zimmermann, Alexander

2016-09-01

In the last decades, an increasing number of studies analyzed spatial patterns in throughfall by means of variograms. The estimation of the variogram from sample data requires an appropriate sampling scheme: most importantly, a large sample and a layout of sampling locations that often has to serve both variogram estimation and geostatistical prediction. While some recommendations on these aspects exist, they focus on Gaussian data and high ratios of the variogram range to the extent of the study area. However, many hydrological data, and throughfall data in particular, do not follow a Gaussian distribution. In this study, we examined the effect of extent, sample size, sampling design, and calculation method on variogram estimation of throughfall data. For our investigation, we first generated non-Gaussian random fields based on throughfall data with large outliers. Subsequently, we sampled the fields with three extents (plots with edge lengths of 25 m, 50 m, and 100 m), four common sampling designs (two grid-based layouts, transect and random sampling) and five sample sizes (50, 100, 150, 200, 400). We then estimated the variogram parameters by method-of-moments (non-robust and robust estimators) and residual maximum likelihood. Our key findings are threefold. First, the choice of the extent has a substantial influence on the estimation of the variogram. A comparatively small ratio of the extent to the correlation length is beneficial for variogram estimation. Second, a combination of a minimum sample size of 150, a design that ensures the sampling of small distances and variogram estimation by residual maximum likelihood offers a good compromise between accuracy and efficiency. Third, studies relying on method-of-moments based variogram estimation may have to employ at least 200 sampling points for reliable variogram estimates. These suggested sample sizes exceed the number recommended by studies dealing with Gaussian data by up to 100 %. Given that most previous throughfall studies relied on method-of-moments variogram estimation and sample sizes ≪200, currently available data are prone to large uncertainties.

Development of a Simple Dipstick Assay for Operational Monitoring of DDT.

PubMed

Ismail, Hanafy M; Kumar, Vijay; Singh, Rudra P; Williams, Christopher; Shivam, Pushkar; Ghosh, Ayan; Deb, Rinki; Foster, Geraldine M; Hemingway, Janet; Coleman, Michael; Coleman, Marlize; Das, Pradeep; Paine, Mark J I

2016-01-01

Indoor residual spraying (IRS) of DDT is used to control visceral leishmaniasis (VL) in India. However, the quality of spraying is severely compromised by a lack of affordable field assays to monitor target doses of insecticide. Our aim was to develop a simple DDT insecticide quantification kit (IQK) for monitoring DDT levels in an operational setting. DDT quantification was based on the stoichiometric release of chloride from DDT by alkaline hydrolysis and detection of the released ion using Quantab chloride detection strips. The assay was specific for insecticidal p,p`-DDT (LoQ = 0.082 g/m2). Bostik discs were effective in post spray wall sampling, extracting 25-70% of active ingredient depending on surface. Residual DDT was sampled from walls in Bihar state in India using Bostik adhesive discs and DDT concentrations (g p,p`-DDT/m2) were determined using IQK and HPLC (n = 1964 field samples). Analysis of 161 Bostik samples (pooled sample pairs) by IQK and HPLC produced excellent correlation (R2 = 0.96; Bland-Altman bias = -0.0038). IQK analysis of the remaining field samples matched HPLC data in identifying households that had been under sprayed, in range or over sprayed. A simple dipstick assay has been developed for monitoring DDT spraying that gives comparable results to HPLC. By making laboratory-based analysis of DDT dosing accessible to field operatives, routine monitoring of DDT levels can be promoted in low- and middle- income countries to maximise the effectiveness of IRS.

Screening of pesticide residues in soil and water samples from agricultural settings

PubMed Central

Akogbéto, Martin C; Djouaka, Rousseau F; Kindé-Gazard, Dorothée A

2006-01-01

Background The role of agricultural practices in the selection of insecticide resistance in malaria vectors has so far been hypothesized without clear evidence. Many mosquito species, Anopheles gambiae in particular, lay their eggs in breeding sites located around agricultural settings. There is a probability that, as a result of farming activities, insecticide residues may be found in soil and water, where they exercise a selection pressure on the larval stage of various populations of mosquitoes. To confirm this hypothesis, a study was conducted in the Republic of Benin to assess the environmental hazards which can be generated from massive use of pesticides in agricultural settings. Methods Lacking an HPLC machine for direct quantification of insecticide residues in samples, this investigation was performed using indirect bioassays focussed on the study of factors inhibiting the normal growth of mosquito larvae in breeding sites. The speed of development was monitored as well as the yield of rearing An. gambiae larvae in breeding sites reconstituted with water and soil samples collected in agricultural areas known to be under pesticide pressure. Two strains of An. gambiae were used in this indirect bioassay: the pyrethroid-susceptible Kisumu strain and the resistant Ladji strain. The key approach in this methodology is based on comparison of the growth of larvae in test and in control breeding sites, the test samples having been collected from two vegetable farms. Results Results obtained clearly show the presence of inhibiting factors on test samples. A normal growth of larvae was observed in control samples. In breeding sites simulated by using a few grams of soil samples from the two vegetable farms under constant insecticide treatments (test samples), a poor hatching rate of Anopheles eggs coupled with a retarded growth of larvae and a low yield of adult mosquitoes from hatched eggs, was noticed. Conclusion Toxic factors inhibiting the hatching of anopheles eggs and the growth of larvae are probably pesticide residues from agricultural practices. Samples used during this indirect assay have been stored in the laboratory and will be analysed with HPLC techniques to confirm hypothesis of this study and to identify the various end products found in soil and water samples from agricultural settings under pesticide pressure. PMID:16563153

Validity of Gō models: comparison with a solvent-shielded empirical energy decomposition.

PubMed

Paci, Emanuele; Vendruscolo, Michele; Karplus, Martin

2002-12-01

Do Gō-type model potentials provide a valid approach for studying protein folding? They have been widely used for this purpose because of their simplicity and the speed of simulations based on their use. The essential assumption in such models is that only contact interactions existing in the native state determine the energy surface of a polypeptide chain, even for non-native configurations sampled along folding trajectories. Here we use an all-atom molecular mechanics energy function to investigate the adequacy of Gō-type potentials. We show that, although the contact approximation is accurate, non-native contributions to the energy can be significant. The assumed relation between residue-residue interaction energies and the number of contacts between them is found to be only approximate. By contrast, individual residue energies correlate very well with the number of contacts. The results demonstrate that models based on the latter should give meaningful results (e.g., as used to interpret phi values), whereas those that depend on the former are only qualitative, at best.

Residual stress analysis of energy-dispersive diffraction data using a two-detector setup: Part I - Theoretical concept

NASA Astrophysics Data System (ADS)

Apel, Daniel; Meixner, Matthias; Liehr, Alexander; Klaus, Manuela; Degener, Sebastian; Wagener, Guido; Franz, Christian; Zinn, Wolfgang; Genzel, Christoph; Scholtes, Berthold

2018-01-01

A new goniometer setup for energy-dispersive X-ray diffraction is introduced which is based on simultaneous data acquisition with two detectors D1 and D2, both of them freely movable in a horizontal as well as in a vertical plane. From the multitude of measurement configurations that can be realised with this setup, we figured out three efficient concepts which aim at the fast analysis of residual stress depth profiles by combining the diffraction data gathered with the two detectors. The characteristic feature of the first two configurations consists in the vertical (horizontal) positioning of the first (second) detector, which results in a diffraction geometry where the two scattering vectors span a plane that coincides with the X-circle used for sample tilt. Because each detector does see the sample under another viewing angle, both the positive and the negative ψ-branch are covered by just one χ-tilt between 0°and 90°(configuration 1) and 0°and 60°(configuration 2), thus allowing for the simultaneous analysis of the in- and out-of-plane residual stress depth gradients σii(τ) and σi3(τ) (i = 1 , 2), respectively, from data sets dD1hkl(χ) and dD2hkl(χ). The third configuration introduced in this paper is based on a ϕ-rotation of the sample under a constant tilt angle χ and enables a fast and reliable tracing of shear stress fields σi3(τ) (i = 1, 2).

Pesticide Residues in Food: Attitudes, Beliefs, and Misconceptions among Conventional and Organic Consumers.

PubMed

Koch, Severine; Epp, Astrid; Lohmann, Mark; Böl, Gaby-Fleur

2017-12-01

Pesticide use and pesticide residues in foods have been the subject of controversial public discussions and media coverage in Germany. Against this background, a better understanding of public risk perceptions is needed to promote efficient public health communication. To this end, this study captures the German public's perception of pesticide residues in foods. A representative sample of the population aged 14 years and older (n = 1,004) was surveyed via computer-assisted telephone interviewing on their attitudes and knowledge with regard to pesticide residues. Based on questions regarding their typical consumer behavior, respondents were classified into conventional and organic consumers to identify differences as well as similarities between these two consumer types. As assessed with an open-ended question, both organic and conventional consumers viewed pesticides, chemicals, and toxins as the greatest threats to food quality and safety. Evaluating the risks and benefits of pesticide use, more than two-thirds of organic consumers (70%) rated the risks as greater than the benefits, compared with just over one-half of conventional consumers (53%). Concern about the detection of pesticide residues in the food chain and bodily fluids was significantly higher among organic compared with conventional consumers. Only a minority of respondents was aware that legal limits for pesticide residues (referred to as maximum residue levels) exist, with 69% of organic and 61% of conventional consumers believing that the presence of pesticide residues in foods is generally not permitted. A lack of awareness of maximum residue levels was associated with heightened levels of concern about pesticide residues. Finally, general exposure to media reporting on pesticide residues was associated with more frequent knowledge of legal limits for pesticide residues, whereas actively seeking information on pesticide residues was not. The possible mechanisms underlying these findings are discussed.

Human errors and measurement uncertainty

NASA Astrophysics Data System (ADS)

Kuselman, Ilya; Pennecchi, Francesca

2015-04-01

Evaluating the residual risk of human errors in a measurement and testing laboratory, remaining after the error reduction by the laboratory quality system, and quantifying the consequences of this risk for the quality of the measurement/test results are discussed based on expert judgments and Monte Carlo simulations. A procedure for evaluation of the contribution of the residual risk to the measurement uncertainty budget is proposed. Examples are provided using earlier published sets of expert judgments on human errors in pH measurement of groundwater, elemental analysis of geological samples by inductively coupled plasma mass spectrometry, and multi-residue analysis of pesticides in fruits and vegetables. The human error contribution to the measurement uncertainty budget in the examples was not negligible, yet also not dominant. This was assessed as a good risk management result.

Pesticide residues in grain from Kazakhstan and potential health risks associated with exposure to detected pesticides.

PubMed

Lozowicka, B; Kaczynski, P; Paritova, Capital A Cyrillic Е; Kuzembekova, G B; Abzhalieva, A B; Sarsembayeva, N B; Alihan, K

2014-02-01

This paper presents the first study of pesticide residue results in grain from Kazakhstan. A total of 80 samples: barley, oat, rye, and wheat were collected and tested in the accredited laboratory. Among 180 pesticides, 10 active substances were detected. Banned pesticides, such as DDTs, γ-HCH, aldrin and diazinon were found in cereal grain. Chlorpyrifos methyl and pirimiphos methyl were the most frequently detected residues. No residues were found in 77.5% of the samples, 13.75% contained pesticide residues at or below MRLs, and 8.75% above MRLs. The greatest percentage of samples with residues (29%) was noted for wheat, and the lowest for rye (20%). Obtained data were used to estimate potential health risks associated with exposure to these pesticides. The highest estimated daily intakes (EDIs) were as follows: 789% of the ADI for aldrin (wheat) and 49.8% of the ADI for pirimiphos methyl (wheat and rye). The acute risk from aldrin and tebuconazole in wheat was 315.9% and 98.7% ARfD, respectively. The results show that despite the highest EDIs of pesticide residues in cereals, the current situation could not be considered a serious public health problem. Nevertheless, an investigation into continuous monitoring of pesticide residues in grain is recommended. Copyright © 2013 Elsevier Ltd. All rights reserved.

Consumer exposure to pesticide residues in apples from the region of south-eastern Poland.

PubMed

Szpyrka, Ewa; Kurdziel, Anna; Słowik-Borowiec, Magdalena; Grzegorzak, Magdalena; Matyaszek, Aneta

2013-11-01

The production of apples in Poland is the largest among the countries of the European Union, and therefore, the consumption of these fruits is high in our country. The aim of this study was to determine the presence of pesticide residues in Polish apples and to assess if these residues pose a risk to the health of the consumer. Furthermore, compliance with legal regulations concerning the use of plant protection products in crop cultivation was ascertained. Pesticide residues were found in 192 samples (61.5% of tested samples). In six samples (1.9%), residues exceeded maximum residue limits. Violations concerned the insecticides: indoxacarb, diazinon and fenitrothion. The highest long-term consumer exposure was found in the case of consumption of apples with diazinon residue for both groups, adults and toddlers [4% acceptable daily intake (ADI), adults; 21% ADI, toddlers]. The highest values of short-term exposure were obtained in the case of consumption of apples with indoxacarb [5% acute reference dose (ARfD), adults; 27% ARfD, toddlers] and fenitrothion (4% ARfD, adults; 23% ARfD, toddlers). Although fungicides are the pesticides found most often in apples, the consumption of apples with insecticide residues constitutes the greatest hazard to human health.

Determination of benazolin-ethyl residues in soil and rape seed by SPE clean-up and GC with electron capture detection.

PubMed

Liu, Xiaolu; Yang, Tao; Hu, Jiye

2013-01-01

A method has been developed and established for residue determination of benazolin-ethyl in soil and rape seed samples by gas chromatography with electron capture detection (GC-ECD). Limits of quantification of the method are 0.005 mg/kg for both soil and rape seed, which are sufficiently below the maximum residue limit, and the limit of detection is 0.0023 ng. The average recoveries of the analyte range from 85.89 to 105.84% with relative standard deviations (coefficient of variation) less than 5.53% at the three spike levels (0.005, 0.1 and 0.5 mg/kg). The half-life of benazolin-ethyl in soil from the experimental field is 4.62 days. The final residues of benazolin-ethyl in soil and rape seed samples are lower than 0.005 mg/kg at harvest time. Direct confirmation of the analyte in real samples is achieved by GC-mass spectrometry. It is demonstrated that the proposed method is simple, rapid and efficient, and reliable to detect benazolin-ethyl residues in soil and rape seed samples.

Residual Stress Measurement and Calibration for A7N01 Aluminum Alloy Welded Joints by Using Longitudinal Critically Refracted ( LCR) Wave Transmission Method

NASA Astrophysics Data System (ADS)

Zhu, Qimeng; Chen, Jia; Gou, Guoqing; Chen, Hui; Li, Peng; Gao, W.

2016-10-01

Residual stress measurement and control are highly important for the safety of structures of high-speed trains, which is critical for the structure design. The longitudinal critically refracted wave technology is the most widely used method in measuring residual stress with ultrasonic method, but its accuracy is strongly related to the test parameters, namely the flight time at the free-stress condition ( t 0), stress coefficient ( K), and initial stress (σ0) of the measured materials. The difference of microstructure in the weld zone, heat affected zone, and base metal (BM) results in the divergence of experimental parameters. However, the majority of researchers use the BM parameters to determine the residual stress in other zones and ignore the initial stress (σ0) in calibration samples. Therefore, the measured residual stress in different zones is often high in errors and may result in the miscalculation of the safe design of important structures. A serious problem in the ultrasonic estimation of residual stresses requires separation between the microstructure and the acoustoelastic effects. In this paper, the effects of initial stress and microstructure on stress coefficient K and flight time t 0 at free-stress conditions have been studied. The residual stress with or without different corrections was investigated. The results indicated that the residual stresses obtained with correction are more accurate for structure design.

Smoothing data series by means of cubic splines: quality of approximation and introduction of a repeating spline approach

NASA Astrophysics Data System (ADS)

Wüst, Sabine; Wendt, Verena; Linz, Ricarda; Bittner, Michael

2017-09-01

Cubic splines with equidistant spline sampling points are a common method in atmospheric science, used for the approximation of background conditions by means of filtering superimposed fluctuations from a data series. What is defined as background or superimposed fluctuation depends on the specific research question. The latter also determines whether the spline or the residuals - the subtraction of the spline from the original time series - are further analysed.Based on test data sets, we show that the quality of approximation of the background state does not increase continuously with an increasing number of spline sampling points and/or decreasing distance between two spline sampling points. Splines can generate considerable artificial oscillations in the background and the residuals.We introduce a repeating spline approach which is able to significantly reduce this phenomenon. We apply it not only to the test data but also to TIMED-SABER temperature data and choose the distance between two spline sampling points in a way that is sensitive for a large spectrum of gravity waves.

ESTIMATING CHILDREN'S DERMAL AND NON-DIETARY INGESTION EXPOSURE AND DOSE WITH EPA'S SHEDS MODEL

EPA Science Inventory

A physically-based stochastic model (SHEDS) has been developed to estimate pesticide exposure and dose to children via dermal residue contact and non-dietary ingestion. Time-location-activity data are sampled from national survey results to generate a population of simulated ch...

CTEPP STANDARD OPERATING PROCEDURE FOR COLLECTION OF DISLODGEABLE RESIDUES -- PUF ROLLER SAMPLES FOR PERSISTENT ORGANIC POLLUTANTS (SOP-2.18)

EPA Science Inventory

This SOP describes the method to collect transferable residues from indoor floor surfaces. The sampling procedures described are applicable to bare floors or covered floor surfaces, e.g., carpeting and vinyl flooring. The samples will be collected only in the day care centers o...

Organochlorine insecticide residues are found in surface, irrigated water samples from several districts in Bangladesh.

PubMed

Chowdhury, Alamgir Zaman; Islam, Mohammad Nazrul; Moniruzzaman, Mohammed; Gan, Siew Hua; Alam, Md Khorshed

2013-02-01

The purpose of this study was to investigate the occurrence and distribution of organochlorines such as aldrin, dieldrin, dichlorodiphenyldichloroethylene (DDE), dichlorodiphenyldichloroethane (DDD), dichlorodiphenyltrichloroethane (DDT), endrin, lindane and heptachlor insecticide residues in irrigated surface water samples collected from 22 districts in Bangladesh. The concentrations of the pesticides were determined using gas chromatography mass spectrophotometry. Water samples from five locations (Feni, Nawabganj, Putia, Burichang and Chatak) were contaminated with DDT; the highest DDT concentration detected was 8.29 μg/L, and its metabolite, DDE, was detected at 4.06 μg/L. Water samples from four other locations (Natore, Sikderpara, Chatak and Rajoir) were contaminated with heptachlor residues, and the highest level detected was 5.24 μg/L, which is the above the maximum contaminant level recommended by the World Health Organisation. A water sample collected from Chatak, Sunamganj, was contaminated with both DDT and heptachlor pesticide residues. None of the water samples were contaminated with aldrin, DDD, dieldrin, endrin or lindane. It is concluded that continuous, long-term monitoring and essential steps to limit the use of the pesticides in Bangladesh are needed.

Risk assessment and risk management at the Canadian Food Inspection Agency (CFIA): a perspective on the monitoring of foods for chemical residues.

PubMed

Bietlot, Henri P; Kolakowski, Beata

2012-08-01

The Canadian Food Inspection Agency (CFIA) uses 'Ranked Risk Assessment' (RRA) to prioritize chemical hazards for inclusion in monitoring programmes or method development projects based on their relative risk. The relative risk is calculated for a chemical by scoring toxicity and exposure in the 'risk model scoring system' of the Risk Priority Compound List (RPCL). The relative ranking and the risk management options are maintained and updated in the RPCL. The ranking may be refined by the data generated by the sampling and testing programs. The two principal sampling and testing programmes are the National Chemical Residue Monitoring Program (NCRMP) and the Food Safety Action Plan (FSAP). The NCRMP sampling plans focus on the analysis of federally registered products (dairy, eggs, honey, meat and poultry, fresh and processed fruit and vegetable commodities, and maple syrup) for residues of veterinary drugs, pesticides, environmental contaminants, mycotoxins, and metals. The NCRMP is complemented by the Food Safety Action Plan (FSAP) targeted surveys. These surveys focus on emerging chemical hazards associated with specific foods or geographical regions for which applicable maximum residue limits (MRLs) are not set. The data from the NCRMP and FSAP also influence the risk management (follow-up) options. Follow-up actions vary according to the magnitude of the health risk, all with the objective of preventing any repeat occurrence to minimize consumer exposure to a product representing a potential risk to human health. © Her Majesty the Queen in Right of Canada 2012. Drug Testing and Analysis © 2012 John Wiley & Sons, Ltd.

Quantitative structure activity relationship and risk analysis of some pesticides in the goat milk.

PubMed

Muhammad, Faqir; Awais, Mian Muhammad; Akhtar, Masood; Anwar, Muhammad Irfan

2013-01-04

The detection and quantification of different pesticides in the goat milk samples collected from different localities of Faisalabad, Pakistan was performed by HPLC using solid phase microextraction. The analysis showed that about 50% milk samples were contaminated with pesticides. The mean±SEM levels (ppm) of cyhalothrin, endosulfan, chlorpyrifos and cypermethrin were 0.34±0.007, 0.063±0.002, 0.034±0.002 and 0.092±0.002, respectively; whereas, methyl parathion was not detected in any of the analyzed samples. Quantitative structure activity relationship (QSAR) models were suggested to predict the residues of unknown pesticides in the goat milk using their known physicochemical characteristics including molecular weight (MW), melting point (MP), and log octanol to water partition coefficient (Ko/w) in relation to the characteristics such as pH, % fat, specific gravity and refractive index of goat milk. The analysis revealed good correlation coefficient (R2 = 0.985) for goat QSAR model. The coefficients for Ko/w and refractive index for the studied pesticides were higher in goat milk. This suggests that these are better determinants for pesticide residue prediction in the milk of these animals. Based upon the determined pesticide residues and their provisional tolerable daily intakes, risk analysis was also conducted which showed that daily intake levels of pesticide residues including cyhalothrin, chlorpyrifos and cypermethrin in present study are 2.68, 5.19 and 2.71 times higher, respectively in the goat milk. This intake of pesticide contaminated milk might pose health hazards to humans in this locality.

Quantitative structure activity relationship and risk analysis of some pesticides in the goat milk

PubMed Central

2013-01-01

The detection and quantification of different pesticides in the goat milk samples collected from different localities of Faisalabad, Pakistan was performed by HPLC using solid phase microextraction. The analysis showed that about 50% milk samples were contaminated with pesticides. The mean±SEM levels (ppm) of cyhalothrin, endosulfan, chlorpyrifos and cypermethrin were 0.34±0.007, 0.063±0.002, 0.034±0.002 and 0.092±0.002, respectively; whereas, methyl parathion was not detected in any of the analyzed samples. Quantitative structure activity relationship (QSAR) models were suggested to predict the residues of unknown pesticides in the goat milk using their known physicochemical characteristics including molecular weight (MW), melting point (MP), and log octanol to water partition coefficient (Ko/w) in relation to the characteristics such as pH, % fat, specific gravity and refractive index of goat milk. The analysis revealed good correlation coefficient (R2 = 0.985) for goat QSAR model. The coefficients for Ko/w and refractive index for the studied pesticides were higher in goat milk. This suggests that these are better determinants for pesticide residue prediction in the milk of these animals. Based upon the determined pesticide residues and their provisional tolerable daily intakes, risk analysis was also conducted which showed that daily intake levels of pesticide residues including cyhalothrin, chlorpyrifos and cypermethrin in present study are 2.68, 5.19 and 2.71 times higher, respectively in the goat milk. This intake of pesticide contaminated milk might pose health hazards to humans in this locality. PMID:23369514

Residue levels and risk assessment of pesticides in nuts of China.

PubMed

Liu, Yihua; Shen, Danyu; Li, Shiliang; Ni, Zhanglin; Ding, Ming; Ye, Caifen; Tang, Fubin

2016-02-01

The pesticide residue levels of three nuts (chestnut, walnut, pinenut) collected from seven main producing areas of China were investigated. Twenty-nine pesticides, including organophosphates (OPs), organochlorines (OCs), pyrethroids (PYs) and two fungicides (triadimefon and buprofezin) were analyzed by gas chromatography (GC). Four OPs (acephate, dimethoate, chlorpyrifos and parathion-methyl) were found in 11.4% samples, with the concentrations of 19.0 µg kg(-1) to 74.0 µg kg(-1). Six OCs (DDT, HCH, endosulfan, quintozene, aldrin and dieldrin) were found in 18.2% samples, with the concentrations of 2.0 µg kg(-1) to 65.7 µg kg(-1). Among OCs, p,p-DDE and α-HCH were the dominant isomer for DDT and HCH. Five PYs (fenpropathrin, fenvalerate, cypermethrin, bifenthrin and cyhalothrin) were found in 15.9% samples, with the concentrations of 2.5 µg kg(-1) to 433.0 µg kg(-1). Fenpropathrin was the most frequently detected pesticide. In addition, triadimefon and buprofezin were detected only in two samples. For the tested nuts, 25.0% samples with multiple residues (containing more than two pesticides) were noted, even up to 9.1% samples with five pesticide residues. The residue of 15.9% samples was higher than the maximum residue limits (MRLs) of China. The short-term risks for the tested nuts were below 1.2%, and the highest long-term risk was 12.58%. The cumulative risk (cHI) for the tested pesticides were 8.43% (OPs), 0.42% (OCs), 12.82% (PYs) and 0.15% (fungicides), respectively. The total cHI was 21.82%. There was no significant health risk for consumers via nuts consumption. Copyright © 2015 Elsevier Ltd. All rights reserved.

Measures of precision for dissimilarity-based multivariate analysis of ecological communities.

PubMed

Anderson, Marti J; Santana-Garcon, Julia

2015-01-01

Ecological studies require key decisions regarding the appropriate size and number of sampling units. No methods currently exist to measure precision for multivariate assemblage data when dissimilarity-based analyses are intended to follow. Here, we propose a pseudo multivariate dissimilarity-based standard error (MultSE) as a useful quantity for assessing sample-size adequacy in studies of ecological communities. Based on sums of squared dissimilarities, MultSE measures variability in the position of the centroid in the space of a chosen dissimilarity measure under repeated sampling for a given sample size. We describe a novel double resampling method to quantify uncertainty in MultSE values with increasing sample size. For more complex designs, values of MultSE can be calculated from the pseudo residual mean square of a permanova model, with the double resampling done within appropriate cells in the design. R code functions for implementing these techniques, along with ecological examples, are provided. © 2014 The Authors. Ecology Letters published by John Wiley & Sons Ltd and CNRS.

Determination of quinolone residues in infant and young children powdered milk combining solid-phase extraction and ultra-performance liquid chromatography-tandem mass spectrometry.

PubMed

Herrera-Herrera, Antonio V; Hernández-Borges, Javier; Rodríguez-Delgado, Miguel A; Herrero, Miguel; Cifuentes, Alejandro

2011-10-21

The present work describes a method based on solid-phase extraction (SPE) and ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) for the simultaneous determination of three quinolones (pipemidic acid, oxolinic acid and flumequine) and twelve fluoroquinolones (marbofloxacin, fleroxacin, pefloxacin, levofloxacin, norfloxacin, ciprofloxacin, enrofloxacin, danofloxacin, lomefloxacin, difloxacin, sarafloxacin, and moxifloxacin) in different infant and young children powdered milks. After suitable deproteination of the reconstituted powdered samples, a SPE procedure was developed providing recovery values higher than 84% (RSDs lower than 13%) for all the analytes, with limits of detection between 0.04 and 0.52 μg/kg. UPLC-MS/MS analyses were carried out in less than 10 min. Sixteen infant and young children powdered milk samples of different origin, type and composition bought at Spanish markets were analyzed. Residues of the selected antibiotics were not detected in any of the analyzed samples. Copyright © 2011 Elsevier B.V. All rights reserved.

Variation of transition temperatures and residual resistivity ratio in vapor-grown FeSe

DOE PAGES

Böhmer, A. E.; Taufour, V.; Straszheim, W. E.; ...

2016-07-29

The study of the iron-based superconductor FeSe has blossomed with the availability of high-quality single crystals, obtained through flux/vapor-transport growth techniques below the structural transformation temperature of its tetragonal phase, T≈450°C. Here, we report on the variation of sample morphology and properties due to small modifications in the growth conditions. A considerable variation of the superconducting transition temperature T c, from 8.8 K to 3 K, which cannot be correlated with the sample composition, is observed. Instead, we point out a clear correlation between T c and disorder, as measured by the residual resistivity ratio. Notably, the tetragonal-to-orthorhombic structural transitionmore » is also found to be quite strongly disorder dependent (T s≈72–90K) and linearly correlated with T c.« less

Validation of the LacTek test applied to spiked extracts of tissue samples: determination of performance characteristics.

PubMed

Mitchell, J M; Yee, A J; McNab, W B; Griffiths, M W; McEwen, S A

1999-01-01

LacTek tests are competitive enzyme-linked immunosorbent assays intended for rapid detection of antimicrobial residues in bovine milk. In this study, the LacTek test protocol was modified for use with extracts of bovine tissue to detect beta-lactam, tetracycline, and sulfamethazine residues. Test performance characteristics--precision, accuracy, ruggedness, practicability, and analytical specificity and sensitivity--were investigated. Results suggest that LacTek tests can be easily adapted to detect antimicrobial residues in extracts of lean ground beef. However, positive samples may not contain residues at violative concentrations (i.e., Canadian maximum residue limits), and therefore, additional analysis would be required for final confirmation and quantitation (e.g., chromatography).

Development and application of a population physiologically based pharmacokinetic model for penicillin G in swine and cattle for food safety assessment.

PubMed

Li, Miao; Gehring, Ronette; Riviere, Jim E; Lin, Zhoumeng

2017-09-01

Penicillin G is a widely used antimicrobial in food-producing animals, and one of the most predominant drug residues in animal-derived food products. Due to reduced sensitivity of bacteria to penicillin, extralabel use of penicillin G is common, which may lead to violative residues in edible tissues and cause adverse reactions in consumers. This study aimed to develop a physiologically based pharmacokinetic (PBPK) model to predict drug residues in edible tissues and estimate extended withdrawal intervals for penicillin G in swine and cattle. A flow-limited PBPK model was developed with data from Food Animal Residue Avoidance Databank using Berkeley Madonna. The model predicted observed drug concentrations in edible tissues, including liver, muscle, and kidney for penicillin G both in swine and cattle well, including data not used in model calibration. For extralabel use (5× and 10× label dose) of penicillin G, Monte Carlo sampling technique was applied to predict times needed for tissue concentrations to fall below established tolerances for the 99th percentile of the population. This model provides a useful tool to predict tissue residues of penicillin G in swine and cattle to aid food safety assessment, and also provide a framework for extrapolation to other food animal species. Copyright © 2017 Elsevier Ltd. All rights reserved.

Study of consumer fireworks post-blast residues by ATR-FTIR.

PubMed

Martín-Alberca, Carlos; Zapata, Félix; Carrascosa, Héctor; Ortega-Ojeda, Fernando E; García-Ruiz, Carmen

2016-03-01

Specific analytical procedures are requested for the forensic analysis of pre- and post-blast consumer firework samples, which present significant challenges. Up to date, vibrational spectroscopic techniques such as Fourier transform infrared spectroscopy (FTIR) have not been tested for the analysis of post-blast residues in spite of their interesting strengths for the forensic field. Therefore, this work proposes a simple and fast procedure for the sampling and analysis of consumer firework post-blast residues by a portable FTIR instrument with an Attenuated Total Reflection (ATR) accessory. In addition, the post-blast residues spectra of several consumer fireworks were studied in order to achieve the identification of their original chemical compositions. Hence, this work analysed 22 standard reagents usually employed to make consumer fireworks, or because they are related to their combustion products. Then, 5 different consumer fireworks were exploded, and their residues were sampled with dry cotton swabs and directly analysed by ATR-FTIR. In addition, their pre-blast fuses and charges were also analysed in order to stablish a proper comparison. As a result, the identification of the original chemical compositions of the post-blast samples was obtained. Some of the compounds found were potassium chlorate, barium nitrate, potassium nitrate, potassium perchlorate or charcoal. An additional study involving chemometric tools found that the results might greatly depend on the swab head type used for the sampling, and its sampling efficiency. The proposed procedure could be used as a complementary technique for the analysis of consumer fireworks post-blast residues. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of Residual Chlorine and Turbidity in Drinking Water. Instructor's Manual.

ERIC Educational Resources Information Center

Office of Water Program Operations (EPA), Cincinnati, OH. National Training and Operational Technology Center.

This instructor's guide presents analytical methods for residual chlorine and turbidity. Topics include sample handling, permissable concentration levels, substitution of residual chlorine for bacteriological work, public notification, and the required analytical techniques to determine residual chlorine and turbidity. This publication is intended…

Policy-driven development of cost-effective, risk-based surveillance strategies.

PubMed

Reist, M; Jemmi, T; Stärk, K D C

2012-07-01

Animal health and residue surveillance verifies the good health status of the animal population, thereby supporting international free trade of animals and animal products. However, active surveillance is costly and time-consuming. The development of cost-effective tools for animal health and food hazard surveillance is therefore a priority for decision-makers in the field of veterinary public health. The assumption of this paper is that outcome-based formulation of standards, legislation leaving room for risk-based approaches and close collaboration and a mutual understanding and exchange between scientists and policy makers are essential for cost-effective surveillance. We illustrate this using the following examples: (i) a risk-based sample size calculation for surveys to substantiate freedom from diseases/infection, (ii) a cost-effective national surveillance system for Bluetongue using scenario tree modelling and (iii) a framework for risk-based residue monitoring. Surveys to substantiate freedom from infectious bovine rhinotracheitis and enzootic bovine leucosis between 2002 and 2009 saved over 6 million € by applying a risk-based sample size calculation approach, and by taking into account prior information from repeated surveys. An open, progressive policy making process stimulates research and science to develop risk-based and cost-efficient survey methodologies. Early involvement of policy makers in scientific developments facilitates implementation of new findings and full exploitation of benefits for producers and consumers. Copyright © 2012 Elsevier B.V. All rights reserved.

Fast and selective determination of total protein in milk powder via titration of moving reaction boundary electrophoresis.

PubMed

Guo, Cheng-ye; Wang, Hou-yu; Liu, Xiao-ping; Fan, Liu-yin; Zhang, Lei; Cao, Cheng-xi

2013-05-01

In this paper, moving reaction boundary titration (MRBT) was developed for rapid and accurate quantification of total protein in infant milk powder, from the concept of moving reaction boundary (MRB) electrophoresis. In the method, the MRB was formed by the hydroxide ions and the acidic residues of milk proteins immobilized via cross-linked polyacrylamide gel (PAG), an acid-base indicator was used to denote the boundary motion. As a proof of concept, we chose five brands of infant milk powders to study the feasibility of MRBT method. The calibration curve of MRB velocity versus logarithmic total protein content of infant milk powder sample was established based on the visual signal of MRB motion as a function of logarithmic milk protein content. Weak influence of nonprotein nitrogen (NPN) reagents (e.g., melamine and urea) on MRBT method was observed, due to the fact that MRB was formed with hydroxide ions and the acidic residues of captured milk proteins, rather than the alkaline residues or the NPN reagents added. The total protein contents in infant milk powder samples detected via the MRBT method were in good agreement with those achieved by the classic Kjeldahl method. In addition, the developed method had much faster measuring speed compared with the Kjeldahl method. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Pesticide Residues in Commercial Lettuce, Onion, and Potato Samples From Bolivia-A Threat to Public Health?

PubMed

Skovgaard, Marlene; Encinas, Susana Renjel; Jensen, Olaf Chresten; Andersen, Jens Hinge; Condarco, Guido; Jørs, Erik

2017-01-01

Bolivia does not have a surveillance program for pesticide residues in food. The few published studies have suggested that pesticide contamination in food may present a public health problem. Data are lacking for all foods except tomatoes and breast milk. In this study 10 potato, 10 onion, and 10 lettuce samples from La Paz were sampled on August 15, 2015 at a local market and screened for 283 pesticides. Residues of cypermethrin, chlorpyrifos, difenoconazol, or/and λ-cyhalothrin were detected in 50% of the lettuce samples, whereas no pesticides were found in potatoes and onions. In 20% of the lettuce samples, the measurements were above the maximum residue limits, and 2 or 3 pesticides were identified simultaneously. Washing almost halved the pesticide levels, but still 20% of the samples showed measurements above the limits. No samples contained concentrations of pesticides which alone or together would lead to exposures that exceeded the acceptable daily intake or the acute reference dose. To protect consumers from pesticide poisonings and chronic effects, the development of measures for prevention, control, and monitoring of food contamination by pesticides in Bolivia is suggested.

Pesticide Residues in Commercial Lettuce, Onion, and Potato Samples From Bolivia—A Threat to Public Health?

PubMed Central

Skovgaard, Marlene; Renjel Encinas, Susana; Jensen, Olaf Chresten; Andersen, Jens Hinge; Condarco, Guido; Jørs, Erik

2017-01-01

Bolivia does not have a surveillance program for pesticide residues in food. The few published studies have suggested that pesticide contamination in food may present a public health problem. Data are lacking for all foods except tomatoes and breast milk. In this study 10 potato, 10 onion, and 10 lettuce samples from La Paz were sampled on August 15, 2015 at a local market and screened for 283 pesticides. Residues of cypermethrin, chlorpyrifos, difenoconazol, or/and λ-cyhalothrin were detected in 50% of the lettuce samples, whereas no pesticides were found in potatoes and onions. In 20% of the lettuce samples, the measurements were above the maximum residue limits, and 2 or 3 pesticides were identified simultaneously. Washing almost halved the pesticide levels, but still 20% of the samples showed measurements above the limits. No samples contained concentrations of pesticides which alone or together would lead to exposures that exceeded the acceptable daily intake or the acute reference dose. To protect consumers from pesticide poisonings and chronic effects, the development of measures for prevention, control, and monitoring of food contamination by pesticides in Bolivia is suggested. PMID:28469451

Organophosphorus pesticide residues in vegetables from farms, markets, and a supermarket around Kwan Phayao Lake of Northern Thailand.

PubMed

Sapbamrer, Ratana; Hongsibsong, Surat

2014-07-01

This study investigated organophosphorus (OP) residues in vegetables from 27 farms, 106 markets, and 1 supermarket around Kwan Phayao Lake, Northern Thailand, between August and September 2013. Types of vegetables sampled were all vegetables cultivated or sold around the study site. The most common OP pesticides detected in farm samples were chlorpyrifos (50 %), malathion (31.8 %), monocrotophos (31.8 %), diazinon (13.6 %), omethoate (13.6 %), and dicrotophos (9.1 %). The most common OP pesticides detected in market samples were chlorpyrifos (33.9 %), diazinon (18.6 %), parathion-methyl (3.4 %), profenofos (3.4 %), primiphos-ethyl (3.4 %), and fenitrothion (1.7 %). The OP pesticides detected in supermarket samples were chlorpyrifos (33.3 %), and diazinon (66.7 %). Among the compounds detected, chlorpyrifos was detected in most of the vegetable samples from all sources. The highest chlorpyrifos level in farm samples were found in lemon balm (2.423 mg/kg) followed by Vietnamese coriander (0.835 mg/kg), and cowpea (0.027 mg/kg). The highest level in markets samples were found in garlic (7.785 mg/kg) followed by Chinese cabbage (2.864 mg/kg) and Vietnamese coriander (1.308 mg/kg). Residues from supermarket samples were found only in parsley (0.027 mg/kg). The findings showed that 16 samples (59.3 %) from farms and 14 samples (13.2 %) from markets contained OP residues at or above the maximum residue limits established by the European Union. It is concluded that awareness, safety education, and strict regulation of pesticide use are necessary.

Differentiation between consumption and external contamination when testing for cocaine and cannabis in hair samples.

PubMed

Tsanaclis, Lolita; Nutt, James; Bagley, Kim; Bevan, Sian; Wicks, John

2014-06-01

It is possible for hair to be externally contaminated by drugs like cannabis or cocaine, which are smoked or snorted. Three steps are commonly employed to minimize the chance of external contamination causing misinterpretation of the results of a hair test. The first consists of decontamination of hair samples by washing the hair before analysis, the second is the use of cut-off levels, and the third is the detection of both the parent drugs and appropriate levels of their metabolite(s) in the hair sample. We propose an additional step for the assessment of drug use using hair samples combined with decontamination data. Hair samples from 186 drug users were analyzed along with their wash residues by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The results of the hair analysis of the 140 samples for cocaine showed that 85.5% (N=89) of the samples passed 'cocaine use' criteria for metabolites ratios and 12.5% (N=13) for wash residue criteria (<10% of cocaine in the wash residue) leading to conclusive interpretation. Only two cases (1.9%) had an uncertain conclusion of drug consumption because cocaine levels in the wash residue were >10% of the levels in the hair. The results of the cannabis set of samples (N=46) were not as clear-cut, as a comparatively large number of samples (15.2%) had relatively high levels of THC in the wash residues. To use this approach, it is important that laboratories testing drugs in hair samples can demonstrate that the method utilized does not generate significant levels of the cocaine metabolites. Copyright © 2014 John Wiley & Sons, Ltd.

Determination of imidocarb residues in bovine and ovine liver and milk by immunobiosensor.

PubMed

Traynor, I M; Thompson, C S; Armstrong, L; Fodey, T; Danaher, M; Jordan, K; Kennedy, D G; Crooks, S R H

2013-01-01

Imidocarb (IMD) is a veterinary drug that has been used for more than 30 years to treat and prevent parasitic diseases. Pharmacokinetic studies have shown that substantial levels of IMD residues are retained in the edible tissues and milk of cattle and sheep for up to 6 months after administration. This has led to concern regarding the potential adverse effects posed through human consumption of edible tissue or milk from treated animals if the recommended withdrawal periods for the drug are not properly implemented. While MRLs have been established by the European Union, it is important that analytical methods are available to monitor food samples for potentially violative levels of IMD residues. A qualitative biosensor-based immunoassay was developed to allow the detection of IMD at less than the European Union MRLs of 50 μg kg(-1) for milk and 2 mg kg(-1) for bovine and ovine liver. Validation of the developed methods provided a detection capability of <25 μg kg(-1) in milk and <0.75 mg kg(-1) in liver. A comparison study was undertaken, with IMD incurred milk and ovine liver samples analysed by the newly developed procedures and results compared with those obtained by LC-MS/MS. The newly developed screening method was applied to both incurred milk and liver samples. This faster, cheaper and reliable screening method has potential use in sample analysis to ensure compliance with legislative requirements.

Phenotypic and genetic structure of traits delineating personality disorder.

PubMed

Livesley, W J; Jang, K L; Vernon, P A

1998-10-01

The evidence suggests that personality traits are hierarchically organized with more specific or lower-order traits combining to form more generalized higher-order traits. Agreement exists across studies regarding the lower-order traits that delineate personality disorder but not the higher-order traits. This study seeks to identify the higher-order structure of personality disorder by examining the phenotypic and genetic structures underlying lower-order traits. Eighteen lower-order traits were assessed using the Dimensional Assessment of Personality Disorder-Basic Questionnaire in samples of 656 personality disordered patients, 939 general population subjects, and a volunteer sample of 686 twin pairs. Principal components analysis yielded 4 components, labeled Emotional Dysregulation, Dissocial Behavior, Inhibitedness, and Compulsivity, that were similar across the 3 samples. Multivariate genetic analyses also yielded 4 genetic and environmental factors that were remarkably similar to the phenotypic factors. Analysis of the residual heritability of the lower-order traits when the effects of the higher-order factors were removed revealed a substantial residual heritable component for 12 of the 18 traits. The results support the following conclusions. First, the stable structure of traits across clinical and nonclinical samples is consistent with dimensional representations of personality disorders. Second, the higher-order traits of personality disorder strongly resemble dimensions of normal personality. This implies that a dimensional classification should be compatible with normative personality. Third, the residual heritability of the lower-order traits suggests that the personality phenotypes are based on a large number of specific genetic components.

Global variations in abyssal peridotite compositions

NASA Astrophysics Data System (ADS)

Warren, Jessica M.

2016-04-01

Abyssal peridotites are ultramafic rocks collected from mid-ocean ridges that are the residues of adiabatic decompression melting. Their compositions provide information on the degree of melting and melt-rock interaction involved in the formation of oceanic lithosphere, as well as providing constraints on pre-existing mantle heterogeneities. This review presents a compilation of abyssal peridotite geochemical data (modes, mineral major elements, and clinopyroxene trace elements) for > 1200 samples from 53 localities on 6 major ridge systems. On the basis of composition and petrography, peridotites are classified into one of five lithological groups: (1) residual peridotite, (2) dunite, (3) gabbro-veined and/or plagioclase-bearing peridotite, (4) pyroxenite-veined peridotite, and (5) other types of melt-added peridotite. Almost a third of abyssal peridotites are veined, indicating that the oceanic lithospheric mantle is more fertile, on average, than estimates based on residual peridotites alone imply. All veins appear to have formed recently during melt transport beneath the ridge, though some pyroxenites may be derived from melting of recycled oceanic crust. A limited number of samples are available at intermediate and fast spreading rates, with samples from the East Pacific Rise indicating high degrees of melting. At slow and ultra-slow spreading rates, residual abyssal peridotites define a large (0-15% modal clinopyroxene and spinel Cr# = 0.1-0.6) compositional range. These variations do not match the prediction for how degree of melting should vary as a function of spreading rate. Instead, the compositional ranges of residual peridotites are derived from a combination of melting, melt-rock interaction and pre-existing compositional variability, where melt-rock interaction is used here as a general term to refer to the wide range of processes that can occur during melt transport in the mantle. Globally, 10% of abyssal peridotites are refractory (0% clinopyroxene, spinel Cr# > 0.5, bulk Al2O3 < 1 wt.%) and some ridge sections are dominated by harzburgites while lacking a significant basaltic crust. Abyssal ultramafic samples thus indicate that the mantle is multi-component, probably consisting of at least three components (lherzolite, harzburgite, and pyroxenite). Overall, the large compositional range among residual and melt-added peridotites implies that the oceanic lithospheric mantle is heterogeneous, which will lead to the generation of further heterogeneities upon subduction back into the mantle.

Examining Plasmodium falciparum and P. vivax clearance subsequent to antimalarial drug treatment in the Myanmar-China border area based on quantitative real-time polymerase chain reaction.

PubMed

Lo, Eugenia; Nguyen, Jennifer; Oo, Winny; Hemming-Schroeder, Elizabeth; Zhou, Guofa; Yang, Zhaoqing; Cui, Liwang; Yan, Guiyun

2016-04-16

Recent emergence of artemisinin-resistant P. falciparum has posed a serious hindrance to the elimination of malaria in the Greater Mekong Subregion. Parasite clearance time, a measure of change in peripheral parasitaemia in a sequence of samples taken after treatment, can be used to reflect the susceptibility of parasites or the efficiency of antimalarials. The association of genetic polymorphisms and artemisinin resistance has been documented. This study aims to examine clearance time of P. falciparum and P. vivax parasitemia as well as putative gene mutations associated with residual or recurred parasitemia in Myanmar. A total of 63 P. falciparum and 130 P. vivax samples collected from two internally-displaced populations and one surrounding village were examined for parasitemia changes. At least four samples were taken from each patient, at the first day of diagnosis up to 3 months following the initial treatment. The amount of parasite gene copy number was estimated using quantitative real-time PCR based on a species-specific region of the 18S rRNA gene. For samples that showed residual or recurred parasitemia after treatment, microsatellites were used to identify the 'post-treatment' parasite genotype and compared such with the 'pre-treatment' genotype. Mutations in genes pfcrt, pfmdr1, pfatp6, pfmrp1 and pfK13 that are potentially associated with ACT resistance were examined to identify if mutation is a factor for residual or persistent parasitemia. Over 30% of the P. falciprium infections showed delayed clearance of parasitemia after 2-3 days of treatment and 9.5% showed recurred parasitemia. Mutations in codon 876 of the pfmrp1 corroborated significance association with slow clearance time. However, no association was observed in the variation in pfmdr1 gene copy number as well as mutations of various codonsinpfatp6, pfcrt, and pfK13 with clearance time. For P. vivax, over 95% of the infections indicated cleared parasitemia at days 2-3 of treatment. Four samples were found to be re-infected with new parasite strains based on microsatellite genotypes after initial treatment. The appearance of P.falciparum infected samples showing delayed clearance or recurred parasitemia after treatment raises concerns on current treatment and ACT drug resistance.

Determination of Residual Chlorine and Turbidity in Drinking Water. Student Manual.

ERIC Educational Resources Information Center

Office of Water Program Operations (EPA), Cincinnati, OH. National Training and Operational Technology Center.

This student's manual covers analytical methods for residual chlorine and turbidity. Topics include sample handling, permissable concentration levels, substitution of residual chlorine for bacteriological work, public notification, and the required analytical techniques to determine residual chlorine and turbidity. The publication is intended for…

Residues and potential ecological risks of veterinary antibiotics in manures and composts associated with protected vegetable farming.

PubMed

Zhang, Haibo; Luo, Yongming; Wu, Longhua; Huang, Yujuan; Christie, Peter

2015-04-01

Veterinary antibiotics (VAs) are emerging contaminants and enter into soil principally by agricultural application of organic fertilizer. A total of 33 solid animal manures and 17 compost samples from protected vegetable farms in nine areas of China were analyzed for the antibiotic classes of tetracyclines, fluoroquinolones, sulfonamides, and macrolides (17 substances in total). Oxytetracycline was found as a dominant compound in the samples, and its highest concentration reached 416.8 mg kg(-1) in a chicken manure sample from Shouguang, Shandong Province. Among the samples, animal manures (especially pig manure) contained higher VA residues than composts. However, fluoroquinolones exhibited higher persistence in the compost samples than other antibiotic classes. This is particularly the case in the rice husk compost, which contained the highest level of ofloxacin and ciprofloxacin (1334.5 and 1717.4 μg kg(-1) on average, respectively). The veterinary antibiotic profile in the risk husk compost had a good relationship with that in the corresponding manures. The refined commercial compost had the lowest VA residues among the compost samples in general. This implied that composting process might be important to reduce the antibiotic residue. High residue of antibiotics in soil was assumed to be a hazard to ecosystem. This is especially noticeable under current application rates (150 t ha(-1) a(-1)) in protected vegetable farming because over half of the samples exhibited a risk quotient (RQ) >1 for one or more antibiotics.

Rapid ion-pair liquid chromatographic method for the determination of fenbendazole marker residue in fermented dairy products.

PubMed

Vousdouka, Venetia I; Papapanagiotou, Elias P; Angelidis, Apostolos S; Fletouris, Dimitrios J

2017-04-15

A simple, rapid and sensitive liquid chromatographic method that allows for the quantitative determination of fenbendazole residues in fermented dairy products is described. Samples were extracted with a mixture of acetonitrile-phosphoric acid and the extracts were defatted with hexane to be further partitioned into ethyl acetate. The organic layer was evaporated to dryness and the residue was reconstituted in mobile phase. Separation of fenbendazole and its sulphoxide, sulphone, and p-hydroxylated metabolites was carried out isocratically with a mobile phase containing both positively and negatively charged pairing ions. Overall recoveries ranged from 79.8 to 88.8%, while precision data, based on within and between days variations, suggested an overall relative standard deviation of 6.3-11.0%. The detection and quantification limits were lower than 9 and 21μg/kg, respectively. The method has been successfully applied to quantitate fenbendazole residues in Feta cheese and yoghurt made from spiked and incurred ovine milk. Copyright © 2016 Elsevier Ltd. All rights reserved.

Determination of diacylhydrazines-type insect growth regulator JS-118 residues in cabbage and soil by high performance liquid chromatography with DAD detection.

PubMed

Hu, J-Y; Deng, Z-B; Qin, D-M

2009-12-01

JS-118 is a diacylhydrazines-type insect growth regulator used extensively in China now. An analytical method for residues determination of JS-118 in cabbage and soil samples by high performance liquid chromatography with DAD detection was established and optimized. Primary secondary amine solid phase extraction cartridge was used for sample preparation. Mean recoveries for the analyte ranged from 96.6% to 107.0% with CV value less than 4.7%. The limit of quantification is 0.01 mg/kg. Direct confirmation of JS-118 residues in samples was realized by high performance liquid chromatography-mass spectrometry. The proposed method is simple, rapid and reliable to perform and could be utilized for monitoring of pesticides residues.

Pesticides and their metabolites in wells of Suffolk County, New York, 1998

USGS Publications Warehouse

Phillips, Patrick J.; Eckhardt, D.A.; Terracciano, S.A.; Rosenmann, Larry

1999-01-01

Five insecticide residues and 20 herbicide residues were detected in water samples collected from 50 shallow wells screened in the surficial sand and gravel aquifer in Suffolk County, Long Island in areas with known or suspected residues. Laboratory analytical methods with extremely low detection limits - from 0.001 to 0.2 ?g/L (micrograms per liter) - were used to analyze the samples for 60 pesticide residues. Forty-four of the samples contained at least one pesticide residue, and some samples contained as many as 11 different pesticides or pesticide metabolites. Only four water- quality standards were exceeded in the samples collected in this study. Dieldrin exceeded the New York State Class GA standard (0.004 ?g/L) in samples from eight wells. The Federal and New York State Maximum Contaminant Level for simazine (4 ?g/L) was exceeded in samples from two wells, and the State Class GA standard for simazine (0.5 ?g/L) was exceeded in samples from six wells. Federal water-quality standards have not been established for many of the compounds detected in this study, including herbicide metabolites. Maximum concentrations of four herbicide metabolites -metolachlor ESA (ethanesulfonic acid), metolachlor OA (oxanilic acid), and the alachlor metabolites alachlor ESA and alachlor OA -exceeded 20 ?g/L. The maximum concentration of one herbicide (tebuthiuron) exceeded 10 ?g/L, and the maximum concentration of three herbicides (simazine, metolachlor, and atrazine) and one herbicide metabolite (deisopropylatrazine) ranged from 1 to 10 ?g/L. The herbicide metolachlor, which is used on potato fields in Suffolk County, and its metabolites (metolachlor ESA and metolachlor OA) were most frequently detected in samples from agricultural areas. The herbicides simazine and tebuthiuron, which were used in utility rights-of-way, and the simazine metabolite deisopropylatrazine were detected at concentrations greater than 0.05 ?g/L most frequently in samples from residential and mixed land-use areas. The results of this investigation are not necessarily representative of conditions throughout the remainder of Long Island, because these samples were collected in areas of known or suspected residues.

Annotating Protein Functional Residues by Coupling High-Throughput Fitness Profile and Homologous-Structure Analysis

PubMed Central

Du, Yushen; Wu, Nicholas C.; Jiang, Lin; Zhang, Tianhao; Gong, Danyang; Shu, Sara; Wu, Ting-Ting

2016-01-01

ABSTRACT Identification and annotation of functional residues are fundamental questions in protein sequence analysis. Sequence and structure conservation provides valuable information to tackle these questions. It is, however, limited by the incomplete sampling of sequence space in natural evolution. Moreover, proteins often have multiple functions, with overlapping sequences that present challenges to accurate annotation of the exact functions of individual residues by conservation-based methods. Using the influenza A virus PB1 protein as an example, we developed a method to systematically identify and annotate functional residues. We used saturation mutagenesis and high-throughput sequencing to measure the replication capacity of single nucleotide mutations across the entire PB1 protein. After predicting protein stability upon mutations, we identified functional PB1 residues that are essential for viral replication. To further annotate the functional residues important to the canonical or noncanonical functions of viral RNA-dependent RNA polymerase (vRdRp), we performed a homologous-structure analysis with 16 different vRdRp structures. We achieved high sensitivity in annotating the known canonical polymerase functional residues. Moreover, we identified a cluster of noncanonical functional residues located in the loop region of the PB1 β-ribbon. We further demonstrated that these residues were important for PB1 protein nuclear import through the interaction with Ran-binding protein 5. In summary, we developed a systematic and sensitive method to identify and annotate functional residues that are not restrained by sequence conservation. Importantly, this method is generally applicable to other proteins about which homologous-structure information is available. PMID:27803181

Comparison of sample preparation methods combined with fast gas chromatography-mass spectrometry for ultratrace analysis of pesticide residues in baby food.

PubMed

Hercegová, Andrea; Dömötörová, Milena; Kruzlicová, Dása; Matisová, Eva

2006-05-01

Four sample preparation techniques were compared for the ultratrace analysis of pesticide residues in baby food: (a) modified Schenck's method based on ACN extraction with SPE cleaning; (b) quick, easy, cheap, effective, rugged, and safe (QuEChERS) method based on ACN extraction and dispersive SPE; (c) modified QuEChERS method which utilizes column-based SPE instead of dispersive SPE; and (d) matrix solid phase dispersion (MSPD). The methods were combined with fast gas chromatographic-mass spectrometric analysis. The effectiveness of clean-up of the final extract was determined by comparison of the chromatograms obtained. Time consumption, laboriousness, demands on glassware and working place, and consumption of chemicals, especially solvents, increase in the following order QuEChERS < modified QuEChERS < MSPD < modified Schenck's method. All methods offer satisfactory analytical characteristics at the concentration levels of 5, 10, and 100 microg/kg in terms of recoveries and repeatability. Recoveries obtained for the modified QuEChERS method were lower than for the original QuEChERS. In general the best LOQs were obtained for the modified Schenck's method. Modified QuEChERS method provides 21-72% better LOQs than the original method.

Pesticide residues in leafy vegetables, stalk and stem vegetables from South Korea: a long-term study on safety and health risk assessment.

PubMed

Park, Duck Woong; Kim, Kwang Gon; Choi, Eun Ah; Kang, Gyeong Ri; Kim, Tae Sun; Yang, Yong Shik; Moon, Su Jin; Ha, Dong Ryong; Kim, Eun Sun; Cho, Bae Sik

2016-01-01

South Korea has a unique food culture. South Koreans enjoy wrapping meat and eating or making kimchi (traditionally fermented Korean food) and eating using raw leafy vegetables, stalk and stem vegetables. Therefore, there is a high chance of being exposed to pesticide residues of vegetables. The objective of this study was to investigate pesticide residues in leafy vegetables, stalk and stem vegetables from South Korea. A total of 8496 samples were mainly collected from Gwangju and Jeonnam area (the largest production region of leafy vegetables, stalk and stem vegetables) in South Korea from 2010 to 2014. A total of 230 pesticides were used for multi-residue analysis of pesticides. Among 8496 samples, 61 different pesticides (1029 times) were detected in 890 samples, of which 118 samples (1.4%) exceeded the Korea maximum residue limits (MRLs). Samples exceeding the MRLs were mostly found in leafy vegetables (brassica lee ssp. namai, leafy lettuce, spinach, perilla leaves, crown daisy, marsh mallow, aster scaber, pimpinella brachycarpa) and Chinese chive. Procymidone, dimethomorph and azoxystrobin were the most frequently found pesticides. A risk assessment of pesticides exceeding the MRLs was evaluated by calculating the estimated daily intake (EDI) and the acceptable daily intake (ADI). The ratio of EDI to ADI was 0.003-30.4%.

Decontamination of chlorantraniliprole residues on cabbage and cauliflower through household processing methods.

PubMed

Kar, Abhijit; Mandal, Kousik; Singh, Balwinder

2012-04-01

A supervised field trial was conducted to study the residues of chlorantraniliprole on cabbage and cauliflower. Three applications of chlorantraniliprole at 10 days interval were made @ 9.25 and 18.50 g a.i. ha(-1). The samples of marketable size heads and curds of cabbage and cauliflower were collected at 0 and 1 day after the last application. QuEChERS sample preparation was used for the determination of chlorantraniliprole residues on cabbage heads and cauliflower curds. The residues of chlorantraniliprole were quantified by high performance liquid chromatography (HPLC) with photo diode array (PDA) detector and confirmed by high performance thin layer chromatography (HPTLC). Washing of cabbage and cauliflower with tap water removed about 17%-40% of chlorantraniliprole residues. However, boiling removed 100% of chlorantraniliprole residues on cabbage and cauliflower in both the cases.

Pesticide residues in raspberries (Rubus idaeus L.) and dietary risk assessment.

PubMed

Łozowicka, B; Kaczyński, P; Jankowska, M; Rutkowska, E; Hrynko, I

2012-01-01

The aim of this study was to evaluate the residues of 140 pesticides in raspberries from north-eastern Poland (2005-2010). Gas chromatography with electron capture detector (GC-ECD) and nitrogen phosphorous detector (GC-NPD) was used. Among the 128 samples, 66 (51.6%) were found to detect residues: 14.1% contained one pesticide and around 38% multiple pesticide residues. The most frequently detected were pyrimethanil residues (36.0%). Twenty-seven (21.1%) raspberry samples exceeded the maximum residue limits. The estimated daily intakes ranged from 0.003% to 3.183% of the acceptable daily intake (ADI) for adults 0.008% and 9.7% for toddlers, respectively. The most critical case is procymidone, the acute risk was 180.9% of acute reference dose (ARfD) for toddlers and for adults (83% of ARfD) which is high.

Trace elements by instrumental neutron activation analysis for pollution monitoring

NASA Technical Reports Server (NTRS)

Sheibley, D. W.

1975-01-01

Methods and technology were developed to analyze 1000 samples/yr of coal and other pollution-related samples. The complete trace element analysis of 20-24 samples/wk averaged 3-3.5 man-hours/sample. The computerized data reduction scheme could identify and report data on as many as 56 elements. In addition to coal, samples of fly ash, bottom ash, crude oil, fuel oil, residual oil, gasoline, jet fuel, kerosene, filtered air particulates, ore, stack scrubber water, clam tissue, crab shells, river sediment and water, and corn were analyzed. Precision of the method was plus or minus 25% based on all elements reported in coal and other sample matrices. Overall accuracy was estimated at 50%.

Assessment of Residual Stresses in 3013 Inner and Outer Containers and Teardrop Samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stroud, Mary Ann; Prime, Michael Bruce; Veirs, Douglas Kirk

2015-12-08

This report is an assessment performed by LANL that examines packaging for plutonium-bearing materials and the resilience of its design. This report discusses residual stresses in the 3013 outer, the SRS/Hanford and RFETS/LLNL inner containers, and teardrop samples used in studies to assess the potential for SCC in 3013 containers. Residual tensile stresses in the heat affected zones of the closure welds are of particular concern.

Determination of organophosphorus pesticides and their major degradation product residues in food samples by HPLC-UV.

PubMed

Peng, Guilong; He, Qiang; Lu, Ying; Mmereki, Daniel; Zhong, Zhihui

2016-10-01

A simple method based on dispersive solid-phase extraction (DSPE) and dispersive liquid-liquid microextraction method based on solidification of floating organic droplets (DLLME-SFO) was developed for the extraction of chlorpyrifos (CP), chlorpyrifos-methyl (CPM), and their main degradation product 3,5,6-trichloro-2-pyridinol (TCP) in tomato and cucumber samples. The determination was carried out by high performance liquid chromatography with ultraviolet detection (HPLC-UV). In the DSPE-DLLME-SFO, the analytes were first extracted with acetone. The clean-up of the extract by DSPE was carried out by directly adding activated carbon sorbent into the extract solution, followed by shaking and filtration. Under the optimum conditions, the proposed method was sensitive and showed a good linearity within a range of 2-500 ng/g, with the correlation coefficients (r) varying from 0.9991 to 0.9996. The enrichment factors ranged from 127 to 138. The limit of detections (LODs) were in the range of 0.12-0.68 ng/g, and the relative standard deviations (RSDs) for 50 ng/g of each analytes in tomato samples were in the range of 3.25-6.26 % (n = 5). The proposed method was successfully applied for the extraction and determination of the mentioned analytes residues in tomato and cucumber samples, and satisfactory results were obtained.

Comparison of pulse glow discharge-ion mobility spectrometry and liquid chromatography with tandem mass spectrometry based on multiplug filtration cleanup for the analysis of tricaine mesylate residues in fish and water.

PubMed

Zou, Nan; Chen, Ronghua; Qin, Yuhong; Song, Shuangyu; Tang, Xinglin; Pan, Canping

2016-09-01

Analytical methods based on multiplug filtration cleanup coupled with pulse glow discharge-ion mobility spectrometry and liquid chromatography tandem mass spectrometry were developed for the analysis of tricaine mesylate residue in fish and fish-raising water samples. A silica fiber holder and an appropriate new interface were designed to make the direct introduction of the fiber into the pulse glow discharge-ion mobility spectrometry introduction mechanism. The multiplug filtration cleanup method with adsorption mixtures was optimized for the determination of tricaine mesylate in fish samples. Good linear relationships were obtained by the two methods. For fish samples, limits of detection were 6 and 0.6 μg/kg by ion mobility spectrometry and liquid chromatography with tandem mass spectrometry, respectively. The matrix effect of the established liquid chromatography tandem mass spectrometry method was negligible for fish samples but that of the ion mobility spectrometry method was not. The two methods were compared. The ion mobility spectrometry system could be used a rapid screening tool on site with the advantage of rapidity, simplicity, and portability, and the liquid chromatography tandem mass spectrometry system could be used for validation in laboratory conditions with the advantage of lower limit of detection, stability, and precision. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sol-gel-graphene-based fabric-phase sorptive extraction for cow and human breast milk sample cleanup for screening bisphenol A and residual dental restorative material before analysis by HPLC with diode array detection.

PubMed

Samanidou, Victoria; Filippou, Olga; Marinou, Eirini; Kabir, Abuzar; Furton, Kenneth G

2017-06-01

Fabric-phase sorptive extraction has already been recognized as a simple and green alternative to the conventional sorbent-based sorptive microextraction techniques, using hybrid organic-inorganic sorbent coatings chemically bonded to a flexible fabric surface. Herein, we have investigated the synergistic combination of the advanced material properties offered by sol-gel graphene sorbent and the simplicity of Fabric phase sorptive extraction approach in selectively extracting bisphenol A and residual monomers including bisphenol A glycerolatedimethacrylate, urethane dimethacrylate, and triethylene glycol dimethacrylate derived dental restorative materials from cow and human breast milk samples. Different coatings were evaluated. Final method development employed sol-gel graphene coated media. The main experimental parameters influencing extraction of the compounds, such as sorbent chemistry used, sample loading conditions, elution solvent, sorption stirring time, elution time, impact of protein precipitation, amount of sample, and matrix effect, were investigated and optimized. Absolute recovery values from standard solutions were 50% for bisphenol A, 78% for T triethylene glycol dimethacrylate, 110% for urethane dimethacrylate, and 103% for bisphenol A glycerolatedimethacrylate, while respective absolute recovery values from milk were 30, 52, 104, and 42%. Method validation was performed according to European Decision 657/2002/EC in terms of selectivity, sensitivity, linearity, accuracy, and precision. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Class-conditional feature modeling for ignitable liquid classification with substantial substrate contribution in fire debris analysis.

PubMed

Lopatka, Martin; Sigman, Michael E; Sjerps, Marjan J; Williams, Mary R; Vivó-Truyols, Gabriel

2015-07-01

Forensic chemical analysis of fire debris addresses the question of whether ignitable liquid residue is present in a sample and, if so, what type. Evidence evaluation regarding this question is complicated by interference from pyrolysis products of the substrate materials present in a fire. A method is developed to derive a set of class-conditional features for the evaluation of such complex samples. The use of a forensic reference collection allows characterization of the variation in complex mixtures of substrate materials and ignitable liquids even when the dominant feature is not specific to an ignitable liquid. Making use of a novel method for data imputation under complex mixing conditions, a distribution is modeled for the variation between pairs of samples containing similar ignitable liquid residues. Examining the covariance of variables within the different classes allows different weights to be placed on features more important in discerning the presence of a particular ignitable liquid residue. Performance of the method is evaluated using a database of total ion spectrum (TIS) measurements of ignitable liquid and fire debris samples. These measurements include 119 nominal masses measured by GC-MS and averaged across a chromatographic profile. Ignitable liquids are labeled using the American Society for Testing and Materials (ASTM) E1618 standard class definitions. Statistical analysis is performed in the class-conditional feature space wherein new forensic traces are represented based on their likeness to known samples contained in a forensic reference collection. The demonstrated method uses forensic reference data as the basis of probabilistic statements concerning the likelihood of the obtained analytical results given the presence of ignitable liquid residue of each of the ASTM classes (including a substrate only class). When prior probabilities of these classes can be assumed, these likelihoods can be connected to class probabilities. In order to compare the performance of this method to previous work, a uniform prior was assumed, resulting in an 81% accuracy for an independent test of 129 real burn samples. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

Screening of pesticide residues in honeybee wax comb by LC-ESI-MS/MS. A pilot study.

PubMed

Herrera López, Sonia; Lozano, Ana; Sosa, Alexis; Hernando, M Dolores; Fernández-Alba, Amadeo R

2016-11-01

A developed multi-residue method using microflow-LC-ESI-QqQ-MS provided a wide-scope analysis for medium-polar and polar pesticide residues (120 compounds including breakdown products). Honeybee wax comb samples were extracted using a generic QuEChERS based procedure. Acceptable recoveries at concentration levels of 5 and 50 μg kg(-1) were within the 70-120% range with an associated precision RSD <20%. The LOQ values were mostly 5 μg kg(-1) for almost all pesticides. Aprox. 31 of 120 LC-amenable pesticides tested (25.8%) were detected in a pilot study of 60 samples. Pesticide residues detected using the proposed method were: the breakdown products of amitraz, DMPF and DMF, an acaricide used for Varroa mite control, with a range of concentration from 5 to 464 μg kg(-1) (sum of DMPF + DMF), organophosphate insecticides from 1 to 464 μg kg(-1), acaricides at concentrations > 9 μg kg(-1); fungicides at concentrations ranging from 1 to 23 μg kg(-1.) The number of positive detections due to herbicides was lower as expected and at a lower level of concentration, from 1 to 5.9 μg kg(-1). Copyright © 2016 Elsevier Ltd. All rights reserved.

Studies of pesticide residues in tomatoes and cucumbers from Kazakhstan and the associated health risks.

PubMed

Lozowicka, Bozena; Abzeitova, Elmira; Sagitov, Abai; Kaczynski, Piotr; Toleubayev, Kazbek; Li, Alina

2015-10-01

The aim of the present study was to assess the level of pesticide residues in vegetables in the Almaty Region of Kazakhstan and to determine the potential health risks associated with the exposures to these pesticides. A total of 82 samples of cucumbers and tomatoes from top agro-based market and greenhouses were analysed using a gas chromatography-micro electron capture detector/nitrogen-phosphorous detector (GC-μECD/NPD), a multiresidue method to analyse 184 different pesticide types. The results indicated that more than half of samples (59 %) contained 29 pesticides, in which 10 are not registered in Kazakhstan, ranging from 0.01 to 0.88 mg kg(-1), and 28 % contained pesticide residues above maximum residue levels (MRLs). The estimated daily intakes (EDIs) ranged from 0.01 % of the acceptable daily intake (ADI) for pyrimethanil to 12.05 % of the ADI for lambda-cyhalothrin. The most critical commodity is triazophos and flusilazole in tomatoes, contributing 70.8 and 42.5 % to the acute hazard index (aHI). The results provided important information on the current pesticide contamination status of two commonly consumed vegetables and pointed an urgent need to control the use of plant protection products applied, especially potentially persistent pesticides, such as endosulfan and dicofol. These results also show that the detected pesticides may be considered a public health problem.

Analysis of imazaquin in soybeans by solid-phase extraction and high-performance liquid chromatography.

PubMed

Guo, C; Hu, J-Y; Chen, X-Y; Li, J-Z

2008-02-01

An analytical method for the determination imazaquin residues in soybeans was developed. The developed liquid/liquid partition and strong anion exchange solid-phase extraction procedures provide the effective cleanup, removing the greatest number of sample matrix interferences. By optimizing mobile-phase pH water/acetonitrile conditions with phosphoric acid, using a C-18 reverse-phase chromatographic column and employing ultraviolet detection, excellent peak resolution was achieved. The combined cleanup and chromatographic method steps reported herein were sensitive and reliable for determining the imazaquin residues in soybean samples. This method is characterized by recovery >88.4%, precision <6.7% CV, and sensitivity of 0.005 ppm, in agreement with directives for method validation in residue analysis. Imazaquin residues in soybeans were further confirmed by high performance liquid chromatography-mass spectrometry (LC-MS). The proposed method was successfully applied to the analysis of imazaquin residues in soybean samples grown in an experimental field after treatments of imazaquin formulation.

Low-Complexity Lossless and Near-Lossless Data Compression Technique for Multispectral Imagery

NASA Technical Reports Server (NTRS)

Xie, Hua; Klimesh, Matthew A.

2009-01-01

This work extends the lossless data compression technique described in Fast Lossless Compression of Multispectral- Image Data, (NPO-42517) NASA Tech Briefs, Vol. 30, No. 8 (August 2006), page 26. The original technique was extended to include a near-lossless compression option, allowing substantially smaller compressed file sizes when a small amount of distortion can be tolerated. Near-lossless compression is obtained by including a quantization step prior to encoding of prediction residuals. The original technique uses lossless predictive compression and is designed for use on multispectral imagery. A lossless predictive data compression algorithm compresses a digitized signal one sample at a time as follows: First, a sample value is predicted from previously encoded samples. The difference between the actual sample value and the prediction is called the prediction residual. The prediction residual is encoded into the compressed file. The decompressor can form the same predicted sample and can decode the prediction residual from the compressed file, and so can reconstruct the original sample. A lossless predictive compression algorithm can generally be converted to a near-lossless compression algorithm by quantizing the prediction residuals prior to encoding them. In this case, since the reconstructed sample values will not be identical to the original sample values, the encoder must determine the values that will be reconstructed and use these values for predicting later sample values. The technique described here uses this method, starting with the original technique, to allow near-lossless compression. The extension to allow near-lossless compression adds the ability to achieve much more compression when small amounts of distortion are tolerable, while retaining the low complexity and good overall compression effectiveness of the original algorithm.

Greenhouse gas emissions and the interrelation of urban and forest sectors in reclaiming one hectare of land in the Pacific Northwest.

PubMed

Trlica, Andrew; Brown, Sally

2013-07-02

The interrelation between urban areas and land use options for greenhouse gas mitigation was evaluated by assessing the utility of urban residuals for soil reclamation. Long-term impacts on soil C storage for mine lands restored with urban organic residuals were quantified by sampling historic sites reclaimed both conventionally and with residuals-based amendments. Use of amendments resulted in greater C storage compared to conventional practices for all sites sampled, with increases ranging from 14.2 Mg C ha(-1) in a coalmine in WA to 38.4 Mg C ha(-1) for a copper mine in British Columbia. Expressed as Mg C per Mg amendment, effective C increases ranged from 0.03 to 0.31 Mg C per Mg amendment. Results were applied to three alternative land-use scenarios to model the net GHG balance for a site restored to forest or low-density development. The model included construction of 3.9 243 m(2)-homes, typical of urban sprawl. Emissions for home and road construction and use over a 30-year period resulted in net emissions of 1269 Mg CO2. In contrast, conventional reclamation to forestland or reclamation with 100 Mg of residuals resulted in net GHG reductions of -293 and -475 Mg CO2. Construction of an equivalent number of smaller homes in an urban core coupled with restoration of 1 ha with amendments was close to carbon neutral. These results indicate that targeted use of urban residuals for forest reclamation, coupled with high-density development, can increase GHG mitigation across both sectors.

FIELD SAMPLING OF RESIDUAL AVIATION GASOLINE IN SANDY SOIL

EPA Science Inventory

Two complimentary field sampling methods for the determination of residual aviation gasoline content in the contaminated capillary fringe of a fine, uniform, sandy soil were investigated. The first method featured filed extrusion of core barrels into pint size Mason jars, while ...

Shrinkage Behavior of Polystyrene-based Foam Molded Parts Depending on Volatile Matter Content and Other Factors

NASA Astrophysics Data System (ADS)

Ghafafian, Carineh

Polymer foam materials play a large role in the modern world. Expanded polystyrene (EPS) bead foam is a lightweight, low density, and good thermal and acoustic insulating material whose properties make it attractive for a number of applications, especially as building insulation. However, EPS also experiences post-molding shrinkage; it shrinks dimensionally from its molded size after processing. This means parts must be stored in warehouses until they are considered stable by the industry standard, DIN EN 1603. This often takes 11--18 weeks and is thus very timely and expensive. This study aims to decrease the post-molding shrinkage time of EPS foam by understanding the mechanisms of shrinkage behavior. Samples were split into two groups based on their amount of initial volatile matter content and storage conditions, then compared to a control group. Based on thermogravimetric analysis and gas chromatography with mass spectrometry, the volatile matter content and composition was found to not be the sole contributor to EPS foam dimensional stability. Residual stress testing was done with the hole drilling method and Raman spectroscopy. As this type of testing has not been done with polymer foams before, the aim was to see if either method could reliably produce residual stress values. Both methods measured residual stress values with unknown accuracy. All samples stored at a higher temperature (60°C) reached dimensional stability by the end of this study. Thus, air diffusion into EPS foam, encouraged by the high temperature storage, was found to play a significant role in post-molding shrinkage.

Radiocarbon-based assessment of fossil fuel-derived contaminant associations in sediments.

PubMed

White, Helen K; Reddy, Christopher M; Eglinton, Timothy I

2008-08-01

Hydrophobic organic contaminants (HOCs) are associated with natural organic matter (OM) in the environment via mechanisms such as sorption or chemical binding. The latter interactions are difficult to quantitatively constrain, as HOCs can reside in different OM pools outside of conventional analytical windows. Here, we exploited natural abundance variations in radiocarbon (14C) to trace various fossil fuel-derived HOCs (14C-free) within chemically defined fractions of contemporary OM (modern 14C content) in 13 samples including marine and freshwater sediments and one dust and one soil sample. Samples were sequentially treated by solvent extraction followed by saponification. Radiocarbon analysis of the bulk sample and resulting residues was then performed. Fossil fuel-derived HOCs released by these treatments were quantified from an isotope mass balance approach as well as by gas chromatography-mass spectrometry. For the majority of samples (n = 13), 98-100% of the total HOC pool was solvent extractable. Nonextracted HOCs are only significant (29% of total HOC pool)in one sample containing p,p-2,2-bis(chlorophenyl)-1,1,1-trichloroethane and its metabolites. The infrequency of significant incorporation of HOCs into nonextracted OM residues suggests that most HOCs are mobile and bioavailable in the environment and, as such, have a greater potential to exert adverse effects.

Near-lossless multichannel EEG compression based on matrix and tensor decompositions.

PubMed

Dauwels, Justin; Srinivasan, K; Reddy, M Ramasubba; Cichocki, Andrzej

2013-05-01

A novel near-lossless compression algorithm for multichannel electroencephalogram (MC-EEG) is proposed based on matrix/tensor decomposition models. MC-EEG is represented in suitable multiway (multidimensional) forms to efficiently exploit temporal and spatial correlations simultaneously. Several matrix/tensor decomposition models are analyzed in view of efficient decorrelation of the multiway forms of MC-EEG. A compression algorithm is built based on the principle of “lossy plus residual coding,” consisting of a matrix/tensor decomposition-based coder in the lossy layer followed by arithmetic coding in the residual layer. This approach guarantees a specifiable maximum absolute error between original and reconstructed signals. The compression algorithm is applied to three different scalp EEG datasets and an intracranial EEG dataset, each with different sampling rate and resolution. The proposed algorithm achieves attractive compression ratios compared to compressing individual channels separately. For similar compression ratios, the proposed algorithm achieves nearly fivefold lower average error compared to a similar wavelet-based volumetric MC-EEG compression algorithm.

An In Situ Method for Sizing Insoluble Residues in Precipitation and Other Aqueous Samples

PubMed Central

Axson, Jessica L.; Creamean, Jessie M.; Bondy, Amy L.; Capracotta, Sonja S.; Warner, Katy Y.; Ault, Andrew P.

2015-01-01

Particles are frequently incorporated into clouds or precipitation, influencing climate by acting as cloud condensation or ice nuclei, taking up coatings during cloud processing, and removing species through wet deposition. Many of these particles, particularly ice nuclei, can remain suspended within cloud droplets/crystals as insoluble residues. While previous studies have measured the soluble or bulk mass of species within clouds and precipitation, no studies to date have determined the number concentration and size distribution of insoluble residues in precipitation or cloud water using in situ methods. Herein, for the first time we demonstrate that Nanoparticle Tracking Analysis (NTA) is a powerful in situ method for determining the total number concentration, number size distribution, and surface area distribution of insoluble residues in precipitation, both of rain and melted snow. The method uses 500 μL or less of liquid sample and does not require sample modification. Number concentrations for the insoluble residues in aqueous precipitation samples ranged from 2.0–3.0(±0.3)×108 particles cm−3, while surface area ranged from 1.8(±0.7)–3.2(±1.0)×107 μm2 cm−3. Number size distributions peaked between 133–150 nm, with both single and multi-modal character, while surface area distributions peaked between 173–270 nm. Comparison with electron microscopy of particles up to 10 μm show that, by number, > 97% residues are <1 μm in diameter, the upper limit of the NTA. The range of concentration and distribution properties indicates that insoluble residue properties vary with ambient aerosol concentrations, cloud microphysics, and meteorological dynamics. NTA has great potential for studying the role that insoluble residues play in critical atmospheric processes. PMID:25705069

Development of a Simple Dipstick Assay for Operational Monitoring of DDT

PubMed Central

Ismail, Hanafy M.; Kumar, Vijay; Singh, Rudra P.; Williams, Christopher; Shivam, Pushkar; Ghosh, Ayan; Deb, Rinki; Foster, Geraldine M.; Hemingway, Janet; Coleman, Michael; Coleman, Marlize; Das, Pradeep; Paine, Mark J. I.

2016-01-01

Background Indoor residual spraying (IRS) of DDT is used to control visceral leishmaniasis (VL) in India. However, the quality of spraying is severely compromised by a lack of affordable field assays to monitor target doses of insecticide. Our aim was to develop a simple DDT insecticide quantification kit (IQK) for monitoring DDT levels in an operational setting. Methodology/ principle findings DDT quantification was based on the stoichiometric release of chloride from DDT by alkaline hydrolysis and detection of the released ion using Quantab chloride detection strips. The assay was specific for insecticidal p,p`-DDT (LoQ = 0.082 g/m2). Bostik discs were effective in post spray wall sampling, extracting 25–70% of active ingredient depending on surface. Residual DDT was sampled from walls in Bihar state in India using Bostik adhesive discs and DDT concentrations (g p,p`-DDT/m2) were determined using IQK and HPLC (n = 1964 field samples). Analysis of 161 Bostik samples (pooled sample pairs) by IQK and HPLC produced excellent correlation (R2 = 0.96; Bland-Altman bias = −0.0038). IQK analysis of the remaining field samples matched HPLC data in identifying households that had been under sprayed, in range or over sprayed. Interpretation A simple dipstick assay has been developed for monitoring DDT spraying that gives comparable results to HPLC. By making laboratory-based analysis of DDT dosing accessible to field operatives, routine monitoring of DDT levels can be promoted in low- and middle- income countries to maximise the effectiveness of IRS. PMID:26760773

Revealing Pesticide Residues Under High Pesticide Stress in Taiwan's Agricultural Environment Probed by Fresh Honey Bee (Hymenoptera: Apidae) Pollen.

PubMed

Nai, Yu-Shin; Chen, Tsui-Yao; Chen, Yi-Cheng; Chen, Chun-Ting; Chen, Bor-Yann; Chen, Yue-Wen

2017-10-01

Significant pesticide residues are among the most serious problems for sustainable agriculture. In the beekeeping environment, pesticides not only impact a honey bee's survival, but they also contaminate bee products. Taiwan's agricultural environment has suffered from pesticide stress that was higher than that found in Europe and America. This study deciphered problems of pesticide residues in fresh honey bee pollen samples collected from 14 monitoring apiaries in Taiwan, which reflected significant contaminations within the honey bee population. In total, 155 pollen samples were screened for 232 pesticides, and 56 pesticides were detected. Among the residues, fluvalinate and chlorpyrifos showed the highest concentrations, followed by carbendazim, carbaryl, chlorfenapyr, imidacloprid, ethion, and flufenoxuron. The average frequency of pesticide residues detected in pollen samples was ca. 74.8%. The amounts and types of pesticides were higher in winter and in southwestern Taiwan. Moreover, five of these pollen samples were contaminated with 11-15 pesticides, with average levels between 1,560 and 6,390 μg/kg. Compared with the literature, this study emphasized that pollen gathered by honey bee was highly contaminated with more pesticides in Taiwan than in the America, France, and Spain. The ubiquity of pesticides in the pollen samples was likely due to the field applications of common pesticides. Recently, the Taiwanese government began to improve the pesticide policy. According to the resurvey data in 2016, there were reductions in several pesticide contamination parameters in pollen samples from west to southwest Taiwan. A long-term investigation of pollen pesticide residues should be conducted to inspect pesticides usage in Taiwan's agriculture. © The Author 2017. Published by Oxford University Press on behalf of Entomological Society of America. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Assessing Children’s Dietary Pesticide Exposure: Direct Measurement of Pesticide Residues in 24-Hr Duplicate Food Samples

PubMed Central

Lu, Chensheng; Schenck, Frank J.; Pearson, Melanie A.; Wong, Jon W.

2010-01-01

Background The data presented here are a response to calls for more direct measurements of pesticide residues in foods consumed by children and provide an opportunity to compare direct measures of pesticide residues in foods representing actual consumption with those reported by the U.S. Department of Agriculture Pesticide Data Program. Objective We measured pesticide residues in 24-hr duplicate food samples collected from a group of 46 young children participating in the Children’s Pesticide Exposure Study (CPES). Methods Parents were instructed to collect 24-hr duplicate food samples of all conventional fruits, vegetables, and fruit juices equal to the quantity consumed by their children, similarly prewashed/prepared, and from the same source or batch. Individual or composite food items were analyzed for organophosphate (OP) and pyrethroid insecticide residues. Results We collected a total of 239 24-hr duplicate food samples collected from the 46 CPES children. We found 14% or 5% of those food samples contained at least one OP or pyrethroid insecticide, respectively. We measured a total of 11 OP insecticides, at levels ranging from 1 to 387 ng/g, and three pyrethroid insecticides, at levels ranging from 2 to 1,133 ng/g, in children’s food samples. We found that many of the food items consumed by the CPES children were also on the list of the most contaminated food commodities reported by the Environmental Working Group. Conclusions The frequent consumption of food commodities with episodic presence of pesticide residues that are suspected to cause developmental and neurological effects in young children supports the need for further mitigation. PMID:20639183

Identification of beta-lactam antibiotics in tissue samples containing unknown microbial inhibitors.

PubMed

Moats, W A; Romanowski, R D; Medina, M B

1998-01-01

Antibiotic residues in animal tissues can be detected by various screening tests based on microbial inhibition. In the 7-plate assay used by the U.S. Department of Agriculture's Food Safety and Inspection Service (FSIS), penicillinase is incorporated into all but one plate to distinguish beta-lactam antibiotics from other types. However, beta-lactams such as cloxacillin and the cephalosporins are resistant to degradation by penicillinase. They may not be identified as beta-lactams by this procedure, and thus, they may be identified as unidentified microbial inhibitors (UMIs). However, these penicillinase-resistant compounds can be degraded by other beta-lactamases. The present study describes an improved screening protocol to identify beta-lactam antibiotics classified as UMIs. A multiresidue liquid chromatographic procedure based on a method for determining beta-lactams in milk was also used to identify and quantitate residues. The 2 methods were tested with 24 tissue FSIS samples classified as containing UMIs. Of these, 3 contained penicillin G, including one at a violative level, and 5 contained a metabolite of ceftiofur. The others were negative for beta-lactam antibiotics.

Development of a hybrid proximal sensing method for rapid identification of petroleum contaminated soils.

PubMed

Chakraborty, Somsubhra; Weindorf, David C; Li, Bin; Ali Aldabaa, Abdalsamad Abdalsatar; Ghosh, Rakesh Kumar; Paul, Sathi; Nasim Ali, Md

2015-05-01

Using 108 petroleum contaminated soil samples, this pilot study proposed a new analytical approach of combining visible near-infrared diffuse reflectance spectroscopy (VisNIR DRS) and portable X-ray fluorescence spectrometry (PXRF) for rapid and improved quantification of soil petroleum contamination. Results indicated that an advanced fused model where VisNIR DRS spectra-based penalized spline regression (PSR) was used to predict total petroleum hydrocarbon followed by PXRF elemental data-based random forest regression was used to model the PSR residuals, it outperformed (R(2)=0.78, residual prediction deviation (RPD)=2.19) all other models tested, even producing better generalization than using VisNIR DRS alone (RPD's of 1.64, 1.86, and 1.96 for random forest, penalized spline regression, and partial least squares regression, respectively). Additionally, unsupervised principal component analysis using the PXRF+VisNIR DRS system qualitatively separated contaminated soils from control samples. Fusion of PXRF elemental data and VisNIR derivative spectra produced an optimized model for total petroleum hydrocarbon quantification in soils. Copyright © 2015 Elsevier B.V. All rights reserved.

Multiresidue method for pesticide residue analysis in food of animal and plant origin based on GC or LC and MS or MS/MS.

PubMed

Muñoz, Eva; Muñoz, Gloria; Pineda, Laura; Serrahima, Eulalia; Centrich, Francesc

2012-01-01

A multiresidue method based on GC or LC and MS or MS/MS for the determination of 204 pesticides in diverse food matrixes of animal and plant origin is described. The method can include different stages of cleanup according to the chemical characteristics of each sample. Samples were extracted using accelerated solvent extraction. Those with a high fat content or that contained chlorophyll required further purification by gel permeation chromatography and/or SPE (ENVI-Carb). The methodology developed here was fully validated; the LOQs for the 204 pesticides are presented. The LOQ values lie between 0.01 to 0.02 mg/kg. However, in some cases, mainly in baby food, they were as low as 0.003 mg/kg, thereby meeting European Union requirements on maximum residue levels for pesticides, as outlined in European regulation 396/2005 and the Commission Directive 2003/13/EC. The procedure has been accredited for a wide scope of pesticides and matrixes by the Spanish Accreditation Body (ENAC) following ISO/IEC 17025:2005, as outlined in ENAC technical note NT-19.

Evaluation of residual radioactivity in human tissues associated with weapons testing at the nevada test site. Technical report, 1 June 1981-31 March 1989

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wrenn, M.E.; Singh, N.P.; Paschoa, A.S.

1992-11-01

Residual radioactivity consisting of 239 Pu were measured by radiochemistry and alpha spectrometry in samples of bone and soft tissues from 100 autopsies or surgeries from northern and southwestern Utah and from control areas in Colorado and Pennsylvania. Based upon the isotopic ratio 240 Pu/239 Pu contamination was attributable to atmospheric weapons tests at the Nevada Test Site (NTS). In addition, 110 thyroid tissue samples obtained from tissue blocks made at autopsy of veterans dying at the VA hospital in Salt Lake City in the 1940's and 1950's were measured for 129 I (half life 16 million year) and 127more » I (stable) by neutron activation. The results were analyzed by year of death, by periods before and during atmospheric nuclear weapons testing at the NTS and by origin of usual residence. A model was developed to relate thyroid dose from 131 I to the measured 124/127 I ratios, and thyroid dose estimates were made based upon the measured ratios.« less

Propellant Residues Deposition from Firing of 40-mm Grenades

DTIC Science & Technology

2010-09-01

the snow surface downrange of the firing positions in three sampling units on each pad. Samples were analyzed and results compo- sited to derive an...Processing and Analysis ..................................................................... 10 3.1 Snow samples...mm howitzers, propel- lant residues containing DNT were collected from the snow -covered area in front of one of the guns (Walsh, M.E. et al. 2004

Feasibility of using a bacteriophage-based structural color sensor for screening the geographical origins of agricultural products

NASA Astrophysics Data System (ADS)

Seol, Daun; Moon, Jong-Sik; Lee, Yujin; Han, Jiye; Jang, Daeil; Kang, Dong-Jin; Moon, Jiyoung; Jang, Eunjin; Oh, Jin-Woo; Chung, Hoeil

2018-05-01

An M13 bacteriophage-based color sensor, which can change its structural color upon interaction with a gaseous molecule, was evaluated as a screening tool for the discrimination of the geographical origins of three different agricultural products (garlic, onion, and perilla). Exposure of the color sensor to sample odors induced the self-assembled M13 bacteriophage bundles to swell by the interaction of amino acid residues (repeating units of four glutamates) on the bacteriophage with the odor components, resulting in a change in the structural color of the sensor. When the sensor was exposed to the odors of garlic and onion samples, the RGB color changes were considerable because of the strong interactions of the odor components such as disulfides with the glutamate residues on the sensor. Although the patterns of the color variations were generally similar between the domestic and imported samples, some degrees of dissimilarities in their intensities were also observed. Although the magnitude of color change decreased for perilla, the color change patterns between the two groups were somewhat different. With the acquired RGB data, a support vector machine was employed to distinguish the domestic and imported samples, and the resulting accuracies in the measurements of garlic, onion, and perilla samples were 94.1, 88.7, and 91.6%, respectively. The differences in the concentrations of the odor components between both groups and/or the presence of specific components exclusively in the odor of one group allowed the color sensor-based discrimination. The demonstrated color sensor was thus shown to be a potentially versatile and simple as an on-site screening tool. Strategies able to further improve the sensor performance were also discussed.

Feasibility of using a bacteriophage-based structural color sensor for screening the geographical origins of agricultural products.

PubMed

Seol, Daun; Moon, Jong-Sik; Lee, Yujin; Han, Jiye; Jang, Daeil; Kang, Dong-Jin; Moon, Jiyoung; Jang, Eunjin; Oh, Jin-Woo; Chung, Hoeil

2018-05-15

An M13 bacteriophage-based color sensor, which can change its structural color upon interaction with a gaseous molecule, was evaluated as a screening tool for the discrimination of the geographical origins of three different agricultural products (garlic, onion, and perilla). Exposure of the color sensor to sample odors induced the self-assembled M13 bacteriophage bundles to swell by the interaction of amino acid residues (repeating units of four glutamates) on the bacteriophage with the odor components, resulting in a change in the structural color of the sensor. When the sensor was exposed to the odors of garlic and onion samples, the RGB color changes were considerable because of the strong interactions of the odor components such as disulfides with the glutamate residues on the sensor. Although the patterns of the color variations were generally similar between the domestic and imported samples, some degrees of dissimilarities in their intensities were also observed. Although the magnitude of color change decreased for perilla, the color change patterns between the two groups were somewhat different. With the acquired RGB data, a support vector machine was employed to distinguish the domestic and imported samples, and the resulting accuracies in the measurements of garlic, onion, and perilla samples were 94.1, 88.7, and 91.6%, respectively. The differences in the concentrations of the odor components between both groups and/or the presence of specific components exclusively in the odor of one group allowed the color sensor-based discrimination. The demonstrated color sensor was thus shown to be a potentially versatile and simple as an on-site screening tool. Strategies able to further improve the sensor performance were also discussed. Copyright © 2018. Published by Elsevier B.V.

Method and apparatus for determination of material residual stress

NASA Technical Reports Server (NTRS)

Chern, Engmin J. (Inventor); Flom, Yury (Inventor)

1993-01-01

A device for the determination of residual stress in a material sample consisting of a sensor coil, adjacent to the material sample, whose resistance varies according to the amount of stress within the material sample, a mechanical push-pull machine for imparting a gradually increasing compressional and tensional force on the material sample, and an impedance gain/phase analyzer and personal computer (PC) for sending an input signal to and receiving an input signal from the sensor coil is presented. The PC will measure and record the change in resistance of the sensor coil and the corresponding amount of strain of the sample. The PC will then determine, from the measurements of change of resistance and corresponding strain of the sample, the point at which the resistance of the sensor coil is at a minimum and the corresponding value and type of strain of the sample at that minimum resistance point, thereby, enabling a calculation of the residual stress in the sample.

Screening of quinolone antibiotic residues in chicken meat and beef sold in the markets of Ankara, Turkey.

PubMed

Er, Buket; Onurdag, Fatma Kaynak; Demirhan, Burak; Ozgacar, Selda Özgen; Oktem, Aysel Bayhan; Abbasoglu, Ufuk

2013-08-01

This study aimed to find the effects of quinolone antibiotics in chicken and beef used in Ankara, Turkey. Total number of 127 chicken and 104 beef meat samples were collected randomly from local markets for analysis. Extraction and determination of quinolones were made by ELISA procedure. One hundred eighteen of 231 (51.1%) examined chicken meat and beef samples were found to contain quinolone antibiotic residue. Among the chicken meat and beef samples, 58 (45.7%) of chicken meat samples and 60 (57.7%) of beef meat samples were positive for quinolones, respectively. The mean levels (±SE) of quinolones were found to be 30.81 ± 0.45 µg/kg and 6.64 ± 1.11 µg/kg in chicken and beef samples, respectively. This study indicated that some chicken and beef meat sold in Ankara contains residues of quinolone antibiotics.

Study on the abuse of amantadine in tissues of broiler chickens by HPLC-MS/MS.

PubMed

You, X; Yang, S; Zhao, J; Zhang, Y; Zhao, L; Cheng, Y; Hou, C; Xu, Z

2017-10-01

To evaluate the residual target tissues for better monitoring of amantadine abuse in broiler chickens, 22-day-old commercial Arbor Acres broiler chickens were, respectively, fed with 10, 20, and 40 mg/kg of amantadine for five consecutive days. Plasma, breast, and liver tissue samples from the chickens were collected 0, 4, 16, 24, 48, 96, 144, and 312 h after amantadine withdrawal. The high-performance liquid chromatography-tandem mass spectrometry method was used to detect the concentrations of amantadine. The highest concentration was found in the chicken liver and it took the longest time for amantadine to vanish by metabolism. In the high-dose group, amantadine residues were still detected 312 h after amantadine withdrawal. As the amantadine dose increased, amantadine residues in the chicken liver were more slowly to disappear than in other tissues. Even if approximately the same concentration of amantadine residues was found in chicken breast and plasma samples, it took a shorter time before the residues were eliminated. In the medium- and high-dose groups, the concentrations of amantadine residues in chicken liver samples were substantially higher than those in chicken breast and plasma samples, and it took more time to eliminate them. Therefore, the chicken liver can be used as a target tissue to detect illegal use of amantadine. © 2017 John Wiley & Sons Ltd.

Determination of thiamethoxam residues in banana stem and fruit through LC-MS/MS.

PubMed

Suganthi, A; Nikita, S A; Kousika, J; Bhuvaneswari, K; Sridharan, S

2018-04-18

An analytical method based on liquid chromatography coupled with mass spectroscopy/mass spectroscopy was developed and validated for the determination of thiamethoxam residues in banana fruit and stem tissue samples. In this study, Waters Alliance LC and Acquity TQD were used with an electrospray ionization interface in the positive ion mode. An isocratic flow of 0.5% HCOOH in water and 0.05% HCOOH in CH 3 CN was used for separation. Thiamethoxam residue was extracted from the samples using CH 3 CN and a dispersive solid-phase extraction method was used for subsequent cleanup. Linearity studies were conducted between 0.001 and 0.1 μg mL -1 of standard solution with three replicates for each concentration. Satisfactory recoveries (107.21 to 115.16% and 90.94 to 109.22%) and high precision (relative standard deviations of 3.71 to 12.83% and 3.24 to 10.78%) were obtained for the banana stem and banana fruit matrix, respectively. The lower limits of detection and quantification achieved were 0.002 and 0.008 μg g -1 for banana stem and 0.001and 0.005 μg g -1 for banana fruit, respectively. The developed method was used to analyze the banana stem and fruit samples collected from thiamethoxam-treated fields and stems from the local market.

Estimates of diet selection in cattle grazing cornstalk residues by measurement of chemical composition and near infrared reflectance spectroscopy of diet samples collected by ruminal evacuation.

PubMed

Petzel, Emily A; Smart, Alexander J; St-Pierre, Benoit; Selman, Susan L; Bailey, Eric A; Beck, Erin E; Walker, Julie A; Wright, Cody L; Held, Jeffrey E; Brake, Derek W

2018-05-04

Six ruminally cannulated cows (570 ± 73 kg) fed corn residues were placed in a 6 × 6 Latin square to evaluate predictions of diet composition from ruminally collected diet samples. After complete ruminal evacuation, cows were fed 1-kg meals (dry matter [DM]-basis) containing different combinations of cornstalk and leaf and husk (LH) residues in ratios of 0:100, 20:80, 40:60, 60:40, 80:20, and 100:0. Diet samples from each meal were collected by removal of ruminal contents after 1-h and were either unrinsed, hand-rinsed or machine-rinsed to evaluate effects of endogenous compounds on predictions of diet composition. Diet samples were analyzed for neutral (NDF) and acid (ADF) detergent fiber, acid detergent insoluble ash (ADIA), acid detergent lignin (ADL), crude protein (CP), and near infrared reflectance spectroscopy (NIRS) to calculate diet composition. Rinsing type increased NDF and ADF content and decreased ADIA and CP content of diet samples (P < 0.01). Rinsing tended to increase (P < 0.06) ADL content of diet samples. Differences in concentration between cornstalk and LH residues within each chemical component were standardized by calculating a coefficient of variation (CV). Accuracy and precision of estimates of diet composition were analyzed by regressing predicted diet composition and known diet composition. Predictions of diet composition were improved by increasing differences in concentration of chemical components between cornstalk and LH residues up to a CV of 22.6 ± 5.4%. Predictions of diet composition from unrinsed ADIA and machine-rinsed NIRS had the greatest accuracy (slope = 0.98 and 0.95, respectively) and large coefficients of determination (r2 = 0.86 and 0.74, respectively). Subsequently, a field study (Exp. 2) was performed to evaluate predictions of diet composition in cattle (646 ± 89 kg) grazing corn residue. Five cows were placed in 1 of 10 paddocks and allowed to graze continuously or to strip-graze corn residues. Predictions of diet composition from ADIA, ADL, and NIRS did not differ (P = 0.99), and estimates of cornstalk intake tended to be greater (P = 0.09) in strip-grazed compared to continuously grazed cows. These data indicate that diet composition can be predicted by chemical components or NIRS by ruminal collection of diet samples among cattle grazing corn residues.

Residual strength of GFR/POM as a function of damage

NASA Astrophysics Data System (ADS)

Zachariev, G.; Rudolph, H.-V.; Ivers, H.

2010-07-01

A relation between the residual strength and the dispersed damage accumulated in a short fiber reinforced polyoximethylene (GFR/POM) samples under tension is found. For that purpose dependencies of damage and residual strength on loading percentage are used. Damage as a function of loading percentage is known for the material under study. To find the dependency of residual strength on loading percentage a subsidiary function is introduced and a method is proposed for determination of the parameters in the dependency on the basis of the experimental data. Both damage and residual strength are measured after unloading samples that have been loaded applying different loading percentages. Damage is the accumulation of new internal surfaces that arise under mechanical loading in the whole volume of the material. They are registered by a new original method of X-ray refraction. The analytical relation between the residual strength and damage accumulated is compared to the experimental results found for the residual strength under different damage degrees.

Organochlorine pesticides in plasma of migrating peregrine falcons at Padre Island, Texas, Spring 1978-80 vs. Spring 1984

USGS Publications Warehouse

Henny, C.J.; Riddle, K.E.; Hulse, C.S.

1985-01-01

A spring concentration of migrating Peregrine Falcons (Falco peregrinus) was first discovered at Padre Island, Texas, in April 1978. The birds were first captured and blood-sampled for monitoring residue burdens and trends in the late 1970' s. Only 29 Peregrines were sampled in 1978 and 1979, but 111 were sampled in 1980. The initial investigation showed that DDE in the plasma of spring migrants returning from Latin America for the first time declined significantly during the study (through 1980). In the spring of 1984, 48 Peregrines were captured at Padre Island with blood samples again collected. This report will compare plasma residue data from the earlier study with residues obtained in 1984.

Activity-based assay for ricin-like toxins

DOEpatents

Keener, William K.; Ward, Thomas E.

2007-02-06

A method of detecting N-glycosylase activity in a sample involves incubating an oligodeoxyribonucleotide substrate containing a deoxyadenosine or deoxyuridine residue with the sample to be tested such that the N-glycosylase, if present, hydrolyzes the deoxyadenosine or deoxyuridine residue to result in an N-glycosylase product having an abasic site. A primer is annealed to the N-glycosylase product, and the primer is extended with a DNA polymerase, such as Taq DNA polymerase, that pauses at abasic sites. The resulting extension products are melted from the N-glycosylase product, allowed to form hairpins due to self-complementarity, and further extended in the presence of labeled precursors to result in labeled products. Extension products synthesized from undigested substrate as template do not result in labeled products. Thus, detection of labeled products results in detection of N-glycosylase activity. Oligodeoxyribonucleotide substrates, primer, and positive controls and a kit for N-glycosylase assay are also disclosed.

Determination of residual stress in a microtextured α titanium component using high-energy synchrotron X-rays

DOE PAGES

Park, Jun -Sang; Ray, Atish K.; Dawson, Paul R.; ...

2016-05-02

A shrink-fit sample is manufactured with a Ti-8Al-1Mo-1V alloy to introduce a multiaxial residual stress field in the disk of the sample. A set of strain and orientation pole figures are measured at various locations across the disk using synchrotron high-energy X-ray diffraction. Two approaches—the traditional sin 2Ψ method and the bi-scale optimization method—are taken to determine the stresses in the disk based on the measured strain and orientation pole figures, to explore the range of solutions that are possible for the stress field within the disk. While the stress components computed using the sin 2Ψ method and the bi-scalemore » optimization method have similar trends, their magnitudes are significantly different. Lastly, it is suspected that the local texture variation in the material is the cause of this discrepancy.« less

Emissions of volatile organic compounds from maize residue open burning in the northern region of Thailand

NASA Astrophysics Data System (ADS)

Sirithian, Duanpen; Thepanondh, Sarawut; Sattler, Melanie L.; Laowagul, Wanna

2018-03-01

Emission factors for speciated volatile organic compounds (VOCs) from maize residue burning were determined in this study based on chamber experiments. Thirty-six VOC species were identified by Gas Chromatography/Mass Spectrometer (GC/MS). They were classified into six groups, including alkanes, alkenes, oxygenated VOCs, halogenated VOCs, aromatics and other. The emission factor for total VOCs was estimated as about 148 mg kg-1 dry mass burned. About 68.4% of the compounds were aromatics. Field samplings of maize residues were conducted to acquire the information of fuel characteristics including fuel loading, fraction of maize residues that were actually burned as well as proximate and elemental analysis of maize residues. The emission factors were then applied to estimate speciated VOC emissions from maize residue open burning at the provincial level in the upper-northern region of Thailand for the year 2014. Total burned area of maize covered an area of about 500,000 ha which was about 4.7% of the total area of upper-northern region of the country. It was found that total VOC emissions released during the burning season (January-April) was about 79.4 tons. Ethylbenzene, m,p-xylene, 1,2,4-trimethylbenzene, acetaldehyde and o-xylene were the major contributors, accounting for more than 65% of total speciated VOC emissions.

Effects of storage and processing on residue levels of chlorpyrifos in soybeans.

PubMed

Zhao, Liuwei; Ge, Jing; Liu, Fengmao; Jiang, Naiwen

2014-05-01

The residue levels of chlorpyrifos in soybeans during storage and processing were investigated. Soybeans were treated with chlorpyrifos aqueous solution and placed in a sealed plastic container. The residue of chlorpyrifos was determined in soybeans at six time points within 0 and 112days during storage and oil processing of the soybeans was conducted. The analysis of the residues of chlorpyrifos was carried out by gas chromatography-mass spectrometry (GC-MS). Results show that the dissipation of chlorpyrifos in soybeans is about 62% during the storage period. Moreover, the carryover of the residues from soybeans into oil is found to be related to the processing methods. Processing factor, which is defined as the ratio of chlorpyrifos residue concentration in oil sample to that in the soybean samples, was 11 and 0.25 after cold and hot pressing, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

Method and apparatus for the evaluation of a depth profile of thermo-mechanical properties of layered and graded materials and coatings

DOEpatents

Finot, Marc; Kesler, Olivera; Suresh, Subra

1998-01-01

A technique for determining properties such as Young's modulus, coefficient of thermal expansion, and residual stress of individual layers within a multi-layered sample is presented. The technique involves preparation of a series of samples, each including one additional layer relative to the preceding sample. By comparison of each sample to a preceding sample, properties of the topmost layer can be determined, and residual stress at any depth in each sample, resulting from deposition of the top layer, can be determined.

Monitoring the Presence of 13 Active Compounds in Surface Water Collected from Rural Areas in Northwestern Spain

PubMed Central

Iglesias, Alejandra; Nebot, Carolina; Vázquez, Beatriz I.; Coronel-Olivares, Claudia; Franco Abuín, Carlos M.; Cepeda, Alberto

2014-01-01

Drug residues are considered environmental contaminants, and their occurrence has recently become a matter of concern. Analytical methods and monitoring systems are therefore required to control the continuous input of these drug residues into the environment. This article presents a suitable HPLC-ESI-MS/MS method for the simultaneous extraction, detection and quantification of residues of 13 drugs (antimicrobials, glucocorticosteroids, anti-inflammatories, anti-hypertensives, anti-cancer drugs and triphenylmethane dyes) in surface water. A monitoring study with 549 water samples was carried out in northwestern Spain to detect the presence of drug residues over two sampling periods during 2010, 2011 and 2012. Samples were collected from rural areas with and without farming activity and from urban areas. The 13 analytes were detected, and 18% of the samples collected showed positive results for the presence of at least one analyte. More collection sites were located in rural areas than in urban areas. However, more positive samples with higher concentrations and a larger number of analytes were detected in samples collected from sites located after the discharge of a WWTP. Results indicated that the WWTPs seems to act as a concentration point. Positive samples were also detected at a site located near a drinking water treatment plant. PMID:24837665

Identification and quantification of pesticide residues in water samples of Dhamrai Upazila, Bangladesh

NASA Astrophysics Data System (ADS)

Hasanuzzaman, M.; Rahman, M. A.; Salam, M. A.

2017-10-01

Being agricultural country, different types of pesticides are widely used in Bangladesh to prevent the crop losses due to pest attack which are ultimately drain to the water bodies. The present study was conducted to identify and quantify the organochlorine (DDT, DDE and DDD), organophosphorus (malathion, diazinon and chloropyrifos) and carbamate (carbaryl) residues in water samples of different sources from Dhamrai upazila of Bangladesh using high performance liquid chromatography (HPLC) equipped with ultra violate (UV) detector. Thirty water samples from fish pond, cultivated land and tube-well were collected in winter season to analyze the pesticide residues. Among the organophosphorus pesticides, malathion was present in seven water samples ranging from 42.58 to 922.8 μg/L, whereas diazinon was detected in water sample-8 (WS-8) and the concentration was 31.5 μg/L. None of the tested water samples was found to be contaminated with chlorpyrifos, carbaryl or DDT and its metabolites (DDE and DDD). Except for a tube-well water sample, concentrations of the detected residues are above the acceptable limit for human body as assigned by different organizations. To avoid the possible health hazards, the indiscriminate application of pesticides should be restricted and various substitute products like bio-pesticide should be introduced in a broad scale as soon as possible.

Monitoring the presence of 13 active compounds in surface water collected from rural areas in northwestern Spain.

PubMed

Iglesias, Alejandra; Nebot, Carolina; Vázquez, Beatriz I; Coronel-Olivares, Claudia; Abuín, Carlos M Franco; Cepeda, Alberto

2014-05-15

Drug residues are considered environmental contaminants, and their occurrence has recently become a matter of concern. Analytical methods and monitoring systems are therefore required to control the continuous input of these drug residues into the environment. This article presents a suitable HPLC-ESI-MS/MS method for the simultaneous extraction, detection and quantification of residues of 13 drugs (antimicrobials, glucocorticosteroids, anti-inflammatories, anti-hypertensives, anti-cancer drugs and triphenylmethane dyes) in surface water. A monitoring study with 549 water samples was carried out in northwestern Spain to detect the presence of drug residues over two sampling periods during 2010, 2011 and 2012. Samples were collected from rural areas with and without farming activity and from urban areas. The 13 analytes were detected, and 18% of the samples collected showed positive results for the presence of at least one analyte. More collection sites were located in rural areas than in urban areas. However, more positive samples with higher concentrations and a larger number of analytes were detected in samples collected from sites located after the discharge of a WWTP. Results indicated that the WWTPs seems to act as a concentration point. Positive samples were also detected at a site located near a drinking water treatment plant.

Comparison of questionnaire-based estimation of pesticide residue intake from fruits and vegetables with urinary concentrations of pesticide biomarkers.

PubMed

Chiu, Yu-Han; Williams, Paige L; Mínguez-Alarcón, Lidia; Gillman, Matthew; Sun, Qi; Ospina, Maria; Calafat, Antonia M; Hauser, Russ; Chavarro, Jorge E

2018-01-01

We developed a pesticide residue burden score (PRBS) based on a food frequency questionnaire and surveillance data on food pesticide residues to characterize dietary exposure over the past year. In the present study, we evaluated the association of the PRBS with urinary concentrations of pesticide biomarkers. Fruit and vegetable (FV) intake was classified as having high (PRBS≥4) or low (PRBS<4) pesticide residues for 90 men from the EARTH study. Two urine samples per man were analyzed for seven biomarkers of organophosphate and pyrethroid insecticides, and the herbicide 2,4-dichlorophenoxyacetic acid. We used generalized estimating equations to analyze the association of the PRBS with urinary concentrations of pesticide biomarkers. Urinary concentrations of pesticide biomarkers were positively related to high pesticide FV intake but inversely related to low pesticide FV intake. The molar sum of urinary concentrations of pesticide biomarkers was 21% (95% confidence interval (CI): 2%, 44%) higher for each one serving/day increase in high pesticide FV intake, and 10% (95% CI: 1%, 18%) lower for each one serving/day increase in low pesticide FV intake. Furthermore, intake of high pesticide FVs positively related to most individual urinary biomarkers. Our findings support the usefulness of the PRBS approach to characterize dietary exposure to select pesticides.

Evaluation of a new modified QuEChERS method for the monitoring of carbamate residues in high-fat cheeses by using UHPLC-MS/MS.

PubMed

Hamed, Ahmed M; Moreno-González, David; Gámiz-Gracia, Laura; García-Campaña, Ana M

2017-01-01

A simple and efficient method for the determination of 28 carbamates in high-fat cheeses is proposed. The methodology is based on a modified quick, easy, cheap, effective, rugged, and safe procedure as sample treatment using a new sorbent (Z-Sep + ) followed by ultra-high performance liquid chromatography with tandem mass spectrometry determination. The method has been validated in different kinds of cheese (Gorgonzola, Roquefort, and Camembert), achieving recoveries of 70-115%, relative standard deviations lower than 13% and limits of quantification lower than 5.4 μg/kg, below the maximum residue levels tolerated for these compounds by the European legislation. The matrix effect was lower than ±30% for all the studied pesticides. The combination of ultra-high performance liquid chromatography and tandem mass spectrometry with this modified quick, easy, cheap, effective, rugged, and safe procedure using Z-Sep + allowed a high sample throughput and an efficient cleaning of extracts for the control of these residues in cheeses with a high fat content. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fluorescence spectra of blood plasma treated with ultraviolet irradiation in vivo

NASA Astrophysics Data System (ADS)

Zalesskaya, G. A.; Maslova, T. O.

2010-09-01

We have studied the fluorescence spectra of blood plasma from patients with acute coronary syndrome, and also the effect of therapeutic doses of in vivo ultraviolet blood irradiation (UBI) on the spectra. We have established that the maxima in the fluorescence spectra of the original plasma samples, obtained from unirradiated blood, are located in the wavelength interval 330-340 nm, characteristic for the fluorescence of tryptophan residues. In extracorporeal UBI ( λ = 254 nm), we observed changes in the shape and also both a blue and a red shift in the maxima of the fluorescence spectra, differing in magnitude for blood plasma samples from different patients in the test group. We show that UBI-initiated changes in the fluorescence spectra of the plasma depend on the original pathological disturbances of metabolite levels, and also on the change in the oxygen-transport function of the blood and the acid-base balance, affecting the oxidative stability of the plasma. We have concluded that UV irradiation, activating buffer systems in the blood, has an effect on the universal and specific interactions of the tryptophan residue with the amino acid residues and water surrounding it.

Total sulfur determination in residues of crude oil distillation using FT-IR/ATR and variable selection methods

NASA Astrophysics Data System (ADS)

Müller, Aline Lima Hermes; Picoloto, Rochele Sogari; Mello, Paola de Azevedo; Ferrão, Marco Flores; dos Santos, Maria de Fátima Pereira; Guimarães, Regina Célia Lourenço; Müller, Edson Irineu; Flores, Erico Marlon Moraes

2012-04-01

Total sulfur concentration was determined in atmospheric residue (AR) and vacuum residue (VR) samples obtained from petroleum distillation process by Fourier transform infrared spectroscopy with attenuated total reflectance (FT-IR/ATR) in association with chemometric methods. Calibration and prediction set consisted of 40 and 20 samples, respectively. Calibration models were developed using two variable selection models: interval partial least squares (iPLS) and synergy interval partial least squares (siPLS). Different treatments and pre-processing steps were also evaluated for the development of models. The pre-treatment based on multiplicative scatter correction (MSC) and the mean centered data were selected for models construction. The use of siPLS as variable selection method provided a model with root mean square error of prediction (RMSEP) values significantly better than those obtained by PLS model using all variables. The best model was obtained using siPLS algorithm with spectra divided in 20 intervals and combinations of 3 intervals (911-824, 823-736 and 737-650 cm-1). This model produced a RMSECV of 400 mg kg-1 S and RMSEP of 420 mg kg-1 S, showing a correlation coefficient of 0.990.

Resolution of a disputed albendazole result in the UK Official Control System - time for more guidance?

PubMed

Walker, Michael; Gray, Kirstin; Hopley, Christopher; Mussell, Christopher; Clifford, Louise; Meinerikandathevan, Jayanie; Firpo, Leonardo; Topping, Joanna; Santacruz, Daniel

2017-04-01

Albendazole, one of the benzimidazole anthelmintics, is used in ruminants and has maximum residue limits in muscle, fat and other tissue owing to reported teratogenicity. Albendazole is extensively metabolised in domestic animals and humans with rapid conversion to a sulphoxide and subsequently sulphone and amino sulphone metabolites. Sulphoxide metabolites are responsible for the systemic biological activity of benzimidazole drugs. Herein we report a case of disputed results for albendazole in a consignment sampled at import in which the Official Analyst certified against the consignment for excess albendazole. A laboratory acting for the importer reported data below the MRL, including a finding of the parent drug which is not included in the residue definition. The Government Chemist has a statutory duty as a route of technical appeal in the UK Official Food Control system and the case was referred for referee analysis. We report our findings based on a LC-MS/MS method, which confirmed the official findings, did not reveal the presence of the parent drug but identified hot spots of albendazole marker residues in the consignment. We discuss the need for recommendations on official sampling at import and interpretation of results.

Influence of zirconia framework thickness on residual stress profile in veneering ceramic: measurement by hole-drilling.

PubMed

Mainjot, Amélie K; Schajer, Gary S; Vanheusden, Alain J; Sadoun, Michaël J

2012-04-01

Framework design is reported to influence chipping in zirconia-based restorations, which is an important cause of failure of such restorations. Residual stress profile in the veneering ceramic after the manufacturing process is an important predictive factor of the mechanical behavior of the material. The objective of this study is to investigate the influence of framework thickness on the stress profile measured in zirconia-based structures. The stress profile was measured with the hole-drilling method in bilayered disc samples of 20mm diameter with a 1.5 mm thick veneering ceramic layer. Six different framework thicknesses from 0.5 mm to 3 mm were studied. Two different cooling procedures were also investigated. Compressive stresses were observed in the surface, and tensile stresses in the depth of most of the samples. The slow cooling procedure was found to promote the development of interior tensile stresses, except for the sample with a 3mm thick framework. With the tempering procedure, samples with a 1.5 mm thick framework exhibited the most favorable stress profile, while thicker and thinner frameworks exhibited respectively in surface or interior tensile stresses. The measurements performed highlight the importance of framework thickness, which determine the nature of stresses and can explain clinical failures encountered, especially with thin frameworks. The adequate ratio between veneering ceramic and zirconia is hard to define, restricting the range of indications of zirconia-based restorations until a better understanding of such a delicate veneering process is achieved. Copyright © 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Evolution of Residual Stress and Distortion of Cold-Rolled Bearing Ring from Annealing to Quenched-Tempered Heat Treatment

NASA Astrophysics Data System (ADS)

Lu, Bohan; Lu, Xiaohui

2018-02-01

This study investigates the correlation between the residual stress and distortion behavior of a cold-rolled ring from the annealing to quenching-tempering (QT) process. Due to the cold-rolled process, the external periphery of the bearing ring experiences a compressive residual stress. To relieve the residual stress, cold-rolled rings are annealed at 700 °C which is higher than the starting temperature of recrystallization. When cold-rolled rings are annealed at 700 °C for 15 min, the compressive residual stress is reduced to zero and the outer diameter of the annealed ring becomes larger than that of a non-annealed sample, which is unrelated to annealing time. Simultaneously, the roundness and taper deviation do not obviously change compared with those of non-annealed sample. The stress relaxation during the annealing process was attributed to the recovery and recrystallization of ferrite. Annealing has a genetic influence on the following QT heat treatment, wherein the lowest residual stress is in the non-annealed cold-rolled ring. From the annealing to QT process, the deviation of the outer diameter, roundness, and taper increased with annealing time, a large extend than that of non-annealed samples.

Antibiotic residues in milk and eggs of commercial and local farms at Chittagong, Bangladesh.

PubMed

Chowdhury, Suchayan; Hassan, Mohammad Mahmudul; Alam, Mahabub; Sattar, Sarmina; Bari, Md Saiful; Saifuddin, A K M; Hoque, Md Ahasanul

2015-04-01

The study was conducted to detection and determination of concentration or level of antibiotic residues in milk and egg of local and commercial farms at Chittagong during December 2011 to June 2012. A total of 400 (200 milk and 200 egg) samples were collected from local and commercial dairy cows and local scavenging and commercial poultry farms, respectively. Microbial inhibition test and thin layer chromatography were used for screening and ultra-high performance liquid chromatography was used to estimate the concentrations of antibiotic residues in samples. Tetracycline, amoxicillin, and ciprofloxacin residues were significantly (p ≤ 0.05) higher in commercial farms than local. The boiling insignificantly (p>0.05) reduced residues level in milk and egg. The average concentrations of amoxicillin residue in local milk, commercial milk, local egg, and commercial egg were 9.84 µg/ml, 56.16 µg/ml, 10.46 µg/g and 48.82 µg/g, respectively, in raw samples and were reduced to 9.81 µg/ml, 55.54 µg/ml, 10.29 µg/g, and 48.38 µg/g, respectively, after boiling. Proper maintaining of the withdrawal period and development of active surveillance system are highly recommended for public health security.

Organophosphorus and carbamate pesticide residues detected in water samples collected from paddy and vegetable fields of the Savar and Dhamrai Upazilas in Bangladesh.

PubMed

Chowdhury, Md Alamgir Zaman; Banik, Sanjoy; Uddin, Borhan; Moniruzzaman, Mohammed; Karim, Nurul; Gan, Siew Hua

2012-09-11

Several types of organophosphorous and carbamate pesticides have been used extensively by the farmers in Bangladesh during the last few decades. Twenty seven water samples collected from both paddy and vegetable fields in the Savar and Dhamrai Upazilas in Bangladesh were analyzed to determine the occurrence and distribution of organo-phosphorus (chlorpyrifos, malathion and diazinon) and carbamate (carbaryl and carbofuran) pesticide residues. A high performance liquid chromatograph instrument equipped with a photodiode array detector was used to determine the concentrations of these pesticide residues. Diazinon and carbofuran were detected in water samples collected from Savar Upazila at 0.9 μg/L and 198.7 μg/L, respectively. Malathion was also detected in a single water sample at 105.2 μg/L from Dhamrai Upazila. Carbaryl was the most common pesticide detected in Dhamrai Upazila at 14.1 and 18.1 μg/L, while another water sample from Dhamrai Upazila was contaminated with carbofuran at 105.2 μg/L. Chlorpyrifos was not detected in any sample. Overall, the pesticide residues detected were well above the maximum acceptable levels of total and individual pesticide contamination, at 0.5 and 0.1 μg/L, respectively, in water samples recommended by the European Economic Community (Directive 98/83/EC). The presence of these pesticide residues may be attributed by their intense use by the farmers living in these areas. Proper handling of these pesticides should be ensured to avoid direct or indirect exposure to these pesticides.

Pesticide residues and estrogenic activity in fruit and vegetables sampled from major fresh produce markets in South Africa.

PubMed

Mutengwe, Mbulaheni Thomas; Aneck-Hahn, Natalie Hildegard; Korsten, Lise; Van Zijl, Magdalena Catherina; De Jager, Christiaan

2016-01-01

Food is likely to be one of the major pathways through which people are exposed to endocrine-disrupting chemicals. With the exception of residual effects, there are concerns that a number of naturally occurring and synthetic chemicals exert adverse effects upon endocrine systems in wildlife and humans. The current study reports selected pesticide concentrations and the total estrogenic activity of fruit and vegetables using the recombinant yeast oestrogen screen (YES) and T47D-KBluc reporter gene assays. A total of 53 food samples (27 fruit and 26 vegetables) from Johannesburg and Tshwane fresh produce markets (in South Africa) were analysed. Of these, 17 contained one to three different pesticide residues with concentrations ranging between 0.01 and 0.68 mg kg(-1), whereas in the rest of the samples no residues were detected. All pesticides detected except in one sample were below the maximum residue level (MRL), but others were unauthorised for use in specified fruit and vegetables. Estrogenic activity was detected in 26.4% (14 samples) of the samples tested, and the estradiol equivalents ranged from 0.007 to 2 pg g(-1). Although the estrogenic activity was low, it may contribute to adverse health effects. Continuous monitoring for pesticides in fruit and vegetables is important in view of the unauthorised pesticides detected in produce from South Africa and the endocrine-disrupting chemical activity found.

Pesticide residues in honey bees, pollen and beeswax: Assessing beehive exposure.

PubMed

Calatayud-Vernich, Pau; Calatayud, Fernando; Simó, Enrique; Picó, Yolanda

2018-05-23

In order to study the distribution of pesticide residues in beekeeping matrices, samples of live in-hive worker honey bees (Apis mellifera), fresh stored pollen and beeswax were collected during 2016-2017 from 45 apiaries located in different landscape contexts in Spain. A total of 133 samples were screened for 63 pesticides or their degradation products to estimate the pesticide exposure to honey bee health through the calculation of the hazard quotient (HQ). The influence of the surrounding environment on the content of pesticides in pollen was assessed by comparing the concentrations of pesticide residues found in apiaries from intensive farming landscapes to those found in apiaries located in mountainous, grassland and urban contexts. Beeswax revealed high levels of miticides used in beekeeping such as coumaphos, chlorfenvinphos, fluvalinate and acrinathrin, which were detected in more than 75% of samples. Pollen was predominantly contaminated by miticides but also by insecticides used in agriculture such as chlorpyrifos and acetamiprid, which showed concentrations significantly higher in apiaries located in intensive farming contexts. Pesticides residues were less frequent and at lower concentrations in live honey bees. Beeswax showed the highest average hazard scores (HQ > 5000) to honey bees. Pollen samples contained the largest number of pesticide residues and relevant hazard (HQ > 50) to bees. Acrinathrin was the most important contributor to the hazard quotient scores in wax and pollen samples. The contributions of the pesticides dimethoate and chlorpyrifos to HQ were considered relevant in samples. Copyright © 2018 Elsevier Ltd. All rights reserved.

Dietary exposure to pesticide residues from foods of plant origin and drinks in Lebanon.

PubMed

Nasreddine, Lara; Rehaime, Maria; Kassaify, Zeina; Rechmany, Roula; Jaber, Farouk

2016-08-01

This study assesses the dietary exposure of Lebanese adults to 47 pesticide residues from both foods of plant origin and drinks. The study was conducted using the Total Diet Study protocol in two different areas of Lebanon: Greater Beirut (urban) and Keserwan (semi-rural). A total of 1860 individual foods were collected, prepared, and cooked prior to analysis. Composite samples of similar foods were analyzed, following the QuEChERS Multiresidue method. Eighteen residues were detected/quantified on at least one composite sample, with 66.7 % of the results being quantifiable and 33.3 % detectable. Quantifiable levels ranged between 10.3 and 208 μg/kg. For the composite samples where residues were detected, 55 % had one residue, while 45 % had 2-4 residues. The most frequently detected/quantified pesticide residues included Chlorpyrifos, Procymidone, Primiphos methyl, Dimethoate, and Dieldrin. The dietary exposure assessment was conducted using the deterministic approach with two scenarios: (1) the lower bound (LB) approach and (2) the upper bound (UB) approach. Using the LB approach, mean estimated daily exposures were far below the acceptable daily intakes (ADIs) for all investigated residues. Using the UB approach, which tends to overestimate exposure, mean estimated daily exposures were below the ADIs for all residues except for Dieldrin (semi-rural: 128.7 % ADI; urban: 100.7 % ADI). Estimates of mean exposure to Diazinon reached 50.3 % of ADI in the urban diet and 61.9 % in the semi-rural diet. Findings of this study identify specific pesticide residues as monitoring priorities for which more comprehensive and sensitive analyses are needed in order to refine exposure assessment.

The relationship between blood and muscle samples to monitor for residues of the antibiotic enrofloxacin in chickens.

PubMed

Reyes-Herrera, I; Schneider, M J; Blore, P J; Donoghue, D J

2011-02-01

In 2005, the US Food and Drug Administration withdrew approval for use of enrofloxacin in poultry, thus effectively imposing zero tolerance for residues of this antibiotic in poultry. Conventional residue monitoring for most antibiotics, including enrofloxacin, involves removing poultry carcasses from the processing line and collecting muscle tissues for analysis. Because of the loss of valuable edible products and the difficulties and expense of sampling all the carcasses, only a small portion of carcasses are tested for violative residues. Unlike muscle tissue, blood is readily available from all birds at the beginning of processing and may be used to screen for illegal residues in all poultry carcasses. It is unknown, however, if enrofloxacin concentrations in blood are predictive of muscle concentrations. In an effort to evaluate this relationship, 156 broiler chickens, 5 wk of age, were dosed with either 25 or 50 µg/mL of enrofloxacin for 3 or 7 d, respectively, in the drinking water. Blood and muscle samples were collected at 0, 1, 3, 6, 12, and 24 h (n = 6 birds/group) during the first dosing day, every 48 h during the dosing period, and every 12 h during the withdrawal period for up to 60 h after withdrawal. Enrofloxacin residues were determined in all blood and tissue samples during the dosing periods and in most of the withdrawal period for both doses. These results support the potential to use blood to screen for illegal enrofloxacin residues in edible poultry tissues in an effort to protect the human food supply.

Three essays on price dynamics and causations among energy markets and macroeconomic information

NASA Astrophysics Data System (ADS)

Hong, Sung Wook

This dissertation examines three important issues in energy markets: price dynamics, information flow, and structural change. We discuss each issue in detail, building empirical time series models, analyzing the results, and interpreting the findings. First, we examine the contemporaneous interdependencies and information flows among crude oil, natural gas, and electricity prices in the United States (US) through the multivariate generalized autoregressive conditional heteroscedasticity (MGARCH) model, Directed Acyclic Graph (DAG) for contemporaneous causal structures and Bernanke factorization for price dynamic processes. Test results show that the DAG from residuals of out-of-sample-forecast is consistent with the DAG from residuals of within-sample-fit. The result supports innovation accounting analysis based on DAGs using residuals of out-of-sample-forecast. Second, we look at the effects of the federal fund rate and/or WTI crude oil price shock on US macroeconomic and financial indicators by using a Factor Augmented Vector Autoregression (FAVAR) model and a graphical model without any deductive assumption. The results show that, in contemporaneous time, the federal fund rate shock is exogenous as the identifying assumption in the Vector Autoregression (VAR) framework of the monetary shock transmission mechanism, whereas the WTI crude oil price return is not exogenous. Third, we examine price dynamics and contemporaneous causality among the price returns of WTI crude oil, gasoline, corn, and the S&P 500. We look for structural break points and then build an econometric model to find the consistent sub-periods having stable parameters in a given VAR framework and to explain recent movements and interdependency among returns. We found strong evidence of two structural breaks and contemporaneous causal relationships among the residuals, but also significant differences between contemporaneous causal structures for each sub-period.

Determination of sulfadiazine, trimethoprim, and N(4) -acetyl-sulfadiazine in fish muscle plus skin by Liquid Chromatography-Mass Spectrometry. Withdrawal-time calculation after in-feed administration in gilthead sea bream (Sparus aurata L.) fed two different diets.

PubMed

Zonaras, V; Tyrpenou, A; Alexis, M; Koupparis, M

2016-10-01

This study presents a depletion study for sulfadiazine and trimethoprim in muscle plus skin of gilthead sea bream (Sparus aurata L.). N(4) -acetyl-sulfadiazine, the main metabolite of sulfadiazine (SDZ), was also examined. The fish were held in seawater at a temperature of 24-26 °C. SDZ and trimethoprim (TMP) were administered orally with medicated feed for five consecutive days at daily doses of 25 mg SDZ and 5 mg TMP per kg of fish body weight per day. Two different diets, fish oil- and plant oil-based diets, were investigated. Ten fish were sampled at each of the days 1, 3, 5, 6, 8, 9, 10, and 12 after the start of veterinary medicine administration. However for the calculation of the withdrawal periods, sampling day 1 was set as 24 h after the last dose of the treatment. Fish samples were analyzed for SDZ, TMP, and acetyl-sulfadiazine (AcSDZ) residues by liquid chromatography-mass spectrometry. SDZ and TMP concentrations declined rapidly from muscle plus skin. Considering a maximum residue limit of 100 μg/kg for the total of sulfonamides and 50 μg/kg for TMP residues in fish muscle plus skin, the withdrawal periods of the premix trimethoprim-sulfadiazine 50% were calculated as 5 and 6 days, at 24-26 °C, in fish oil (FO) and plant oil (PO) groups, respectively. The investigation of this work is important to protect consumers by controlling the undesirable residues in fish. © 2016 John Wiley & Sons Ltd.

Water Use Practices Limit the Effectiveness of a Temephos-Based Aedes aegypti Larval Control Program in Northern Argentina

PubMed Central

Garelli, Fernando M.; Espinosa, Manuel O.; Weinberg, Diego; Trinelli, María A.; Gürtler, Ricardo E.

2011-01-01

Background A five-year citywide control program based on regular application of temephos significantly reduced Aedes aegypti larval indices but failed to maintain them below target levels in Clorinda, northern Argentina. Incomplete surveillance coverage and reduced residuality of temephos were held as the main putative causes limiting effectiveness of control actions. Methodology The duration of temephos residual effects in household-owned water-holding tanks (the most productive container type and main target for control) was estimated prospectively in two trials. Temephos was applied using spoons or inside perforated small zip-lock bags. Water samples from the study tanks (including positive and negative controls) were collected weekly and subjected to larval mortality bioassays. Water turnover was estimated quantitatively by adding sodium chloride to the study tanks and measuring its dilution 48 hs later. Principal Findings The median duration of residual effects of temephos applied using spoons (2.4 weeks) was significantly lower than with zip-lock bags (3.4 weeks), and widely heterogeneous between tanks. Generalized estimating equations models showed that bioassay larval mortality was strongly affected by water type and type of temephos application depending on water type. Water type and water turnover were highly significantly associated. Tanks filled with piped water had high turnover rates and short-lasting residual effects, whereas tanks filled with rain water showed the opposite pattern. On average, larval infestations reappeared nine weeks post-treatment and seven weeks after estimated loss of residuality. Conclusions Temephos residuality in the field was much shorter and more variable than expected. The main factor limiting temephos residuality was fast water turnover, caused by householders' practice of refilling tanks overnight to counteract the intermittence of the local water supply. Limited field residuality of temephos accounts in part for the inability of the larval control program to further reduce infestation levels with a treatment cycle period of 3 or 4 months. PMID:21445334

Simultaneous determination of tylosin and josamycin residues in muscles, liver, eggs and milk by MLC with a monolithic column and time-programmed UV detection: application to baby food and formulae

PubMed Central

2014-01-01

Background Tylosin and Josamycin are macrolide antibiotics. They are used in the treatment of pneumonia, arthritis and mastitis in cattle, and mycoplasma infections in poultry. The incorrect use of antibiotics has lead to the presence of antibiotic residues in foods. The residues cause toxic effects on consumers. Results A simple and sensitive method was optimized and validated for the analysis of tylosin and josamycin residues in food samples. Analytical separation was performed in less than 10 min using a RP C18 monolithic column with time-programmed UV detection at 287 nm and 232 nm and a micellar solution of 0.17 M sodium dodecyl sulphate, 14% methanol and 0.3% triethylamine in 0.02 M phosphoric acid buffered at pH 4 as the mobile phase. The method was fully validated in accordance with ICH guidelines. The micellar method was successfully applied to quantitatively determine tylosin and josamycin residues in spiked chicken muscles, chicken liver, bovine muscles, liver, milk and eggs. It was also extended to the determination of tylosin and josamycin residues in chicken-based baby food and baby formulae. The compounds were separated by a monolithic column which, on account of its particular structure, could bear higher flow rates than usually found for this kind of analysis. High extraction efficiency for tylosin and josamycin was obtained without matrix interference in the extraction process and in the subsequent chromatographic determination. No organic solvent was used during the pretreatment step. Hence, it is considered an interesting technique for “green” chemistry. Conclusion The proposed method was validated and successfully applied for the determination of tylosin and josamycin residues in spiked chicken muscles, chicken liver, bovine muscles, liver, milk and eggs. It was also extended to the determination of tylosin and josamycin residues in chicken-based baby food and baby formulae. PMID:24976860

Multiclass screening of >200 pharmaceutical and other residues in aquatic foods by ultrahigh-performance liquid chromatography-quadrupole-Orbitrap mass spectrometry.

PubMed

Kong, Cong; Wang, Yang; Huang, Yuanfei; Yu, Huijuan

2018-05-11

A quick screening method of more than 200 pharmaceutical and other residues in aquatic foods based on ultrahigh-performance liquid chromatography-quadrupole-Orbitrap mass spectrometry (UHPLC-Q/Orbitrap MS) was established. In this method, after the addition of 200 μL of 1 M EDTA-Na 2 , 2 g of each sample homogenate was extracted successively with 10 mL of acetonitrile and 10 mL of ethyl acetate. The extracts were combined, dried under nitrogen flow, and redissolved in 0.1% formic acid in acetonitrile/water (4:6, v/v) for analysis. The prepared samples were analyzed by UHPLC- Q/Orbitrap MS system in Full MS/ddMS 2 (full-scan data-dependent MS/MS) mode. Compound identification was performed through comparison of the sample data with the database for standard chemicals, including the retention time, precursor ion, product ions, and isotope pattern for all 206 compounds. Five different aquatic food matrices (carp, shrimp, crab, eel, and mussel) spiked with the analytes at 1, 10, and 50 ng/g were evaluated to assess recoveries, precision, matrix effects, stability, and detection limits using the method. UHPLC analyses required 25 min, and 178-200 analytes met identification criteria at 50 ng/g depending on the matrix. Furthermore, practical application of this method for real samples displayed strong screening capability. Graphical abstract A quick screening method of >200 pharmaceutical and other residues in aquatic foods based on ultrahighperformance liquid chromatography-quadrupole-Orbitrap mass spectrometer was established. Fivedifferent aquatic food matrices, including carp, shrimp, crab, eel and mussel, were studied to evaluatescreen limit at 1, 10 and 50 μg·kg-1 level. Results suggest the high reliability, high time-efficiency and goodsimplicity of the method.

Assessment of consumer exposure related to improper use of pesticides in the region of southeastern Poland.

PubMed

Szpyrka, Ewa

2015-01-01

Plant protection products are widely used throughout the world in order to prevent a reduction in yield. Although the protection of plants brings many benefits, pesticides are toxic to the environment and to humans. To protect human health, pesticide residue risk assessment should be carried out. The aim of the study was to assess acute risk related to the improper use of pesticides. In 2010-2013, 878 crop samples: 382 fruits, 399 vegetables, 82 cereals and their products, 11 herbs and 4 seeds were tested. Pesticide residues were found in 240 samples (27.3%). Pesticide residues were found most frequently in: fruits (41.6% fruit samples), seed (25.0%), vegetables (19.3%) and herbs (9.1%), and least frequently in cereals and their products (2.4%). Improper pesticide use was determined for 49 samples, mainly for vegetables (24 samples) and fruits (22). Most irregularities associated with the use of plant protection products involved application of a substance not recommended for a given crop (36 samples). In nine samples, applications of plant protection products that were withdrawn from the market were found, and in seven samples, violations of maximum residue levels were determined. Despite there being cases of improper use of plant protection products, no hazard to consumer health was determined. The highest values of short-term exposure were obtained in the case of consumption of blackcurrants with iprodione-a substance not recommended in Poland for protection of blackcurrants (4.3% acceptable daily intake (ADI), adults; 6.8% ADI, children). Since potential consumer risk caused by pesticide residues could not be ruled out, inspections should be carried out continuously.

Optimization of the Mechanical Properties and Residual Stresses in 2024 Aluminum Alloy Through Heat Treatment

NASA Astrophysics Data System (ADS)

Araghchi, M.; Mansouri, H.; Vafaei, R.; Guo, Y.

2018-05-01

Residual stresses induced during quenching of aluminum alloys cause dimensional instability and distortion. In this study, the effects of different concentrations of polyalkylene glycol (PAG) quenchants on residual stresses and mechanical properties of 2024 aluminum alloy were investigated. Surface residual stresses were measured by using hole-drilling strain-gauge method. Also, mechanical properties and microstructure of the heat-treated samples were analyzed using hardness measurements, tensile tests, and transmission electron microscopy. Results showed that quenching into a 15% polymeric solution and aging at 190 °C for 12 h cause 50% reduction in residual stress as compared with quenching in water at 20 °C and naturally aging. Moreover, tensile strength decreased by 104 MPa ( 20%) in compared with the T6 sample.

Effect of Multi-Pass Ultrasonic Surface Rolling on the Mechanical and Fatigue Properties of HIP Ti-6Al-4V Alloy

PubMed Central

Li, Gang; Qu, Shengguan; Xie, Mingxin; Ren, Zhaojun; Li, Xiaoqiang

2017-01-01

The main purpose of this paper was to investigate the effect of a surface plastic deformation layer introduced by multi-pass ultrasonic surface rolling (MUSR) on the mechanical and fatigue properties of HIP Ti-6Al-4V alloys. Some microscopic analysis methods (SEM, TEM and XRD) were used to characterize the modified microstructure in the material surface layer. The results indicated that the material surface layer experienced a certain extent plastic deformation, accompanied by some dense dislocations and twin generation. Moreover, surface microhardness, residual stress and roughness values of samples treated by MUSR were also greatly improved compared with that of untreated samples. Surface microhardness and compressive residual stress were increased to 435 HV and −1173 MPa, respectively. The minimum surface roughness was reduced to 0.13 μm. The maximum depth of the surface hardening layer was about 55 μm. However, the practical influence depth was about 450 μm judging from the tensile and fatigue fracture surfaces. The ultimate tensile strength of the MUSR-treated sample increased to 990 MPa from the initial 963 MPa. The fatigue strength of the MUSR-treated sample was increased by about 25% on the base of 107 cycles, and the lifetime was prolonged from two times to two orders of magnitude at the applied stress amplitudes of 650–560 MPa. The improved mechanical and fatigue properties of MUSR-treated samples should be attributed to the combined effects of the increased microhardness and compressive residual stress, low surface roughness, grain refinement and micro-pore healing in the material surface-modified layer. PMID:28772494

Standardization and performance evaluation of "modified" and "ultrasensitive" versions of the Abbott RealTime HIV-1 assay, adapted to quantify minimal residual viremia.

PubMed

Amendola, Alessandra; Bloisi, Maria; Marsella, Patrizia; Sabatini, Rosella; Bibbò, Angela; Angeletti, Claudio; Capobianchi, Maria Rosaria

2011-09-01

Numerous studies investigating clinical significance of HIV-1 minimal residual viremia (MRV) suggest potential utility of assays more sensitive than those routinely used to monitor viral suppression. However currently available methods, based on different technologies, show great variation in detection limit and input plasma volume, and generally suffer from lack of standardization. In order to establish new tools suitable for routine quantification of minimal residual viremia in patients under virological suppression, some modifications were introduced into standard procedure of the Abbott RealTime HIV-1 assay leading to a "modified" and an "ultrasensitive" protocols. The following modifications were introduced: calibration curve extended towards low HIV-1 RNA concentration; 4 fold increased sample volume by concentrating starting material; reduced volume of internal control; adoption of "open-mode" software for quantification. Analytical performances were evaluated using the HIV-1 RNA Working Reagent 1 for NAT assays (NIBSC). Both tests were applied to clinical samples from virologically suppressed patients. The "modified" and the "ultrasensitive" configurations of the assay reached a limit of detection of 18.8 (95% CI: 11.1-51.0 cp/mL) and 4.8 cp/mL (95% CI: 2.6-9.1 cp/mL), respectively, with high precision and accuracy. In clinical samples from virologically suppressed patients, "modified" and "ultrasensitive" protocols allowed to detect and quantify HIV RNA in 12.7% and 46.6%, respectively, of samples resulted "not-detectable", and in 70.0% and 69.5%, respectively, of samples "detected <40 cp/mL" in the standard assay. The "modified" and "ultrasensitive" assays are precise and accurate, and easily adoptable in routine diagnostic laboratories for measuring MRV. Copyright © 2011 Elsevier B.V. All rights reserved.

Numerical simulation of electromagnetic surface treatment

NASA Astrophysics Data System (ADS)

Sonde, Emmanuel; Chaise, Thibaut; Nelias, Daniel; Robin, Vincent

2018-01-01

Surface treatment methods, such as shot peening or laser shock peening, are generally used to introduce superficial compressive residual stresses in mechanical parts. These processes are carried out during the manufacturing steps or for the purpose of repairing. The compressive residual stresses prevent the initiation and growth of cracks and thus improve the fatigue life of mechanical components. Electromagnetic pulse peening (EMP) is an innovative process that could be used to introduce compressive residual stresses in conductive materials. It acts by generating a high transient electromagnetic field near the working surface. In this paper, the EMP process is presented and a sequentially coupled electromagnetic and mechanical model is developed for its simulation. This 2D axisymmetric model is set up with the commercial finite element software SYSWELD. After description and validation, the numerical model is used to simulate a case of introducing residual stresses of compression in a nickel-based alloy 690 thick sample, by the means of electromagnetic pulses. The results are presented in terms of effective plastic strain and residual mean stress. The influence of the process parameters, such as current intensity and frequency, on the results is analyzed. Finally, the predictability of the process is shown by several correlation studies.

Investigation of enrofloxacin residues in broiler tissues using ELISA and LC-MS/MS.

PubMed

Panzenhagen, Pedro Henrique N; Aguiar, Waldemir S; Gouvêa, Raquel; de Oliveira, Andréa M G; Barreto, Fabiano; Pereira, Virgínia L A; Aquino, Maria Helena C

2016-01-01

This study investigated the efficiency of an enrofloxacin ELISA test kit to detect the presence of enrofloxacin residues in broiler tissues compared with LC-MS/MS. Broiler tissues from 72 samples consisting of 60 breast muscle, six pools of livers (500 g each) and six pools of kidneys (500 g each) were obtained from six different slaughterhouses. Breast muscle from 10 carcasses and pools of livers and kidneys from approximately 200 carcasses of the same flock were collected from each slaughterhouse. ELISA and HPLC were used to identify and quantify the contamination of the samples with enrofloxacin. A total of 72% of the analysed samples contained enrofloxacin residues detected by the ELISA and 22.2% were detected by LC-MS/MS. The mean values of enrofloxacin contamination found in chicken breast by ELISA and HPLC were 8.63 and 12.25 μg kg(-1), respectively. None of the samples exceeded the maximum limit of 100 μg kg(-1) by both methods set by the European Union as well as the Brazilian Agriculture Ministry. All positive samples for enrofloxacin residues detected by LC-MS/MS were also positive by ELISA. These data confirm the efficiency of the ELISA test, and suggest its use as a screening method for enrofloxacin residues in poultry tissues due to its quick results, low price and ease of applicability.

Whole Protein Native Fitness Potentials

NASA Astrophysics Data System (ADS)

Faraggi, Eshel; Kloczkowski, Andrzej

2013-03-01

Protein structure prediction can be separated into two tasks: sample the configuration space of the protein chain, and assign a fitness between these hypothetical models and the native structure of the protein. One of the more promising developments in this area is that of knowledge based energy functions. However, standard approaches using pair-wise interactions have shown shortcomings demonstrated by the superiority of multi-body-potentials. These shortcomings are due to residue pair-wise interaction being dependent on other residues along the chain. We developed a method that uses whole protein information filtered through machine learners to score protein models based on their likeness to native structures. For all models we calculated parameters associated with the distance to the solvent and with distances between residues. These parameters, in addition to energy estimates obtained by using a four-body-potential, DFIRE, and RWPlus were used as training for machine learners to predict the fitness of the models. Testing on CASP 9 targets showed that our method is superior to DFIRE, RWPlus, and the four-body potential, which are considered standards in the field.

Rapid analysis of the chemical composition of agricultural fibers using near infrared spectroscopy and pyrolysis molecular beam mass spectrometry

Treesearch

Stephen S. Kelley; Roger M. Rowell; Mark Davis; Cheryl K. Jurich; Rebecca Ibach

2004-01-01

The chemical composition of a variety of agricultural biomass samples was analyzed with near infrared spectroscopy and pyrolysis molecular beam mass spectroscopy. These samples were selected from a wide array of agricultural residue samples and included residues that had been subjected to a variety of di2erent treatments including solvent extractions and chemical...

Determination of acaricide residues in saudi arabian honey and beeswax using solid phase extraction and gas chromatography.

PubMed

Kamel, Alaa; Al-Ghamdi, Ahmad

2006-01-01

Determination of acaricide residues of flumethrin, tau-fluvalinate, coumaphos, and amitraz in honey and beeswax was carried out using a rapid extraction method utilizing C-18 SPE cartridges and an analytical method utilizing GC with ECD, NPD, and MSD detectors for the four acaricides. Recovery percentages from the extraction method ranged from 90-102%, while the minimum detection levels ranged from 0.01-0.05 mg/kg for the acaricides. Nine of the 21 analyzed samples were found to be contaminated with the acaricides tau-fluvalinate and coumaphos. Neither flumethrin nor amitraz was detected in any of the honey or wax samples. Coumaphos was found only in honey samples in which two samples exceeded the tolerance levels set by EPA and EC regulations. It has not been detected in beeswax. Five honey samples and eight beeswax samples were found to be contaminated with tau-fluvalinate. One of the wax samples was contaminated with a relatively high residue of tau-fluvalinate and contained above 10 mg/kg.

Influence of organic waste and residue mud additions on chemical, physical and microbial properties of bauxite residue sand.

PubMed

Jones, Benjamin E H; Haynes, Richard J; Phillips, Ian R

2011-02-01

In an alumina refinery, bauxite ore is treated with sodium hydroxide at high temperatures and pressures and for every tone of alumina produced, about 2 tones of alkaline, saline bauxite processing waste is also produced. At Alcoa, a dry stacking system of disposal is used, and it is the sand fraction of the processing waste that is rehabilitated. There is little information available regarding the most appropriate amendments to add to the processing sand to aid in revegetation. The purpose of this study was to investigate how the addition of organic wastes (biosolids and poultry manure), in the presence or absence of added residue mud, would affect the properties of the residue sand and its suitability for revegetation. Samples of freshly deposited residue sand were collected from Alcoa's Kwinana refinery. Samples were treated with phosphogypsum (2% v/v), incubated, and leached. A laboratory experiment was then set up in which the two organic wastes were applied at 0 or the equivalent to 60 tones ha(-1) in combination with residue mud added at rates of 0%, 10% and 20% v/v. Samples were incubated for 8 weeks, after which, key chemical, physical and microbial properties of the residue sand were measured along with seed germination. Additions of residue mud increased exchangeable Na(+), ESP and the pH, and HCO (3) (-) and Na(+) concentrations in saturation paste extracts. Additions of biosolids and poultry manure increased concentrations of extractable P, NH (4) (+) , K, Mg, Cu, Zn, Mn and Fe. Addition of residue mud, in combination with organic wastes, caused a marked decrease in macroporosity and a concomitant increase in mesoporosity, available water holding capacity and the quantity of water held at field capacity. With increasing residue mud additions, the percentage of sample present as sand particles (<1 mm diameter) decreased, and the percentage present in aggregated form (>2 mm diameter) increased; greatest aggregation occurred where a combination of residue mud and poultry manure were added. Stability of aggregates, as measured by wet sieving, was greatest where poultry manure was applied. Although total organic C and soluble organic C were greater in biosolids than poultry manure treatments, the reverse was the case for microbial biomass C and basal respiration. In the biosolids and poultry manure treatments, increasing residue mud additions tended to increase soluble C, microbial biomass C and basal respiration. Germination index of watercress was highest in control samples and reduced by additions of biosolids and poultry manure which was attributed to the high EC and possibly high extractable P and NH (4) (+) . The concurrent addition of residue mud and organic wastes can improve chemical, microbial and particularly physical properties of residue sand. Future research should include neutralisation of the mud (e.g. with gypsum) and subsequent leaching to remove salts originating from both the mud and organic wastes.

Variance partitioning of stream diatom, fish, and invertebrate indicators of biological condition

USGS Publications Warehouse

Zuellig, Robert E.; Carlisle, Daren M.; Meador, Michael R.; Potapova, Marina

2012-01-01

Stream indicators used to make assessments of biological condition are influenced by many possible sources of variability. To examine this issue, we used multiple-year and multiple-reach diatom, fish, and invertebrate data collected from 20 least-disturbed and 46 developed stream segments between 1993 and 2004 as part of the US Geological Survey National Water Quality Assessment Program. We used a variance-component model to summarize the relative and absolute magnitude of 4 variance components (among-site, among-year, site × year interaction, and residual) in indicator values (observed/expected ratio [O/E] and regional multimetric indices [MMI]) among assemblages and between basin types (least-disturbed and developed). We used multiple-reach samples to evaluate discordance in site assessments of biological condition caused by sampling variability. Overall, patterns in variance partitioning were similar among assemblages and basin types with one exception. Among-site variance dominated the relative contribution to the total variance (64–80% of total variance), residual variance (sampling variance) accounted for more variability (8–26%) than interaction variance (5–12%), and among-year variance was always negligible (0–0.2%). The exception to this general pattern was for invertebrates at least-disturbed sites where variability in O/E indicators was partitioned between among-site and residual (sampling) variance (among-site  =  36%, residual  =  64%). This pattern was not observed for fish and diatom indicators (O/E and regional MMI). We suspect that unexplained sampling variability is what largely remained after the invertebrate indicators (O/E predictive models) had accounted for environmental differences among least-disturbed sites. The influence of sampling variability on discordance of within-site assessments was assemblage or basin-type specific. Discordance among assessments was nearly 2× greater in developed basins (29–31%) than in least-disturbed sites (15–16%) for invertebrates and diatoms, whereas discordance among assessments based on fish did not differ between basin types (least-disturbed  =  16%, developed  =  17%). Assessments made using invertebrate and diatom indicators from a single reach disagreed with other samples collected within the same stream segment nearly ⅓ of the time in developed basins, compared to ⅙ for all other cases.

MCMC Sampling for a Multilevel Model with Nonindependent Residuals within and between Cluster Units

ERIC Educational Resources Information Center

Browne, William; Goldstein, Harvey

2010-01-01

In this article, we discuss the effect of removing the independence assumptions between the residuals in two-level random effect models. We first consider removing the independence between the Level 2 residuals and instead assume that the vector of all residuals at the cluster level follows a general multivariate normal distribution. We…

Multiresidue screening of milk withheld for sale at dairy farms in central New York State.

PubMed

Pereira, R V; Siler, J D; Bicalho, R C; Warnick, L D

2014-03-01

Many of the drugs commonly used in lactating dairy cows result in residues in the milk, prohibiting its sale for human consumption. Milk withheld for sale because of drug treatment or from cows with high somatic cell counts is commonly called "waste milk." One-third of dairy farms in the United States use waste milk to feed preweaned dairy calves. Limited information is currently available on the effect of this practice on the selection and dissemination of antibiotic-resistant bacteria. Pooled waste milk samples were collected from 34 dairy farms in central New York State with the objective of detecting the presence and quantity of drug residues in these samples. Samples were collected and refrigerated using ice packs and then stored at 4°C upon arrival at the Cornell laboratory (Ithaca, NY). Screening for β-lactam, tetracycline, and sulfonamide residues in the milk was performed using commercial enzyme-linked receptor-binding assay (SNAP) tests (Idexx Laboratories Inc., Westbrook, ME). Samples with a positive SNAP test were selected for screening using a multiresidue liquid chromatography-tandem mass spectrometry (LC-MS/MS) method. The SNAP tests revealed that 75, 14.3, and 7.1% of waste milk samples (n=34) contained β-lactam, tetracycline, and sulfamethazine residues, respectively. Of the samples sent for LC-MS/MS (n=28), half had detectable quantities of drug residues. The most prevalent drugs detected by LC-MS/MS were ceftiofur (39.2%; mean ± SE concentration=0.151 ± 0.042 μg/mL), penicillin G (14.2%; mean ± SE concentration=0.008 ± 0.001 µg/mL), and ampicillin (7.1%; mean ± SE concentration=0.472 ± 0.43 µg/mL). In addition, one sample had detectable concentrations of oxytetracycline and one sample had detectable concentrations of sulfadimethoxine. These results provide insight on drug residues present in waste milk from select farm in upstate New York, and additionally indicate the need for additional studies targeting on-farm treatments that could degrade drug residues present in waste milk and reduce the potential effects on the biosphere from the disposal and use of waste milk as a feed source. Copyright © 2014 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

The influence of solvent processing on polyester bioabsorbable polymers.

PubMed

Manson, Joanne; Dixon, Dorian

2012-01-01

Solvent-based methods are commonly employed for the production of polyester-based samples and coatings in both medical device production and research. The influence of solvent casting and subsequent drying time was studied using thermal analysis, spectroscopy and weight measurement for four grades of 50 : 50 poly(lactic-co-glycolic acid) (PLGA) produced by using chloroform, dichloromethane, and acetone. The results demonstrate that solvent choice and PLGA molecular weight are critical factors in terms of solvent removal rate and maintaining sample integrity, respectively. The protocols widely employed result in high levels of residual solvent and a new protocol is presented together with solutions to commonly encountered problems.

Trends in surface-water quality during implementation of best-management practices in Mill Creek and Muddy Run Basins, Lancaster County, Pennsylvania

USGS Publications Warehouse

Koerkle, Edward H.

2000-01-01

Analyses of water samples collected over a 5-year period (1993-98) in the Mill Creek and Muddy Run Basins during implementation of agricultural best-management practices (BMP’s) indicate statistically significant trends in the concentrations of several nutrient species and in nonfilterable residue (suspended solids). The strongest trends identified were those indicated by a more than 50- percent decrease in the flow-adjusted concentrations of total and dissolved phosphorus and total residue in base flow in the two streams. Analyses of stormflow samples showed a 31-percent decrease in the flow-adjusted concentration of total phosphorus in Mill Creek and a 54-percent decrease in total nonfilterable residue in Muddy Run. A 58-percent increase in the flow-adjusted concentration of total ammonia nitrogen in stormflow was found at Muddy Run.Although the effects of a specific BMP on the indicated trends is uncertain, results of statistical trend tests of the data suggest that stream fencing, possibly in concert with other practices, such as stream crossings for livestock, barnyard runoff control, manure-storage facilities, and rotational grazing, was effective in improving water quality during base flow and probably low to moderate stormflow conditions. Additional improvements in water quality in the Mill Creek and Muddy Run Basins seems likely as the implementation of BMP’s is expected to continue. Thus, the full effect of BMP implementation in the two basins may not be observed for some time.

A gel-based visual immunoassay for non-instrumental detection of chloramphenicol in food samples.

PubMed

Yuan, Meng; Sheng, Wei; Zhang, Yan; Wang, Junping; Yang, Yijin; Zhang, Shuguang; Goryacheva, Irina Yu; Wang, Shuo

2012-11-02

A gel-based non-instrumental immuno-affinity assay was developed for the rapid screening of chloramphenicol (CAP) in food samples with the limit of detection (LOD) of 1 μg L(-1). The immuno-affinity test column (IATC) consisted of a test layer containing anti-CAP antibody coupled gel, and a control layer with anti-HRP antibody coupled gel. Based on the direct competitive immuno-reaction and the horseradish peroxidase enzymatic reaction, the test results could be evaluated visually. Basically, blue color development represented the negative results, while the absence of color development represented the positive results. In this study, CAP spiked samples of raw milk, pasteurized milk, UHT milk, skimmed milk powder, acacia honey, date honey, fish and shrimp were tested. Little or none sample pretreatment was required for this assay. The whole procedure was completed within 10min. In conclusion, the gel-based immuno-affinity test is a simple, rapid, and promising on-site screening method for CAP residues in food samples, with no instrumental requirement. Copyright © 2012 Elsevier B.V. All rights reserved.

Matrix effects in pesticide multi-residue analysis by liquid chromatography-mass spectrometry.

PubMed

Kruve, Anneli; Künnapas, Allan; Herodes, Koit; Leito, Ivo

2008-04-11

Three sample preparation methods: Luke method (AOAC 985.22), QuEChERS (quick, easy, cheap, effective, rugged and safe) and matrix solid-phase dispersion (MSPD) were applied to different fruits and vegetables for analysis of 14 pesticide residues by high-performance liquid chromatography with electrospray ionization-mass spectrometry (HPLC/ESI/MS). Matrix effect, recovery and process efficiency of the sample preparation methods applied to different fruits and vegetables were compared. The Luke method was found to produce least matrix effect. On an average the best recoveries were obtained with the QuEChERS method. MSPD gave unsatisfactory recoveries for some basic pesticide residues. Comparison of matrix effects for different apple varieties showed high variability for some residues. It was demonstrated that the amount of co-extracting compounds that cause ionization suppression of aldicarb depends on the apple variety as well as on the sample preparation method employed.

Influence of fungicide residues on the primary fermentation of young lager beer.

PubMed

Navarro, Simón; Pérez, Gabriel; Navarro, Ginés; Mena, Luis; Vela, Nuria

2007-02-21

The effect of four sterol biosynthesis-inhibiting fungicides added to the pitching wort on the evolution of several organoleptic parameters during the primary fermentation of young lager beer was assessed. Pyrimidine (nuarimol and fenarimol) and triazole (myclobutanil and propiconazole) fungicides were individually supplied to the pitching wort to obtain a concentration of 1 mg/L. A marked influence in the fermentation rate was observed for the samples with propiconazole residues. From the fourth day onward, the fermentation prematurely ceased (stuck fermentation), and therefore, statistical significant differences were found in fermented extract, alcohol content, fermentable carbohydrates, pH, color, and total polyphenol and flavonoid contents of beer. Myclobutanil residues are only influenced in the total polyphenol and flavonoid contents, while differences in the analyzed parameters were not noticeable for the samples containing nuarimol and fenarimol residues in comparison with the blank sample.

Effect of thermal exposure on the residual stress relaxation in a hardened cylindrical sample under creep conditions

NASA Astrophysics Data System (ADS)

Radchenko, V. P.; Saushkin, M. N.; Tsvetkov, V. V.

2016-05-01

This paper describes the effect of thermal exposure (high-temperature exposure) ( T = 675°C) on the residual creep stress relaxation in a surface hardened solid cylindrical sample made of ZhS6UVI alloy. The analysis is carried out with the use of experimental data for residual stresses after micro-shot peening and exposures to temperatures equal to T = 675°C during 50, 150, and 300 h. The paper presents the technique for solving the boundary-value creep problem for the hardened cylindrical sample with the initial stress-strain state under the condition of thermal exposure. The uniaxial experimental creep curves obtained under constant stresses of 500, 530, 570, and 600 MPa are used to construct the models describing the primary and secondary stages of creep. The calculated and experimental data for the longitudinal (axial) tensor components of residual stresses are compared, and their satisfactory agreement is determined.

[Determination of buprofezin, methamidophos, acephate, and triazophos residues in Chinese tea samples by gas chromatography].

PubMed

Zhang, Shuiba; Yi, Jun; Ye, Jianglei; Zheng, Wenhui; Cai, Xueqin; Gong, Zhenbin

2004-03-01

A method has been developed for the simultaneous determination of buprofezin, methamidophos, acephate and triazophos residues in Chinese tea samples. The pesticide residues were extracted from tea samples with a mixture of ethyl acetate and n-hexane (50:50, v/v) at 45 degrees C. The extracts were subsequently treated with a column packed with 40 mg of active carbon by gradient elution with ethyl acetate and n-hexane. Buprofenzin and the three organophosphorus pesticides were analyzed by gas chromatography using a DB-210 capillary column and a nitrogen-phosphorus detector. The recoveries for spiked standards were 73.4%-96.9%. The relative standard deviations were all within 4.63%. The limits of quantitation (3sigma) in the tea samples were about 7.0-12.0 microg/kg.

Estimation of the residual bromine concentration after disinfection of cooling water by statistical evaluation.

PubMed

Megalopoulos, Fivos A; Ochsenkuehn-Petropoulou, Maria T

2015-01-01

A statistical model based on multiple linear regression is developed, to estimate the bromine residual that can be expected after the bromination of cooling water. Make-up water sampled from a power plant in the Greek territory was used for the creation of the various cooling water matrices under investigation. The amount of bromine fed to the circuit, as well as other important operational parameters such as concentration at the cooling tower, temperature, organic load and contact time are taken as the independent variables. It is found that the highest contribution to the model's predictive ability comes from cooling water's organic load concentration, followed by the amount of bromine fed to the circuit, the water's mean temperature, the duration of the bromination period and finally its conductivity. Comparison of the model results with the experimental data confirms its ability to predict residual bromine given specific bromination conditions.

SIMS chemical and isotopic analysis of impact features from LDEF experiments AO187-1 and AO187-2

NASA Technical Reports Server (NTRS)

Stadermann, Frank J.; Amari, Sachiko; Foote, John; Swan, Pat; Walker, Robert M.; Zinner, Ernst

1995-01-01

Previous secondary ion mass spectrometry (SIMS) studies of extended impact features from LDEF capture cell experiment AO187-2 showed that it is possible to distinguish natural and man-made particle impacts based on the chemical composition of projectile residues. The same measurement technique has now been applied to specially prepared gold target impacts from experiment AO187-1 in order to identify the origins of projectiles that left deposits too thin to be analyzed by conventional energy-dispersive x-ray (EDX) spectroscopy. The results indicate that SIMS may be the method of choice for the analysis of impact deposits on a variety of sample surfaces. SIMS was also used to determine the isotopic compositions of impact residues from several natural projectiles. Within the precision of the measurements all analyzed residues show isotopically normal compositions.

Titrimetric and photometric methods for determination of hypochlorite in commercial bleaches.

PubMed

Jonnalagadda, Sreekanth B; Gengan, Prabhashini

2010-01-01

Two methods, simple titration and photometric methods for determination of hypochlorite are developed, based its reaction with hydrogen peroxide and titration of the residual peroxide by acidic permanganate. In the titration method, the residual hydrogen peroxide is estimated by titration with standard permanganate solution to estimate the hypochlorite concentration. The photometric method is devised to measure the concentration of remaining permanganate, after the reaction with residual hydrogen peroxide. It employs 4 ranges of calibration curves to enable the determination of hypochlorite accurately. The new photometric method measures hypochlorite in the range 1.90 x 10(-3) to 1.90 x 10(-2) M, with high accuracy and with low variance. The concentrations of hypochlorite in diverse commercial bleach samples and in seawater which is enriched with hypochlorite were estimated using the proposed method and compared with the arsenite method. The statistical analysis validates the superiority of the proposed method.

Microscopic stress characterisation of functional iron-based alloys by white X-ray microbeam diffraction

NASA Astrophysics Data System (ADS)

Kwon, E. P.; Sato, S.; Fujieda, S.; Shinoda, K.; Kajiwara, K.; Sato, M.; Suzuki, S.

2018-01-01

Microscopic residual stress evolution in an austenite (γ) grain during a shape-memory process in an Fe-Mn-Si-Cr alloy was investigated using the white X-ray microbeam diffraction technique. The stresses were measured on a coarse grain, which had an orientation near <144>, parallel to the tensile loading direction with a high Schmid factor for a martensitic transformation. The magnitude of the residual stresses in a grain of the sample, which was subjected to a 23 % tensile strain and subsequent shape-recovery heating, was found to be very small and comparable to that prior to tensile deformation. Measurements of the recovery strain and microstructural analyses using electron backscatter diffraction suggested that the low residual stresses could be attributed to the significant shape recovery caused by a highly reversible martensitic transformation in the grain with a particular orientation.

Remarks on residual stress measurement by hole-drilling and electronic speckle pattern interferometry.

PubMed

Barile, Claudia; Casavola, Caterina; Pappalettera, Giovanni; Pappalettere, Carmine

2014-01-01

Hole drilling is the most widespread method for measuring residual stress. It is based on the principle that drilling a hole in the material causes a local stress relaxation; the initial residual stress can be calculated by measuring strain in correspondence with each drill depth. Recently optical techniques were introduced to measure strain; in this case, the accuracy of the final results depends, among other factors, on the proper choice of the area of analysis. Deformations are in fact analyzed within an annulus determined by two parameters: the internal and the external radius. In this paper, the influence of the choice of the area of analysis was analysed. A known stress field was introduced on a Ti grade 5 sample and then the stress was measured in correspondence with different values of the internal and the external radius of analysis; results were finally compared with the expected theoretical value.

Remarks on Residual Stress Measurement by Hole-Drilling and Electronic Speckle Pattern Interferometry

PubMed Central

2014-01-01

Hole drilling is the most widespread method for measuring residual stress. It is based on the principle that drilling a hole in the material causes a local stress relaxation; the initial residual stress can be calculated by measuring strain in correspondence with each drill depth. Recently optical techniques were introduced to measure strain; in this case, the accuracy of the final results depends, among other factors, on the proper choice of the area of analysis. Deformations are in fact analyzed within an annulus determined by two parameters: the internal and the external radius. In this paper, the influence of the choice of the area of analysis was analysed. A known stress field was introduced on a Ti grade 5 sample and then the stress was measured in correspondence with different values of the internal and the external radius of analysis; results were finally compared with the expected theoretical value. PMID:25276850

Drug residues in serum of dogs receiving anticancer chemotherapy.

PubMed

Knobloch, A; Mohring, S A I; Eberle, N; Nolte, I; Hamscher, G; Simon, D

2010-01-01

The presence of drug residues in blood samples can represent an occupational hazard. However, studies on cytotoxic drug residues in serum of dogs are lacking in veterinary oncology. To evaluate possible occupational hazards associated with handling of blood samples from dogs receiving oncolytic drugs 7 days after treatment. Twenty-seven client-owned dogs treated for lymphoma or mast cell tumors with vincristine, vinblastine, cyclophosphamide, or doxorubicin. Prospective, observational study. Serum samples were either taken 7 days after administration of vincristine, cyclophosphamide, doxorubicin (lymphoma), and vinblastine (mast cell tumor), or 1-2 days after the last concurrent oral administration of cyclophosphamide (mast cell tumor). Additionally, serum was collected within 5 minutes of treatment. Measurement of drug residues in serum was performed by liquid chromatography tandem mass spectrometry (LC/MS/MS). In 33 samples collected within 5 minute of treatment, the median serum concentrations were vincristine: 37 microg/L (range: 11-87 microg/L), vinblastine: 13 microg/L (range: 13-35 microg/L), cyclophosphamide: 2,484 microg/L (range: 1,209-2,778 microg/L), doxorubicin: 404 microg/L (range: 234-528 microg/L). In 81 serum samples collected 7 days after treatment vinblastine (7 microg/L) was detected in 1 sample, and cyclophosphamide (7 and 9 microg/L) in 2 samples collected 1-2 days after oral administration of cyclophosphamide. Medications were not detected in any of the other samples. Handling of blood samples from dogs receiving oncolytic chemotherapy 7 days after treatment with vincristine, vinblastine, cyclophosphamide, and doxorubicin should not present a health hazard.

High and low frequency unfolded partial least squares regression based on empirical mode decomposition for quantitative analysis of fuel oil samples.

PubMed

Bian, Xihui; Li, Shujuan; Lin, Ligang; Tan, Xiaoyao; Fan, Qingjie; Li, Ming

2016-06-21

Accurate prediction of the model is fundamental to the successful analysis of complex samples. To utilize abundant information embedded over frequency and time domains, a novel regression model is presented for quantitative analysis of hydrocarbon contents in the fuel oil samples. The proposed method named as high and low frequency unfolded PLSR (HLUPLSR), which integrates empirical mode decomposition (EMD) and unfolded strategy with partial least squares regression (PLSR). In the proposed method, the original signals are firstly decomposed into a finite number of intrinsic mode functions (IMFs) and a residue by EMD. Secondly, the former high frequency IMFs are summed as a high frequency matrix and the latter IMFs and residue are summed as a low frequency matrix. Finally, the two matrices are unfolded to an extended matrix in variable dimension, and then the PLSR model is built between the extended matrix and the target values. Coupled with Ultraviolet (UV) spectroscopy, HLUPLSR has been applied to determine hydrocarbon contents of light gas oil and diesel fuels samples. Comparing with single PLSR and other signal processing techniques, the proposed method shows superiority in prediction ability and better model interpretation. Therefore, HLUPLSR method provides a promising tool for quantitative analysis of complex samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Detection of pesticides residues in water samples from organic and conventional paddy fields of Ledang, Johor, Malaysia

NASA Astrophysics Data System (ADS)

Abdullah, Md Pauzi; Othman, Mohamed Rozali; Ishak, Anizan; Nabhan, Khitam Jaber

2016-11-01

Pesticides have been used extensively by the farmers in Malaysia during the last few decades. Sixteen water samples, collected from paddy fields both organic and conventional, from Ledang, Johor, were analyzed to determine the occurrence and distribution of organochlorine (OCPs) and organophosphorus (OPPs) pesticide residues. GC-ECD instrument was used to identify and determine the concentrations of these pesticide residues. Pesticide residues were detected in conventional fields in the range about 0.036-0.508 µg/L higher than detected in organic fields about 0.015-0.428 µg/L. However the level of concentration of pesticide residues in water sample from both paddy fields are in the exceed limit for human consumption, according to European Economic Commission (EEC) (Directive 98/83/EC) at 0.1 µg/L for any pesticide or 0.5 µg/L for total pesticides. The results that the organic plot is still contaminated with pesticides although pesticides were not use at all in plot possibly from historical used as well as from airborne contamination.

microRNA-371a-3p as informative biomarker for the follow-up of testicular germ cell cancer patients.

PubMed

van Agthoven, Ton; Eijkenboom, Wil M H; Looijenga, Leendert H J

2017-08-01

α-fetoprotein (AFP) and human chorionic gonadotropin subunit beta (B-HCG) are informative serum biomarkers for the primary diagnosis and follow-up of testicular germ cell cancer (TGCC) patients. About 20% of TGCC patients with a non-seminoma (NS) and about 80% with a seminoma (SE) are, however, negative for these biomarkers. Embryonic stem cell microRNAs (miRs) may serve as promising alternative serum biomarkers. Here we investigated a retrospective series of serum samples from selected TGCC patients who developed a relapse in time to test the possible additional value of the serum-based ampTSmiR test compared to the conventional serum-based protein biomarkers for follow-up. We investigated 261 retrospective serum samples of six selected fully evaluated TGCC patients with a proven relapse using the ampTSmiR test for miR-371a-3p, miR-373-3p, and miR-367-3p and compared the results to those of the conventional protein biomarkers. At primary diagnosis, elevated serum B-HCG, AFP and LDH levels were found to be informative in 4/6, 3/6 and 3/6 patients, respectively. At primary diagnosis the levels of miR-371a-3p and miR-373-3p were elevated in 4/4, and miR-367-3p in 3/4 patients. For two cases no starting serum sample was available for retrospective miR analysis. Residual disease (overlooked by histopathological examination) was detected in one case by miR-371a-3p only. The miR-371a-3p level was increased in one patient two months before detection of an intracranial metastasis. B-HCG was informative in 3/4 and the ampTSmiR test in 4/4 patients with a relapse or residual disease. None of the biomarkers were informative for the detection of residual mature teratoma. The ampTSmiR test is more sensitive than the conventional TGCC protein biomarkers for the detection of residual disease and relapse, excluding mature teratoma.

Matrix-effect free multi-residue analysis of veterinary drugs in food samples of animal origin by nanoflow liquid chromatography high resolution mass spectrometry.

PubMed

Alcántara-Durán, Jaime; Moreno-González, David; Gilbert-López, Bienvenida; Molina-Díaz, Antonio; García-Reyes, Juan F

2018-04-15

In this work, a sensitive method based on nanoflow liquid chromatography high-resolution mass spectrometry has been developed for the multiresidue determination of veterinary drugs residues in honey, veal muscle, egg and milk. Salting-out supported liquid extraction was employed as sample treatment for milk, veal muscle and egg, while a modified QuEChERS procedure was used in honey. The enhancement of sensitivity provided by the nanoflow LC system also allowed the implementation of high dilution factors as high as 100:1. For all matrices tested, matrix effects were negligible starting from a dilution factor of 100, enabling, thus, the use of external standard calibration instead of matrix-matched calibration of each sample, and the subsequent increase of laboratory throughput. At spiked levels as low as 0.1 or 1 µg kg -1 before the 1:100 dilution, the obtained signals were still significantly higher than the instrumental limit of quantitation (S/N 10). Copyright © 2017 Elsevier Ltd. All rights reserved.

Solid-substrate fermentation of alfalfa for enhanced protein recovery

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bajracharya, R.; Madgett, R.E.

1979-04-01

Solid-substrate fermentations for extraction of protein from pressed alfalfa residues with Aspergillus Sp. QM 9994, Aspergillus niger QM 877, and Rhizopus nigricans QM 387 were conducted in shake flasks. Upon reimbibing and second pressing, total protein recovery from alfalfa was increased from 47.2% for control samples and up to 64.5% for fermented samples. Analysis of juice from fermented samples indicated the presence of cellulase as well as pectinase activities. Dialysis cultures of cellulase-producing fungi showed that total biomass production and solids consumption were much higher than those of a mutant strain lacking the ability to produce cellulase, indicating significant utilizationmore » of cellulosic materials in alfalfa. The biomass yields in the former case ranged from 39-47% based on total solids consumption. Since some of the cellulosic and other carbohydrate constituents in alfalfa may be converted into fungal protein, final alfalfa residues following protein extraction in a commercial process would be less bulky for storage and handling and would be more digestible as a nonruminant animal feed.« less

Nondestructive monitoring damage in composites using scanning laser acoustic microscopy

NASA Technical Reports Server (NTRS)

Wey, A. C.; Kessler, L. W.; Dos Reis, H. L. M.

1992-01-01

Several Nicalon fiber reinforced LAS (lithium alumino-silicate) glass matrix composites were tested to study the relation between the residual strength and the different amounts of damage. The samples were fatigued by four-point cyclic loading at a 5 Hz rate at 500 C for a different number of cycles. 10 MHz scanning laser acoustic microscope (SLAM) images were taken to monitor damage on the samples. Our SLAM results indicate that there were defects already existing throughout the sample before fatigue, and the resultant damage pattern from fatigue could be related to the initial defect distribution in the sample. Finally, the fatigued samples were fractured and the residual strength data could not be explained by the cyclic fatigue alone. Rather, the damage patterns evident in the SLAM images were needed to explain the scatter in the data. The results show that SLAM is useful in nondestructively monitoring damage and estimating residual strength of fatigued ceramic composites.

Applying Incremental Sampling Methodology to Soils Containing Heterogeneously Distributed Metallic Residues to Improve Risk Analysis.

PubMed

Clausen, J L; Georgian, T; Gardner, K H; Douglas, T A

2018-01-01

This study compares conventional grab sampling to incremental sampling methodology (ISM) to characterize metal contamination at a military small-arms-range. Grab sample results had large variances, positively skewed non-normal distributions, extreme outliers, and poor agreement between duplicate samples even when samples were co-located within tens of centimeters of each other. The extreme outliers strongly influenced the grab sample means for the primary contaminants lead (Pb) and antinomy (Sb). In contrast, median and mean metal concentrations were similar for the ISM samples. ISM significantly reduced measurement uncertainty of estimates of the mean, increasing data quality (e.g., for environmental risk assessments) with fewer samples (e.g., decreasing total project costs). Based on Monte Carlo resampling simulations, grab sampling resulted in highly variable means and upper confidence limits of the mean relative to ISM.

Method and apparatus for the evaluation of a depth profile of thermo-mechanical properties of layered and graded materials and coatings

DOEpatents

Finot, M.; Kesler, O.; Suresh, S.

1998-12-08

A technique for determining properties such as Young`s modulus, coefficient of thermal expansion, and residual stress of individual layers within a multi-layered sample is presented. The technique involves preparation of a series of samples, each including one additional layer relative to the preceding sample. By comparison of each sample to a preceding sample, properties of the topmost layer can be determined, and residual stress at any depth in each sample, resulting from deposition of the top layer, can be determined. 11 figs.

Microwave assisted solvent extraction and coupled-column reversed-phase liquid chromatography with UV detection use of an analytical restricted-access-medium column for the efficient multi-residue analysis of acidic pesticides in soils.

PubMed

Hogendoom, E A; Huls, R; Dijkman, E; Hoogerbrugge, R

2001-12-14

A screening method has been developed for the determination of acidic pesticides in various types of soils. Methodology is based on the use of microwave assisted solvent extraction (MASE) for fast and efficient extraction of the analytes from the soils and coupled-column reversed-phase liquid chromatography (LC-LC) with UV detection at 228 nm for the instrumental analysis of uncleaned extracts. Four types of soils, including sand, clay and peat, with a range in organic matter content of 0.3-13% and ten acidic pesticides of different chemical families (bentazone, bromoxynil, metsulfuron-methyl, 2,4-D, MCPA, MCPP, 2,4-DP, 2,4,5-T, 2,4-DB and MCPB) were selected as matrices and analytes, respectively. The method developed included the selection of suitable MASE and LC-LC conditions. The latter consisted of the selection of a 5-microm GFF-II internal surface reversed-phase (ISRP, Pinkerton) analytical column (50 x 4.6 mm, I.D.) as the first column in the RAM-C18 configuration in combination with an optimised linear gradient elution including on-line cleanup of sample extracts and reconditioning of the columns. The method was validated with the analysis of freshly spiked samples and samples with aged residues (120 days). The four types of soils were spiked with the ten acidic pesticides at levels between 20 and 200 microg/kg. Weighted regression of the recovery data showed for most analyte-matrix combinations, including freshly spiked samples and aged residues, that the method provides overall recoveries between 60 and 90% with relative standard deviations of the intra-laboratory reproducibility's between 5 and 25%; LODs were obtained between 5 and 50 microg/kg. Evaluation of the data set with principal component analysis revealed that the parameters (i) increase of organic matter content of the soil samples and (ii) aged residues negatively effect the recovery of the analytes.

Occurrence of agrochemical residues in beeswax samples collected in Italy during 2013-2015.

PubMed

Perugini, Monia; Tulini, Serena M R; Zezza, Daniela; Fenucci, Stefano; Conte, Annamaria; Amorena, Michele

2018-06-01

Considering the importance of honey bees for pollination activity and biodiversity preservation different studies have dealt with the impact of pesticides on honeybee health. Within the hive, beeswax is a matrix of particular interest because most of the chemicals used in agricultural and beekeeping activities can easily accumulate and persist in this matrix long after treatment has ceased, affecting honeybees survival. However, chemical analyses of pesticide residues in beeswax are not mandatory, so there are no residue limits, for beeswax. The present study was carried out with the aim of investigating the beeswax residue pattern in the Italian hives. 178 beeswax samples collected from 2013 to 2015 were analyzed for 247 pesticides. 73.6% of the analyzed samples reported the presence of one or more pesticides. On average every single sample showed a mean of three different pesticides each with a maximum of fourteen compounds, some of which were banned in Europe or not authorized in Italy. The higher frequencies were associated with three acaricides: coumaphos (60.7% of samples), tau-fluvalinate (50%) and chlorphenvinphos (35.4%), but the higher concentrations were associated to pyrethrins and piperonil butoxide. Copyright © 2017 Elsevier B.V. All rights reserved.

Toxic metals and organochlorine pesticides residue in single herbal drugs used in important ayurvedic formulation - 'Dashmoola'.

PubMed

Rai, Vartika; Kakkar, Poonam; Singh, Jyotsna; Misra, Chetna; Kumar, Santosh; Mehrotra, Shanta

2008-08-01

Herbal formulations are getting popularity throughout the world and commercialized extensively for various medicinal properties. WHO has emphasized the need for quality assurance of herbal products, including testing of heavy metals and pesticides residues. 'Dashmoola', a popular herbal formulation, with immunomodulator and febrifugal properties, consists of ten single root drugs. In view of WHO guidelines, single herbal drugs used in 'Dashmoola', were collected from different places of India for testing heavy metals and persistent pesticides residue. Although use of roots in 'Dashmoola' is prescribed in original ayurvedic literature but now many pharmacies use stem in place of roots. Therefore, in the present study both roots and stems were selected for estimation of six heavy metals namely arsenic (As), mercury (Hg), lead (Pb), cadmium (Cd), chromium (Cr) and nickel (Ni). Apart from these, the organochlorine pesticides residue viz. different metabolites of DDT, DDE, isomers of HCH and alpha-endosulfan were checked in total 40 samples of single crude drugs. Heavy metals except Hg, were present in most of the samples. In few samples Pb and Cd concentration were beyond the WHO permissible limits. Although alpha-HCH and gamma-HCH were present in almost all the samples, but other pesticides were not detected in these samples. DDT and DDE were found only in two samples.

Correlated environmental corrections in TOPEX/POSEIDON, with a note on ionospheric accuracy

NASA Technical Reports Server (NTRS)

Zlotnicki, V.

1994-01-01

Estimates of the effectiveness of an altimetric correction, and interpretation of sea level variability as a response to atmospheric forcing, both depend upon assuming that residual errors in altimetric corrections are uncorrelated among themselves and with residual sea level, or knowing the correlations. Not surprisingly, many corrections are highly correlated since they involve atmospheric properties and the ocean surface's response to them. The full corrections (including their geographically varying time mean values), show correlations between electromagnetic bias (mostly the height of wind waves) and either atmospheric pressure or water vapor of -40%, and between atmospheric pressure and water vapor of 28%. In the more commonly used collinear differences (after removal of the geographically varying time mean), atmospheric pressure and wave height show a -30% correlation, atmospheric pressure and water vapor a -10% correlation, both pressure and water vapor a 7% correlation with residual sea level, and a bit surprisingly, ionospheric electron content and wave height a 15% correlation. Only the ocean tide is totally uncorrelated with other corrections or residual sea level. The effectiveness of three ionospheric corrections (TOPEX dual-frequency, a smoothed version of the TOPEX dual-frequency, and Doppler orbitography and radiopositioning integrated by satellite (DORIS) is also evaluated in terms of their reduction in variance of residual sea level. Smooth (90-200 km along-track) versions of the dual-frequency altimeter ionosphere perform best both globally and within 20 deg in latitude from the equator. The noise variance in the 1/s TOPEX inospheric samples is approximately (11 mm) squared, about the same as noise in the DORIS-based correction; however, the latter has its error over scales of order 10(exp 3) km. Within 20 deg of the equator, the DORIS-based correction adds (14 mm) squared to the residual sea level variance.

Residue depletion of tilmicosin in cattle after subcutaneous administration.

PubMed

Jiang, Haiyang; Ding, Shuangyang; Li, Jiancheng; An, Dianjin; Li, Cun; Shen, Jianzhong

2006-07-12

A study of tissue residue depletion of tilmicosin in cattle was conducted after a single subcutaneous injection at the therapeutic level of 10 mg per kg body weight. Eighteen cross cattle were treated with the tilmicosin oil formulation (30%). Three treated animals (two males and one female) were selected randomly to be scarified at 1, 7, 14, 28, and 35 days withdrawal after injection. Samples of the injection site and of muscle, liver, kidney, and fat were collected. Tilmicosin residue concentrations were determined using a high-performance liquid chromatography (HPLC) method with a UV detector at 290 nm. Using a statistical method recommended by the Committee for Veterinary Medical Products of European Medical Evaluation Agency, the withdrawal time of 34 days was established when all tissue residues except samples in the injection site were below the accepted maximum residue limits.

Determination of Multiple Near-Surface Residual Stress Components in Laser Peened Aluminum Alloy via the Contour Method

NASA Astrophysics Data System (ADS)

Toparli, M. Burak; Fitzpatrick, Michael E.; Gungor, Salih

2015-09-01

In this study, residual stress fields, including the near-surface residual stresses, were determined for an Al7050-T7451 sample after laser peening. The contour method was applied to measure one component of the residual stress, and the relaxed stresses on the cut surfaces were then measured by X-ray diffraction. This allowed calculation of the three orthogonal stress components using the superposition principle. The near-surface results were validated with results from incremental hole drilling and conventional X-ray diffraction. The results demonstrate that multiple residual stress components can be determined using a combination of the contour method and another technique. If the measured stress components are congruent with the principal stress axes in the sample, then this allows for determination of the complete stress tensor.

Type Ia supernova Hubble residuals and host-galaxy properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kim, A. G.; Aldering, G.; Aragon, C.

2014-03-20

Kim et al. introduced a new methodology for determining peak-brightness absolute magnitudes of type Ia supernovae from multi-band light curves. We examine the relation between their parameterization of light curves and Hubble residuals, based on photometry synthesized from the Nearby Supernova Factory spectrophotometric time series, with global host-galaxy properties. The K13 Hubble residual step with host mass is 0.013 ± 0.031 mag for a supernova subsample with data coverage corresponding to the K13 training; at <<1σ, the step is not significant and lower than previous measurements. Relaxing the data coverage requirement of the Hubble residual step with the host massmore » is 0.045 ± 0.026 mag for the larger sample; a calculation using the modes of the distributions, less sensitive to outliers, yields a step of 0.019 mag. The analysis of this article uses K13 inferred luminosities, as distinguished from previous works that use magnitude corrections as a function of SALT2 color and stretch parameters: steps at >2σ significance are found in SALT2 Hubble residuals in samples split by the values of their K13 x(1) and x(2) light-curve parameters. x(1) affects the light-curve width and color around peak (similar to the Δm {sub 15} and stretch parameters), and x(2) affects colors, the near-UV light-curve width, and the light-curve decline 20-30 days after peak brightness. The novel light-curve analysis, increased parameter set, and magnitude corrections of K13 may be capturing features of SN Ia diversity arising from progenitor stellar evolution.« less

Residues of 2-hydroxy-3-phenylpyrazine, a degradation product of some β-lactam antibiotics, in environmental water in Vietnam.

PubMed

Sy, Nguyen Van; Harada, Kazuo; Asayama, Megumi; Warisaya, Minae; Dung, Le Hong; Sumimura, Yoshinori; Diep, Khong Thi; Ha, Le Viet; Thang, Nguyen Nam; Hoa, Tran Thi Tuyet; Phu, Tran Minh; Khai, Pham Ngoc; Phuong, Nguyen Thanh; Tuyen, Le Danh; Yamamoto, Yoshimasa; Hirata, Kazumasa

2017-04-01

Antibiotic-resistant bacteria have become a serious problem worldwide, caused in part by the excessive use and discharge of antibiotics into the environment. Ampicillin (ABPC) is a widely used antibiotic. However, this chemical rapidly decomposes in water containing divalent cations like Ca 2+ and Mg 2+ , thus, detection of ABPC in environmental water is difficult. This study was carried out to evaluate the presence of 2-hydroxy-3-phenylpyrazine (HPP), one of the degradation products of ABPC and β-lactam antibiotics with an ABPC substructure, in environmental water. An analytical method for HPP monitoring in environmental water was developed using liquid chromatography/tandem mass spectrometry. The analyte was extracted from water samples and enriched using a solid-phase extraction cartridge. The quantification limit was 1 ng L -1 . The HPP recovery rates from spiked water samples of 25 and 125 ng L -1 were 84.1 and 86.1%, respectively. The method was then used to determine HPP residue levels in 98 environmental water samples from rivers, household ponds, and aquacultural ponds in Vietnam. HPP residues were detected in 60 samples. The HPP detection rates in rivers and household ponds were 42 and 79%, respectively. HPP was not detected in aquacultural ponds. HPP residue concentrations in the samples ranged from 1.3 to 413.3 ng L -1 . The residue levels in rivers flowing through city centres were higher than levels in other sampling locations. The findings of this study suggest that HPP is a promising marker for assessing the discharge of ABPC and β-lactam antibiotics with an ABPC substructure into the environment around sampling sites. Copyright © 2017 Elsevier Ltd. All rights reserved.

Pesticides in persimmons, jujubes and soil from China: Residue levels, risk assessment and relationship between fruits and soils.

PubMed

Liu, Yihua; Li, Shiliang; Ni, Zhanglin; Qu, Minghua; Zhong, Donglian; Ye, Caifen; Tang, Fubin

2016-01-15

Extreme and uncontrolled usage of pesticides produces a number of problems for vegetation and human health. In this study, the existence of organophosphates (OPs), organochlorines (OCs), pyrethroids (PYs) and fungicides (FUs) were investigated in persimmons/jujubes and their planted soils, which were collected from China. One OP (dimethoate), three OCs (DDT, quintozene and aldrin), six PYs (bifenthrin, fenpropathrin, cyhalothrin, cypermethrin, fenvalerate and deltamethrin) and two FUs (triadimefon and buprofezin) were found in 36.4% of persimmons and 70.8% of jujubes, with concentrations from 1.0 μg/kg to 2945.0 μg/kg. The most frequently detected pesticides in the two fruits were fenpropathrin in persimmons and cypermethrin in jujubes, with the detection frequencies of 30.0% and 22.7%, respectively. The residues of 4.5% (persimmon) and 25.0% (jujube) of samples were higher than the maximum residue limits (MRLs) of China. Compared with the fruits, more types of pesticides and higher residues were observed in their planted soils. The most frequently detected pesticides were HCH in persimmon soil and DDT in jujube soil, with the detection frequencies of 10.9% and 12.7%, respectively. For the tested samples, 39.1% of fruit samples and 63.0% of soil samples with multiple residues (containing more than two pesticides) were noted, even up to 8 residues in fruits and 14 residues in soils. Except for cyhalothrin, the other short-term risks for the tested pesticides in the fruits were below 10%, and the highest long-term risk was 14.13% for aldrin and dieldrin. There was no significant health risk for consumers via consumption of the two fruits. Copyright © 2015 Elsevier B.V. All rights reserved.

Organochlorine insecticide residues in the free-tailed bat (Tadarida brasiliensis) at Bracken Cave, Texas

USGS Publications Warehouse

Clark, D.R.; Martin, C.O.; Swineford, D.M.

1975-01-01

Fifty-nine free-tailed bats (Tadarida brasiliensis mexicana ) were collected at Bracken Cave, Texas, and analyzed for organochlorine insecticides and polychlorinated biphenyls (PCBs). Residues of DDE in the brain were greater in 12 young collected from the floor than in 15 young taken from the ceiling, but food deprivation, not higher residues in the brain, apparently caused young to fall....Among 18 pregnant females, residues of DDE and DDT were highest in yearlings. The first lactation by yearlings caused their residue loads to drop sharply. Thereafter, increasing age was accompanied by increasing residues but amounts generally did not exceed those in yearlings.....Residue levels in embryos were a function both of levels in the female parent and degree of embryonic development. Residues accumulated rapidly in nursing young, and lactating females may excrete from 1.3 to 16.2 (mean = 4.3) micrograms of DDE in milk per day. Maximum individual residue loads may be attained toward the end of nursing, and mobilization of these residues during southward migration may subject Bracken Cave free-tails to maximum lifetime residues in the brain....Comparison of our data with residue data for the free-tail population at Eagle Creek Cave (Arizona) in 1970 produced the following conclusions: ( 1) residues of DDE appeared similar in pregnant females, embryos, lactating females, and fallen young for the two populations; (2) residues of DDT and dieldrin appeared greater in pregnant females at Bracken Cave; (3) DDE and DDT occurred at greater levels in guano samples from Bracken Cave. On this basis, the population decline observed at Eagle Creek Cave between 1963 and 1969 does not appear to be related to the residues observed in the 1970 samples taken from that cave.

Application of a luminescent bacterial biosensor for the detection of tetracyclines in routine analysis of poultry muscle samples.

PubMed

Pikkemaat, M G; Rapallini, M L B A; Karp, M T; Elferink, J W A

2010-08-01

Tetracyclines are extensively used in veterinary medicine. For the detection of tetracycline residues in animal products, a broad array of methods is available. Luminescent bacterial biosensors represent an attractive inexpensive, simple and fast method for screening large numbers of samples. A previously developed cell-biosensor method was subjected to an evaluation study using over 300 routine poultry samples and the results were compared with a microbial inhibition test. The cell-biosensor assay yielded many more suspect samples, 10.2% versus 2% with the inhibition test, which all could be confirmed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Only one sample contained a concentration above the maximum residue limit (MRL) of 100 microg kg(-1), while residue levels in most of the suspect samples were very low (<10 microg kg(-1)). The method appeared to be specific and robust. Using an experimental set-up comprising the analysis of a series of three sample dilutions allowed an appropriate cut-off for confirmatory analysis, limiting the number of samples and requiring further analysis to a minimum.

Multi-scale X-ray Microtomography Imaging of Immiscible Fluids After Imbibition

NASA Astrophysics Data System (ADS)

Garing, C.; de Chalendar, J.; Voltolini, M.; Ajo Franklin, J. B.; Benson, S. M.

2015-12-01

A major issue for CO2 storage security is the efficiency and long-term reliability of the trapping mechanisms occurring in the reservoir where CO2 is injected. Residual trapping is one of the key processes for storage security beyond the primary stratigraphic seal. Although classical conceptual models of residual fluid trapping assume that disconnected ganglia are permanently immobilized, multiple mechanisms exist which could allow the remobilization of residually trapped CO2. The aim of this study is to quantify fluid phases saturation, connectivity and morphology after imbibition using x-ray microtomography in order to evaluate potential changes in droplets organization due to differences in capillary pressure between disconnected ganglia. Particular emphasis is placed on the effect of image resolution. Synchrotron-based x-ray microtomographic datasets of air-water spontaneous imbibition were acquired in sintered glass beads and sandstone samples with voxel sizes varying from 0.64 to 4.44 μm. The results show that for both sandstones the residual air phase is homogeneously distributed within the entire pore space and consists of disconnected clusters of multiple sizes and morphologies. The multi-scale analysis of subsamples of few pores and throats imaged at the same location of the sample reveals significant variations in the estimation of connectivity, size and shape of the fluid phases. This is particularly noticeable when comparing the results from the images with voxel sizes above 1 μm with the results from the images acquired with voxel sizes below 1 μm.

Experimental evaluation of coal conversion solid waste residuals. Progress report, August 1-October 31, 1979

DOE Office of Scientific and Technical Information (OSTI.GOV)

Neufeld, R. D.; Bern, J.; Erdogan, H.

1979-11-15

Activities are underway to investigate basic phenomena that would assist demonstration and commercial sized coal conversion facilities in the environmentally acceptable disposal of process solid waste residuals. The approach taken is to consider only those residuals coming from the conversion technology itself, i.e. from gasification, liquefaction, and hot-clean-up steps as well as residuals from the wastewater treatment train. Residuals from the coal mining and coal grinding steps will not be considered in detail since those materials are being handled in some manner in the private sector. Laboratory evalations have been conducted on solid waste samples of fly ash from anmore » existing Capman gasifier. ASTM-A and EPA-EP leaching procedures have been completed on sieved size fractions of the above wastes. Data indicate that smaller size fractions pose greater contamination potential than do larger size particles with a transition zone occurring at particle sizes of about 0.05 inches in diameter. Ames testing of such residuals is reported. Similar studies are under way with samples of H-Coal solid waste residuals.« less

Food residue recycling by swine breeders in a developing economy: a case study in Da Nang, Viet Nam.

PubMed

Kato, Takaaki; Pham, Dung Thi Xuan; Hoang, Hai; Xue, Yonghai; Tran, Quang Van

2012-12-01

This study provides a detailed description of food residue collection by swine breeders in Da Nang, Viet Nam. In January 2011, the study surveyed 30 swine breeders in two villages with respect to locations, methods, prices, quantities, and prospects for food residue collection. The sampled swine breeders regularly visited 55 locations in central Da Nang to collect raw food residue. They then transferred the food residue to their piggeries, boiled it, and fed it to their swine. A regression analysis revealed that the total amount of food residue collected by a farm depends on the number of swine in the farm and the number of collections made per day. Swine breeders in Da Nang were estimated to collect 26.3 metric tons of organic waste per day, which amounted to 4.1% of domestic waste collected by the local government. Among the sampled swine breeders, 93% answered that they would continue using food residue for the next five years. Copyright © 2012 Elsevier Ltd. All rights reserved.

Fermentation process improvement of a Chinese traditional food: soybean residue cake.

PubMed

Yao, Yingzheng; Pan, Siyi; Wang, Kexing; Xu, Xiaoyun

2010-09-01

Fermentation process improvement of soybean residue cake, a Chinese traditional fermented food, and its physicochemical analysis during fermentation were studied. One of the dominant strains in the fermentation was isolated and identified as Mucor racemosus Fresenius. The fermentation process was improved by subsection fermentation. The crude protein content decreased from 19.95 ± 0.03% in the raw soybean residue to 16.85 ± 0.10% in the fermented products, and the formaldehyde nitrogen content increased from 0.068 ± 0.004% to 0.461 ± 0.022% in final fermented cakes. Hardness of samples significantly (P < 0.05) increased whereas springiness, cohesiveness, and resilience significantly (P < 0.05) decreased with increasing fermentation time, respectively. Microstructure observations showed obvious change of the surface of cake samples during the fermentation process. During the soybean processing, it will produce plenty of by-products, and the most part of them is soybean residue. The discarded soybean residue causes economic loss. Fortunately, we can obtain nutritious and delicious fermented soybean residue cakes by fermenting soybean residue as raw material.

Enhancement of high-solids enzymatic hydrolysis of corncob residues by bisulfite pretreatment for biorefinery.

PubMed

Xing, Yang; Bu, Lingxi; Zheng, Tianran; Liu, Shijie; Jiang, Jianxin

2016-12-01

Co-production of glucose, furfural and other green materials based on a lignocellulosic biorefinery is a promising way to realize the commercial application of corncob residues. An effective process was developed for glucose production using low temperature bisulfite pretreatment and high-solids enzymatic hydrolysis. Corncob residues from furfural production (FRs) were pretreated with 0.1g NaHSO 3 /g dry substrate at 100°C for 3h. Lignin was sulfonated and sulfonic groups were produced during pretreatment, which resulted in decreasing the zeta potential of the samples. Compared with raw material, bisulfite pretreatment of FRs increased the glucose yield from 18.6 to 99.45% after 72h hydrolysis at a solids loading of 12.5%. The hydrolysis residues showed a relatively high thermal stability and concentrated high derivatives. Direct pretreatment followed by enzymatic hydrolysis is an environmentally-friendly and economically-feasible method for the production of glucose and high-purity lignin, which could be further converted into high-value products. Copyright © 2016 Elsevier Ltd. All rights reserved.

High-Throughput Analytical Techniques for the Determination of the Residues of 653 Multiclass Pesticides and Chemical Pollutants in Tea, Part VII: A GC-MS, GC-MS/MS, and LC-MS/MS Study of the Degradation Profiles of Pesticide Residues in Green Tea.

PubMed

Chang, Qiao-Ying; Pang, Guo-Fang; Fan, Chun-Lin; Chen, Hui; Yang, Fang; Li, Jie; Wen, Bi-Fang

2016-11-01

GC-MS, GC-tandem MS (MS/MS), and LC-MS/MS were used to mathematically define the degradation profiles of pesticide residues in two field trials. Nineteen pesticides were studied in the first field trial and 11 in the second. The results of the field trials demonstrated that the degradation profiles of pesticide residues in green tea can be described with power functions to successfully estimate the amount of time, following pesticide application, pesticide residues appearing in tea in concentrations at and/or above the maximum residue limit (MRL) decrease to concentrations below the MRL. Stability tests on green tea samples stored at room temperature were conducted to determine whether pesticide-incurred green tea samples prepared according to the method used in the field trials would be suitable for the preparation of reference standards for laboratory-proficiency testing trials. This paper reports the results of a GC-MS, GC-MS/MS, and LC-MS/MS study, as well as the suitability of the samples prepared under these conditions for use as pesticide reference standards in tea analysis.

Supercritical carbon dioxide extraction of 2,4-dichlorophenol from food crop tissues.

PubMed

Thomson, C A; Chesney, D J

1992-04-15

Supercritical fluid extraction with carbon dioxide has been found to be effective for the isolation of residue levels (0.1-1 ppm) of 2,4-dichlorophenol from selected plant tissues. The 2,4-dichlorophenol residues were incompletely extracted with supercritical CO2 alone, since a substantial fraction of the 2,4-dichlorophenol was covalently attached to the plant matrix. An acid pretreatment procedure was developed to partially hydrolyze the plant tissue prior to extraction, releasing the bound 2,4-dichlorophenol residues. Steam distillation showed higher residue levels for field-treated straw samples. This is attributed to the greater degree of hydrolysis inherent in the steam distillation procedure. Supercritical CO2 extraction of field-treated seed samples showed higher levels of 2,4-dichlorophenol residues than did steam distillation. The supercritical fluid extractant was able to solvate 2,4-dichlorophenol residues in the interior of the seed and transport them to the surface for collection. The aqueous medium used in steam distillation was unable to penetrate the hydrophobic seed matrix to the same degree. While the actual extraction time experienced in supercritical fluid extraction was far less than that of steam distillation (45 min vs 6 h, respectively), the total sample preparation time was similar in both methods.

Food safety in Thailand. 3: Pesticide residues detected in mangosteen (Garcinia mangostana L.), queen of fruits.

PubMed

Phopin, Kamonrat; Wanwimolruk, Sompon; Prachayasittikul, Virapong

2017-02-01

For developing countries like Thailand, regulation of pesticide usage exists, but it is not fully enforced. Therefore, pesticide residues in vegetables and fruits have not been well monitored. This study aimed to determine the pesticide residues in mangosteen fruits sold in Thailand. The mangosteen samples (n = 111) were purchased and the contents of 28 pesticides were analysed by GC-MS/MS method. Of the pesticides tested, eight were found in 100% of the mangosteen samples. However, in 97% of these samples, either chlorothalonil, chlorpyrifos, diazinon, dimethoate, metalaxyl or profenofos was detected exceeding their maximum residue limits (MRLs), representing a 97% rate of pesticide detection above the MRL. This rate is much higher than those found in other fruits sold in developed countries. However, this conclusion excludes the fresh Thai mangosteens grown for export, as these are generally cultivated and harvested to GAP standards. Since the edible part of the mangosteen is the pulp, washing the fruits with running water can reduce the risk of pesticide residues contaminating the pulp which would be eaten by the consumer. The findings strongly suggest that routine monitoring of pesticide residues in fruits and vegetables is required to reduce the health risks associated with consuming contaminated food. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

Cellphone-based detection platform for rbST biomarker analysis in milk extracts using a microsphere fluorescence immunoassay.

PubMed

Ludwig, Susann K J; Zhu, Hongying; Phillips, Stephen; Shiledar, Ashutosh; Feng, Steve; Tseng, Derek; van Ginkel, Leendert A; Nielen, Michel W F; Ozcan, Aydogan

2014-11-01

Current contaminant and residue monitoring throughout the food chain is based on sampling, transport, administration, and analysis in specialized control laboratories. This is a highly inefficient and costly process since typically more than 99% of the samples are found to be compliant. On-site simplified prescreening may provide a scenario in which only samples that are suspect are transported and further processed. Such a prescreening can be performed using a small attachment on a cellphone. To this end, a cellphone-based imaging platform for a microsphere fluorescence immunoassay that detects the presence of anti-recombinant bovine somatotropin (rbST) antibodies in milk extracts was developed. RbST administration to cows increases their milk production, but is illegal in the EU and a public health concern in the USA. The cellphone monitors the presence of anti-rbST antibodies (rbST biomarker), which are endogenously produced upon administration of rbST and excreted in milk. The rbST biomarker present in milk extracts was captured by rbST covalently coupled to paramagnetic microspheres and labeled by quantum dot (QD)-coupled detection antibodies. The emitted fluorescence light from these captured QDs was then imaged using the cellphone camera. Additionally, a dark-field image was taken in which all microspheres present were visible. The fluorescence and dark-field microimages were analyzed using a custom-developed Android application running on the same cellphone. With this setup, the microsphere fluorescence immunoassay and cellphone-based detection were successfully applied to milk sample extracts from rbST-treated and untreated cows. An 80% true-positive rate and 95% true-negative rate were achieved using this setup. Next, the cellphone-based detection platform was benchmarked against a newly developed planar imaging array alternative and found to be equally performing versus the much more sophisticated alternative. Using cellphone-based on-site analysis in future residue monitoring can limit the number of samples for laboratory analysis already at an early stage. Therewith, the entire monitoring process can become much more efficient and economical.

Role of Sample Processing Strategies at the European Union National Reference Laboratories (NRLs) Concerning the Analysis of Pesticide Residues.

PubMed

Hajeb, Parvaneh; Herrmann, Susan S; Poulsen, Mette E

2017-07-19

The guidance document SANTE 11945/2015 recommends that cereal samples be milled to a particle size preferably smaller than 1.0 mm and that extensive heating of the samples should be avoided. The aim of the present study was therefore to investigate the differences in milling procedures, obtained particle size distributions, and the resulting pesticide residue recovery when cereal samples were milled at the European Union National Reference Laboratories (NRLs) with their routine milling procedures. A total of 23 NRLs participated in the study. The oat and rye samples milled by each NRL were sent to the European Union Reference Laboratory on Cereals and Feedingstuff (EURL) for the determination of the particle size distribution and pesticide residue recovery. The results showed that the NRLs used several different brands and types of mills. Large variations in the particle size distributions and pesticide extraction efficiencies were observed even between samples milled by the same type of mill.

Organochlorine insecticide residues in soil and earthworms in the Delhi area, India, August-October 1974

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yadav, D.V.; Mittal, P.K.; Agarwal, H.C.

1981-09-01

DDT residues in soil and earthworms from 50 sites in Delhi were monitored. DDT was detected in all but two samples each of soil and earthworms. Among DDT residues, p,p'-DDE was most common and was found in 48 samples each of soil and earthworms; p,p'-DDT was detected in only 43 soil samples and 46 earthworm samples. p,p'-TDE and o,p'-DDT were also present in smaller concentrations in 29 and 15 soil samples and in 43 and 25 earthworm samples, respectively. Maximum total DDT concentration of 2.6 ppm was detected in the soil from Durga Nagar in the vicinity of a DDTmore » factory. The highest concentration of 37.7 ppm total DDT in earthworms was also obtained from the same site. The maximum concentration factor found in the earthworms was 551. The total DDT concentration in the earthworms and soil showed significant correlation.« less

Comparison of the Organic Composition of Cometary Samples with Residues Formed from the UV Irradiation of Astrophysical Ice Analogs

NASA Technical Reports Server (NTRS)

Milam, S. N.; Nuevo, M.; Sandford, S. A.; Cody, G. D.; Kilcoyne, A. L. D.; Stroud, R. M.; DeGregorio, B. T.

2010-01-01

The NASA Stardust mission successfully collected material from Comet 81P/Wild 2 [1], including authentic cometary grains [2]. X-ray absorption near-edge structure (XANES) spectroscopy analysis of these samples indicates the presence of oxygen-rich and nitrogen-rich organic materials, which contain a broad variety of functional groups (carbonyls, C=C bonds, aliphatic chains, amines, arnides, etc.) [3]. One component of these organics appears to contain very little aromatic carbon and bears some similarity to the organic residues produced by the irradiation of ices of interstellar/cometary composition, Stardust samples were also recently shown to contain glycine, the smallest biological amino acid [4]. Organic residues produced froth the UV irradiation of astrophysical ice analogs are already known to contain a large suite of organic molecules including amino acids [5-7], amphiphilic compounds (fatty acids) [8], and other complex species. This work presents a comparison between XANES spectra measured from organic residues formed in the laboratory with similar data of cometary samples collected by the Stardust mission

A comprehensive study of sampling-based optimum signal detection in concentration-encoded molecular communication.

PubMed

Mahfuz, Mohammad U; Makrakis, Dimitrios; Mouftah, Hussein T

2014-09-01

In this paper, a comprehensive analysis of the sampling-based optimum signal detection in ideal (i.e., free) diffusion-based concentration-encoded molecular communication (CEMC) system has been presented. A generalized amplitude-shift keying (ASK)-based CEMC system has been considered in diffusion-based noise and intersymbol interference (ISI) conditions. Information is encoded by modulating the amplitude of the transmission rate of information molecules at the TN. The critical issues involved in the sampling-based receiver thus developed are addressed in detail, and its performance in terms of the number of samples per symbol, communication range, and transmission data rate is evaluated. ISI produced by the residual molecules deteriorates the performance of the CEMC system significantly, which further deteriorates when the communication range and/or the transmission data rate increase(s). In addition, the performance of the optimum receiver depends on the receiver's ability to compute the ISI accurately, thus providing a trade-off between receiver complexity and achievable bit error rate (BER). Exact and approximate detection performances have been derived. Finally, it is found that the sampling-based signal detection scheme thus developed can be applied to both binary and multilevel (M-ary) ASK-based CEMC systems, although M-ary systems suffer more from higher BER.

Determination of pesticide residues in fruit-based soft drinks.

PubMed

García-Reyes, Juan F; Gilbert-López, Bienvenida; Molina-Díaz, Antonio; Fernández-Alba, Amadeo R

2008-12-01

Here we report the first worldwide reconnaissance study of the presence and occurrence of pesticides in fruit-based soft drinks. While there are strict regulations and exhaustive controls for pesticides in fruits, vegetables, and drinking water, scarce attention has been paid to highly consumed derivate products, which may contain these commodities as ingredients. In the case of the fruit-based soft drinks industry, there are no clear regulations, relating to pesticides, which address them, even when there is significant consumption in vulnerable groups such as children. In this work, we have developed a screening method to search automatically for up to 100 pesticides in fruit-based soft drinks extracts based on the application of liquid chromatography-electrospray time-of-flight mass spectrometry (LC-TOF MS). The sample extracts injected were obtained by a preliminary sample treatment step based on solid-phase extraction using hydrophilic-lipophilic balanced polymer-based reverse phase cartridges and methanol as eluting solvent. Subsequent identification, confirmation, and quantitation were carried out by LC-TOF MS analysis: the confirmation of the target species was based on retention time matching and accurate mass measurements of protonated molecules ([M + H]+) and fragment ions (obtaining accuracy errors typically lower than 2 ppm). With the proposed method, we measured over 100 fruit-based soft drink samples, purchased from 15 different countries from companies with brands distributed worldwide and found relatively large concentration levels of pesticides in most of the samples analyzed. The concentration levels detected were of the micrograms per liter level, low when considering the European maximum residue levels (MRLs) set for fruits but very high (i.e., 300 times) when considering the MRLs for drinking or bottled water. The detected pesticides (carbendazim, thiabendazole, imazalil and its main degradate, prochloraz and its main degradate, malathion, and iprodione) are mainly those applied to crops in the final stages of production (postharvest treatment), some of them contain chlorine atoms in their structures. Therefore, steps should be taken with the aim of removing any traces of pesticides in these products, in order to avoid this source of pesticide exposure on the consumer, particularly on vulnerable groups with higher exposure, such as children.

Development and Validation of a Lateral Flow Immunoassay Test Kit for Dual Detection of Casein and β-Lactoglobulin Residues.

PubMed

Masiri, Jongkit; Barrios-Lopez, Brianda; Benoit, Lora; Tamayo, Joshua; Day, Jeffrey; Nadala, Cesar; Sung, Shao-Lei; Samadpour, Mansour

2016-03-01

Allergies to cow's milk are very common and can present as life-threatening anaphylaxis. Consequently, food labeling legislation mandates that foods containing milk residues, including casein and/or β-lactoglobulin, provide an indication of such on the product label. Because contamination with either component independent of the other can occur during food manufacturing, effective allergen management measures for containment of milk residues necessitates the use of dual screening methods. To assist the food industry in improving food safety practices, we have developed a rapid lateral flow immunoassay test kit that reliably reports both residues down to 0.01 μg per swab and 0.1 ppm of protein for foods. The assay utilizes both sandwich and competitive format test lines and is specific for bovine milk residues. Selectivity testing using a panel of matrices with potentially interfering substances, including commonly used sanitizing agents, indicated reduction in the limit of detection by one-to fourfold. With food, residues were easily detected in all cow's milk-based foods tested, but goat and sheep milk residues were not detected. Specificity analysis revealed no cross-reactivity with common commodities, with the exception of kidney beans when present at high concentrations (> 1%). The development of a highly sensitive and rapid test method capable of detecting trace amounts of casein and/or β-lactoglobulin should aid food manufacturers and regulatory agencies in monitoring for milk allergens in environmental and food samples.

A systematic strategy for the identification and determination of pharmaceuticals in environment using advanced LC-MS tools: application to ground water samples.

PubMed

Jindal, Kriti; Narayanam, Mallikarjun; Singh, Saranjit

2015-04-10

In the present study, a novel analytical strategy was employed to study the occurrence of 40 drug residues belonging to different medicinal classes, e.g., antibiotics, β blockers, NSAIDs, antidiabetics, proton pump inhibitors, H2 receptor antagonists, antihypertensives, antihyperlipidemics, etc. in ground water samples collected from villages adjoining to S.A.S. Nagar, Punjab, India. The drug residues were extracted from the samples using solid-phase extraction, and LC-ESI-HRMS and LC-ESI-MS/MS were used for identification and quantitation of the analytes. Initially, qualifier and quantifier MRM transitions were classified for 40 targeted drugs, followed by development of LC-MS methods for the separation of all the drugs, which were divided into three categories to curtail overlapping of peaks. Overall identification was done through matching of retention times and MRM transitions; matching of intensity ratio of qualifier to quantifier transitions; comparison of base peak MS/MS profiles; and evaluation of isotopic abundances (wherever applicable). Final confirmation was carried out through comparison of accurate masses obtained from HRMS studies for both standard and targeted analytes in the samples. The application of the strategy allowed removal of false positives and helped in identification and quantitation of diclofenac in the ground water samples of four villages, and pitavastatin in a sample of one village. Copyright © 2015 Elsevier B.V. All rights reserved.

Residual Symptoms in Depressed Outpatients Who Respond by 50% But Do Not Remit to Antidepressant Medication

PubMed Central

McClintock, Shawn M.; Husain, Mustafa M.; Wisniewski, Stephen R.; Nierenberg, Andrew A.; Stewart, Jonathan W.; Trivedi, Madhukar H.; Cook, Ian; Morris, David; Warden, Diane; Rush, Augustus John

2013-01-01

Little is known about the quantity or quality of residual depressive symptoms in patients with major depressive disorder (MDD) who have responded but not remitted with antidepressant treatment. This report describes the residual symptom domains and individual depressive symptoms in a large representative sample of outpatients with nonpsychotic MDD who responded without remitting after up to 12 weeks of citalopram treatment in the Sequenced Treatment Alternatives to Relieve Depression (STAR*D) study. Response was defined as 50% or greater reduction in baseline 16-item Quick Inventory of Depressive Symptomatology—Self-Report (QIDS-SR16) by treatment exit, and remission as a final QIDS-SR16 of less than 6. Residual symptom domains and individual symptoms were based on the QIDS-SR16 and classified as either persisting from baseline or emerging during treatment. Most responders who did not remit endorsed approximately 5 residual symptom domains and 6 to 7 residual depressive symptoms. The most common domains were insomnia (94.6%), sad mood (70.8%), and decreased concentration (69.6%). The most common individual symptoms were midnocturnal insomnia (79.0%), sad mood (70.8%), and decreased concentration/decision making (69.6%). The most common treatment-emergent symptoms were midnocturnal insomnia (51.4%) and decreased general interest (40.0%). The most common persistent symptoms were midnocturnal insomnia (81.6%), sad mood (70.8%), and decreased concentration/decision making (70.6%). Suicidal ideation was the least common treatment-emergent symptom (0.7%) and the least common persistent residual symptom (17.1%). These findings suggest that depressed outpatients who respond by 50% without remitting to citalopram treatment have a broad range of residual symptoms. Individualized treatments are warranted to specifically address each patient's residual depressive symptoms. PMID:21346613

Bioactive Paper Sensor Based on the Acetylcholinesterase for the Rapid Detection of Organophosphate and Carbamate Pesticides

PubMed Central

Badawy, Mohamed E. I.; El-Aswad, Ahmed F.

2014-01-01

In many countries, people are becoming more concerned about pesticide residues which are present in or on food and feed products. For this reason, several methods have been developed to monitor the pesticide residue levels in food samples. In this study, a bioactive paper-based sensor was developed for detection of acetylcholinesterase (AChE) inhibitors including organophosphate and carbamate pesticides. Based on the Ellman colorimetric assay, the assay strip is composed of a paper support (1 × 10 cm), onto which a biopolymer chitosan gel immobilized in crosslinking by glutaraldehyde with AChE and 5,5′-dithiobis(2-nitrobenzoic) acid (DTNB) and uses acetylthiocholine iodide (ATChI) as an outside reagent. The assay protocol involves introducing the sample to sensing zone via dipping of a pesticide-containing solution. Following an incubation period, the paper is placed into ATChI solution to initiate enzyme catalyzed hydrolysis of the substrate, causing a yellow color change. The absence or decrease of the yellow color indicates the levels of the AChE inhibitors. The biosensor is able to detect organophosphate and carbamate pesticides with good detection limits (methomyl = 6.16 × 10−4 mM and profenofos = 0.27 mM) and rapid response times (~5 min). The results show that the paper-based biosensor is rapid, sensitive, inexpensive, portable, disposable, and easy-to-use. PMID:25484901

[Determination of calcium, magnesium and potassium in nurtured cell by AAS with quick-pulsed nebulization technique and NaOH base digestion].

PubMed

Shi, C; Gao, S; Gun, S

1997-06-01

The sample is digested with 6% NaOH solution and an amount of 50 microl is used for protein content analysis by the method of Comassie Brilliant Blue G250, the residual is diluted with equal 0.4% Lathanurm-EDTA solution. Its Calcium magensium and potassium content are determined by AAS. With quick-pulsed nebulization technique. When a self-made micro-sampling device is used, 20microl of sample volume is needed and it is only the 1/10 approximately 1/20 of the sample volume required for conventional determination. Sensitivity, precision and rate of recovery agree well with those using regular wet ashing method.

Gas-liquid chromatographic and gas-liquid-mass spectometric determination of fenvalerate and permethrin residues in grasshoppers and duck tissue samples

USGS Publications Warehouse

Reichel, W.L.; Kolbe, E.J.; Stafford, C.J.

1981-01-01

A procedure is described for determining fenvalerate and permethrin residues in grasshoppers and duck tissues. Samples are Soxhlet-extracted with hexane and cleaned up by gel permeation chromatography with an in-line alumina column. Samples are analyzed by gas-liquid chromatography with electron capture detection, and confirmed by gas-liquid chromatography-mass spectrometry. The average recovery from fortified tissues was 97%.

Organochlorine Pesticides Residues in Human Breast Milk from the Middle Governorates in Jordan in 2013/2014.

PubMed

Al Antary, Tawfiq M; Alawi, Mahmoud A; Estityah, Hussein; Haddad, Nizar

2017-07-01

One hundred samples of mother breast milk were gathered from six middle governorates and districts in Jordan in 2013/2014 to monitor Organochlorine pesticides pollutants. The results showed clearly that banned organochlorine pesticides are still detected in the monitored samples in low concentration despite banning of these persistent pollutants in Jordan since 36 years ago. However, the results indicated that 1% of the contaminated samples contained β-HCH, 5% γ-HCH, 3% p,p'-DDD, 2% heptachlor, 45% p,p'-DDE and 3% p,p'-DDT. In addition, these monitored samples had no residues of aldrin, dieldrin, α-endosulfan, β-endosulfan, HCB, o,p'-DD, o,p'-DDT and o,p'-DDE. In conclusion, there was a decline in the residues of Organochlorine pesticides, particularly DDT group members.

Development of a direct competitive enzyme-linked immunosorbent assay for parathion residue in food samples.

PubMed

Gui, Wen-Jun; Liu, Yi-Hua; Wang, Chun-Mei; Liang, Xiao; Zhu, Guo-Nian

2009-10-01

A heterologous direct competitive enzyme-linked immunosorbent assay (ELISA) for parathion residue determination is described based on a monoclonal antibody and a new competitor. The effects of several physicochemical factors, such as methanol concentration, ionic strength, pH value, and sample matrix, on the performance of the ELISA were optimized for the sake of obtaining a satisfactory assay sensitivity. Results showed that when the assay medium was in the optimized condition (phosphate buffer solution [PBS] containing 10% [v/v] methanol and 0.2 mol/L NaCl at a pH value of 5.0), the sensitivity (estimated as the IC(50) value) and the limit of detection (LOD, estimated as the IC(10) value) were 1.19 and 0.08 ng/ml, respectively. The precision investigation indicated that the intraassay precision values all were below 10% and that the interassay precision values ranged from 4.89 to 19.12%. In addition, the developed ELISA showed a good linear correlation (r(2)=0.9962) to gas chromatography within the analyte's concentration range of 0.1 to 16 ng/ml. When applied to the fortified samples (parathion adding level: 5-15 microg/kg), the developed ELISA presented mean recoveries of 127.46, 122.52, 91.92, 124.01, 129.72, 99.37, and 87.17% for tomato, cucumber, banana, apple, orange, pear, and sugarcane, respectively. Results indicated that the established ELISA is a potential tool for parathion residue determination.

Jaccard distance based weighted sparse representation for coarse-to-fine plant species recognition.

PubMed

Zhang, Shanwen; Wu, Xiaowei; You, Zhuhong

2017-01-01

Leaf based plant species recognition plays an important role in ecological protection, however its application to large and modern leaf databases has been a long-standing obstacle due to the computational cost and feasibility. Recognizing such limitations, we propose a Jaccard distance based sparse representation (JDSR) method which adopts a two-stage, coarse to fine strategy for plant species recognition. In the first stage, we use the Jaccard distance between the test sample and each training sample to coarsely determine the candidate classes of the test sample. The second stage includes a Jaccard distance based weighted sparse representation based classification(WSRC), which aims to approximately represent the test sample in the training space, and classify it by the approximation residuals. Since the training model of our JDSR method involves much fewer but more informative representatives, this method is expected to overcome the limitation of high computational and memory costs in traditional sparse representation based classification. Comparative experimental results on a public leaf image database demonstrate that the proposed method outperforms other existing feature extraction and SRC based plant recognition methods in terms of both accuracy and computational speed.

Survey on the pesticide residues in tea in south India.

PubMed

Seenivasan, Subbiah; Muraleedharan, NarayananNair

2011-05-01

Tea is considered as a 'health beverage' due its antioxidant properties and resultant beneficial effects on human health. Such a beverage should be free from toxic elements such as pesticide residues and heavy metals. A large scale survey of teas produced in the tea factories of south India had been carried out for a period of three years from 2006 to 2008 and 912 tea samples were analysed for the residues of certain pesticides such as dicofol, ethion, quinalphos, hexaconazole, fenpropathrin, fenvalerate and propargite which are used for pest and disease control in tea in this part of the country. The analytical data proved that only less than 0.5 percentage of tea samples had residues of these pesticides. However, residues of pesticides were below their maximum limits in tea, stipulated by the European Union, Codex Alimentarius Commission of FAO/WHO and Prevention of Food Adulteration Act of Govt. of India.

Levels of pesticides residues in the White Nile water in the Sudan.

PubMed

Nesser, Gibreel A A; Abdelbagi, Azhari O; Hammad, Ahmed Mohammed Ali; Tagelseed, Mirghani; Laing, Mark D

2016-06-01

Twenty-two commonly used pesticides were monitored during autumn, winter, and summer of 2004-2005 in 27 water samples from three sites along the White Nile in Sudan (former Sudan). Sites were selected to reflect pesticides gathered from drainage canals in central Sudan and from upstream sources. Collected samples were extracted and subjected to gas chromatographic analysis. Pesticides levels were measured in nanograms per liter. Pesticides residues were detected in 96 % of the samples with a total residue burden of 4132.6 ng L(-1), and an overall mean concentration and range of 50.99 and not detected-1570 ng L(-1), respectively. Ororganochlorines were the most frequently detected contaminants, which were found in 70 % of the samples, causing a total burden of 2852.8 ng L(-1), followed by pyrethroids 15 % of the samples, with a total burden of 926.5 ng L(-1). The tested herbicides were detected in ˂4 % of the samples with a total burden of 353.3 ng L(-1), while organophosphorus levels were below the detection limit. The most frequent contaminants were the following: heptachlor and its epoxide (52 % of samples), followed by DDTs (dichlorodiphenyltrichloroethanes) (DDT and DDE, in 19 % of the samples), cypermethrin and fenvalerate (in 11 % of the samples), and pendimethalin (in <4 % of the samples). Residues of hexachlorocyclohexane (HCH) isomers (α, β, γ and δ), endosulfan (α and β), p, p-DDD, λ cyhalothrin, deltamethrin, and oxyfluorfen were not detected in the analyzed samples. Generally, levels were least in autumn, and followed by summer and winter. Sources of contamination might include agricultural lands in central Sudan and upstream sources. Both recent and old contaminations were indicated.

Organochlorine pesticide residues in human fat in the United Kingdom 1976-7.

PubMed Central

Abbott, D C; Collins, G B; Goulding, R; Hoodless, R A

1981-01-01

Between May 1976 and August 1977 samples of human body fat were taken during routine necropsies in the United Kingdom on 236 subjects aged over 5 years and four infants aged under 4 months. Comparison with results from earlier studies showed a further decline in residues of pp'-dichlorodiphenyltrichloroethane (pp'-DDT) and dieldrin (HEOD) and increased amounts of hexachlorobenzene residues; concentrations of other compounds were similar to those observed in the studies carried out in 1963-4, 1965-7, and 1969-71. Comparison of the data with those from other countries, showed that the concentrations of organochlorine pesticide residues and polychlorobiphenyls in human fat samples from residents of the United Kingdom remain among the lowest in Europe and, indeed, the world. PMID:6797569

Classification of different kinds of pesticide residues on lettuce based on fluorescence spectra and WT-BCC-SVM algorithm

NASA Astrophysics Data System (ADS)

Zhou, Xin; Jun, Sun; Zhang, Bing; Jun, Wu

2017-07-01

In order to improve the reliability of the spectrum feature extracted by wavelet transform, a method combining wavelet transform (WT) with bacterial colony chemotaxis algorithm and support vector machine (BCC-SVM) algorithm (WT-BCC-SVM) was proposed in this paper. Besides, we aimed to identify different kinds of pesticide residues on lettuce leaves in a novel and rapid non-destructive way by using fluorescence spectra technology. The fluorescence spectral data of 150 lettuce leaf samples of five different kinds of pesticide residues on the surface of lettuce were obtained using Cary Eclipse fluorescence spectrometer. Standard normalized variable detrending (SNV detrending), Savitzky-Golay coupled with Standard normalized variable detrending (SG-SNV detrending) were used to preprocess the raw spectra, respectively. Bacterial colony chemotaxis combined with support vector machine (BCC-SVM) and support vector machine (SVM) classification models were established based on full spectra (FS) and wavelet transform characteristics (WTC), respectively. Moreover, WTC were selected by WT. The results showed that the accuracy of training set, calibration set and the prediction set of the best optimal classification model (SG-SNV detrending-WT-BCC-SVM) were 100%, 98% and 93.33%, respectively. In addition, the results indicated that it was feasible to use WT-BCC-SVM to establish diagnostic model of different kinds of pesticide residues on lettuce leaves.

Measurement of residual stress fields in FHPP welding: a comparison between DSPI combined with hole-drilling and neutron diffraction

NASA Astrophysics Data System (ADS)

Viotti, Matias R.; Albertazzi, Armando; Staron, Peter; Pisa, Marcelo

2013-04-01

This paper shows a portable device to measure mainly residual stress fields outside the optical bench. This system combines the traditional hole drilling technique with Digital Speckle Pattern Interferometry. The novel feature of this device is the high degree of compaction since only one base supports simultaneously the measurement module and the hole-drilling device. The portable device allows the measurement of non-uniform residual stresses in accordance with the ASTM standard. In oil and gas offshore industries, alternative welding procedures among them, the friction hydro pillar processing (FHPP) is highlighted and nowadays is an important maintenance tool since it has the capability to produce structure repairs without risk of explosions. In this process a hole is drilled and filled with a consumable rod of the same material. The rod, which could be cylindrical or conical, is rotated and pressed against the hole, leading to frictional heating. In order to assess features about the residual stress distribution generated by the weld into the rod as well as into the base material around the rod, welded samples were evaluated by neutron diffraction and by the hole drilling technique having a comparison between them. For the hole drilling technique some layers were removed by using electrical discharge machining (EDM) after diffraction measurements in order to assess the bulk stress distribution. Results have shown a good agreement between techniques.

A Comparison of Two Approaches for Measuring Educational Growth from CTBS and P-ACT+ Scores.

ERIC Educational Resources Information Center

Noble, Julie; Sawyer, Richard

The purpose of the study was to compare two regression-based approaches for measuring educational effectiveness in Tennessee high schools: the mean residual approach (MR), and a more general linear models (LM) approach. Data were obtained from a sample of 1,011 students who were enrolled in 48 high schools, and who had taken the Comprehensive…

Ethnic Identity and Substance Use among Mexican-Heritage Preadolescents: Moderator Effects of Gender and Time in the United States

ERIC Educational Resources Information Center

Kulis, Stephen S.; Marsiglia, Flavio F.; Kopak, Albert M.; Olmsted, Maureen E.; Crossman, Ashley

2012-01-01

This study examined interactive relationships among ethnic identity, gender, time in the US, and changes in substance use outcomes among a school-based sample of 1,731 Mexican-heritage preadolescents (ages 9-13). Residual change multilevel models adjusting for school clustering and using multiply imputed data assessed changes from beginning to end…

On the Ground or in the Air? A Methodological Experiment on Crop Residue Cover Measurement in Ethiopia

NASA Astrophysics Data System (ADS)

Kosmowski, Frédéric; Stevenson, James; Campbell, Jeff; Ambel, Alemayehu; Haile Tsegay, Asmelash

2017-10-01

Maintaining permanent coverage of the soil using crop residues is an important and commonly recommended practice in conservation agriculture. Measuring this practice is an essential step in improving knowledge about the adoption and impact of conservation agriculture. Different data collection methods can be implemented to capture the field level crop residue coverage for a given plot, each with its own implication on survey budget, implementation speed and respondent and interviewer burden. In this paper, six alternative methods of crop residue coverage measurement are tested among the same sample of rural households in Ethiopia. The relative accuracy of these methods are compared against a benchmark, the line-transect method. The alternative methods compared against the benchmark include: (i) interviewee (respondent) estimation; (ii) enumerator estimation visiting the field; (iii) interviewee with visual-aid without visiting the field; (iv) enumerator with visual-aid visiting the field; (v) field picture collected with a drone and analyzed with image-processing methods and (vi) satellite picture of the field analyzed with remote sensing methods. Results of the methodological experiment show that survey-based methods tend to underestimate field residue cover. When quantitative data on cover are needed, the best estimates are provided by visual-aid protocols. For categorical analysis (i.e., >30% cover or not), visual-aid protocols and remote sensing methods perform equally well. Among survey-based methods, the strongest correlates of measurement errors are total farm size, field size, distance, and slope. Results deliver a ranking of measurement options that can inform survey practitioners and researchers.

On the Ground or in the Air? A Methodological Experiment on Crop Residue Cover Measurement in Ethiopia.

PubMed

Kosmowski, Frédéric; Stevenson, James; Campbell, Jeff; Ambel, Alemayehu; Haile Tsegay, Asmelash

2017-10-01

Maintaining permanent coverage of the soil using crop residues is an important and commonly recommended practice in conservation agriculture. Measuring this practice is an essential step in improving knowledge about the adoption and impact of conservation agriculture. Different data collection methods can be implemented to capture the field level crop residue coverage for a given plot, each with its own implication on survey budget, implementation speed and respondent and interviewer burden. In this paper, six alternative methods of crop residue coverage measurement are tested among the same sample of rural households in Ethiopia. The relative accuracy of these methods are compared against a benchmark, the line-transect method. The alternative methods compared against the benchmark include: (i) interviewee (respondent) estimation; (ii) enumerator estimation visiting the field; (iii) interviewee with visual-aid without visiting the field; (iv) enumerator with visual-aid visiting the field; (v) field picture collected with a drone and analyzed with image-processing methods and (vi) satellite picture of the field analyzed with remote sensing methods. Results of the methodological experiment show that survey-based methods tend to underestimate field residue cover. When quantitative data on cover are needed, the best estimates are provided by visual-aid protocols. For categorical analysis (i.e., >30% cover or not), visual-aid protocols and remote sensing methods perform equally well. Among survey-based methods, the strongest correlates of measurement errors are total farm size, field size, distance, and slope. Results deliver a ranking of measurement options that can inform survey practitioners and researchers.

Analysis of Phyllostachys pubescens bamboo residues for liquefaction: chemical components, infrared spectroscopy, and thermogravimetry

Treesearch

Jinqiu Qi; Chung-Yun Hse; Todd F. Shupe

2013-01-01

Residues of Phyllostachys pubescens bamboo obtained from central Louisiana, USA, were comprehensively investigated for use in liquefaction. The results showed that bamboo branches had the highest Klason lignin and ash content, about 26% and 2.75%, respectively. The epidermis layer sample had relatively higher carbohydrate content, while the wax layer sample had the...

U/Th dating of carbonate deposits from Constantina (Sevilla), Spain.

PubMed

Alcaraz-Pelegrina, J M; Martínez-Aguirre, A

2007-07-01

Uranium-series method has been applied to continental carbonate deposits from Constantina, Seville, in Spain. All samples analysed were impure carbonates and the leachate-leachate method was used to obtain activity ratios in carbonate fraction. Leachate-residue methods were applied to one of the samples in order to compare with leachate-leachate method, but leachate-residue method assumptions did not meet and ages resulting from leachate-residue methods were not valid. Ages obtained by leachate-leachate method range from 1.8 to 23.5ky BP and are consistent with stratigraphical positions of samples analysed. Initial activity ratios for uranium isotopes are practically constant in this period, thus indicating that no changes in environmental conditions occur between 1.8 and 23.5ky period.

Contamination from organochlorine pesticides (OCPs) in agricultural soils of Kuttanad agroecosystem in India and related potential health risk.

PubMed

Sruthi, S N; Shyleshchandran, M S; Mathew, Sunil Paul; Ramasamy, E V

2017-01-01

The presence and distribution of a few organochlorine pesticides (OCPs) in the paddy fields of the Kuttanad agroecosystem (KAE) was examined in the present study. Kuttanad forms a part of the Vembanad wetland system which is a Ramsar site of international importance in the state of Kerala. This study, to the best of our knowledge, is the first report on the occurrence of OCP residues in KAE. Pesticide residue analysis was done with gas chromatograph (GC-ECD). Twenty-one soil samples were collected for the multiresidual analysis of OCPs. Sixteen OCP residues with a notable concentration were observed from the study area. α-BHC; β-BHC; γ-BHC; δ-BHC; α-chlordane; γ-chlordane; heptachlor; 4,4-DDT; 4,4-DDE; 4,4-DDD; α-endosulfan; β-endosulfan; aldrin; dieldrin; endrin aldehyde; and endrin ketone were the residues observed. The percentage-wise occurrence of OCP residues in the soil samples analysed (total of 63 samples from 21 sites, three samples per site) exhibits the following order: Σ BHC˃ Σ chlordane ˃ Σ dieldrin ˃ Σ aldrin ˃ Σ endrin˃ Σ heptachlor = endosulfan˃ Σ DDT. All pesticides detected from KAE are in the list of priority pollutants of US Environmental Protection Agency (USEPA). The distribution pattern of OCPs in the KAE soils revealed their origin as both historical and recent application of pesticides. Health risk assessment of OCP residues on human population was also conducted. The findings indicated that the concentrations of OCPs were within the permissible limits of USEPA, thus, the human population in the study area was safe.

Carbon Emissions from Residue Burn Piles Estimated Using LiDAR or Ground Based Measurements of Pile Volumes in a Coastal Douglas-Fir Forest

NASA Astrophysics Data System (ADS)

Trofymow, J. A.; Coops, N.; Hayhurst, D.

2012-12-01

Following forest harvest, residues left on site and roadsides are often disposed of to reduce fire risk and free planting space. In coastal British Columbia burn piles are the main method of disposal, particularly for accumulations from log processing. Quantification of residue wood in piles is required for: smoke emission estimates, C budget calculations, billable waste assessment, harvest efficiency monitoring, and determination of bioenergy potentials. A second-growth Douglas-fir dominated (DF1949) site on eastern Vancouver Island and subject of C flux and budget studies since 1998, was clearcut in winter 2011, residues piled in spring and burned in fall. Prior to harvest, the site was divided into 4 blocks to account for harvest plans and ecosite conditions. Total harvested wood volume was scaled for each block. Residue pile wood volume was determined by a standard Waste and Residue Survey (WRS) using field estimates of pile base area and plot density (wood volume / 0.005 ha plot) on 2 piles per block, by a smoke emissions geometric method with pile volumes estimated as ellipsoidal paraboloids and packing ratios (wood volume / pile volume) for 2 piles per block, as well as by five other GIS methods using pile volumes and areas from LiDAR and orthophotography flown August 2011, a LiDAR derived digital elevation model (DEM) from 2008, and total scaled wood volumes of 8 sample piles disassembled November 2011. A weak but significant negative relationship was found between pile packing ratio and pile volume. Block level avoidable+unavoidable residue pile wood volumes from the WRS method (20.0 m3 ha-1 SE 2.8) were 30%-50% of the geometric (69.0 m3 ha-1 SE 18.0) or five GIS/LiDAR (48.0 to 65.7 m3 ha-1 ) methods. Block volumes using the 2008 LiDAR DEM (unshifted 48.0 m3 ha-1 SE 3.9, shifted 53.6 m3 ha-1 SE 4.2) to account for pre-existing humps or hollows beneath piles were not different from those using the 2011 LiDAR DEM (50.3 m3 ha-1 SE 4.0). The block volume ratio (total residue pile / harvest scale, wood volumes x 100) for the WRS method (3.3% SE 0.45) was lower than for LiDAR 2011 method (8.1% SE 0.31). Using wood densities from in situ samples and LiDAR 2011 method wood volumes, total residue pile wood biomass in the blocks was 21.5 t dry mass ha-1 (SE 1.9). Post-burn charred residues were ~1.5 t dry mass ha-1 resulting in C emission estimates of 10 t C ha-1 (SE 0.91), assuming 50% C, and equivalent to 2 - 3 years of pre-harvest stand C uptake (NEP 4.8 t C ha-1 y-1 SE 0.58). Results suggest the WRS method may underestimate residue pile wood volumes, while the geometric method may overestimate depending on packing ratio used. While remote sensing methods reduce uncertainty in estimating volumes or areas of all piles in a block, quantification of packing ratios remains a significant source of uncertainty in determining block level residue pile wood volumes. Additional studies are needed for other forest and harvest types to determine the wider applicability of these findings.

Residual Wage Differences by Gender: Bounding the Estimates.

ERIC Educational Resources Information Center

Sakellariou, Chris N.; Patrinos, Harry A.

1996-01-01

Uses data from the 1986 Canadian labor market activity survey file to derive estimates of residual gender wage gap differences. Investigates these estimates' dependence on experimental design and on assumptions about discrimination-free wage structures. Residual differences persist, even after restricting the sample to a group of highly motivated,…

Distribution of veterinary drug residues among muscles

USDA-ARS?s Scientific Manuscript database

The U.S. Food and Drug Administration sets tolerances for veterinary drug residues in muscle, but does not specify which muscle should be sampled for analysis. The goal of this research was to determine if antibiotic residue levels are dependent on muscle type. In this study, penicillin G (Pen G) d...

Rumsey and Walker_AMT_2016_Table 2.xlsx

EPA Pesticide Factsheets

Table summarizes instrument precision assessed by collocating the two sample boxes. Precision is quantified as the standard deviation of the residuals of an orthogonal least squares regression of concentrations from the two sample boxes. This allows for an estimation of gradient precision and ultimately gradient and flux detection limits. This dataset is associated with the following publication:Rumsey, I. Application of an online ion chromatography-based instrument for gradient flux measurements of speciated nitrogen and sulfur. ENVIRONMENTAL SCIENCE & TECHNOLOGY. American Chemical Society, Washington, DC, USA, 9(6): 2581-2592, (2016).

Approaches to stream solute load estimation for solutes with varying dynamics from five diverse small watershed

USGS Publications Warehouse

Aulenbach, Brent T.; Burns, Douglas A.; Shanley, James B.; Yanai, Ruth D.; Bae, Kikang; Wild, Adam; Yang, Yang; Yi, Dong

2016-01-01

Estimating streamwater solute loads is a central objective of many water-quality monitoring and research studies, as loads are used to compare with atmospheric inputs, to infer biogeochemical processes, and to assess whether water quality is improving or degrading. In this study, we evaluate loads and associated errors to determine the best load estimation technique among three methods (a period-weighted approach, the regression-model method, and the composite method) based on a solute's concentration dynamics and sampling frequency. We evaluated a broad range of varying concentration dynamics with stream flow and season using four dissolved solutes (sulfate, silica, nitrate, and dissolved organic carbon) at five diverse small watersheds (Sleepers River Research Watershed, VT; Hubbard Brook Experimental Forest, NH; Biscuit Brook Watershed, NY; Panola Mountain Research Watershed, GA; and Río Mameyes Watershed, PR) with fairly high-frequency sampling during a 10- to 11-yr period. Data sets with three different sampling frequencies were derived from the full data set at each site (weekly plus storm/snowmelt events, weekly, and monthly) and errors in loads were assessed for the study period, annually, and monthly. For solutes that had a moderate to strong concentration–discharge relation, the composite method performed best, unless the autocorrelation of the model residuals was <0.2, in which case the regression-model method was most appropriate. For solutes that had a nonexistent or weak concentration–discharge relation (modelR2 < about 0.3), the period-weighted approach was most appropriate. The lowest errors in loads were achieved for solutes with the strongest concentration–discharge relations. Sample and regression model diagnostics could be used to approximate overall accuracies and annual precisions. For the period-weighed approach, errors were lower when the variance in concentrations was lower, the degree of autocorrelation in the concentrations was higher, and sampling frequency was higher. The period-weighted approach was most sensitive to sampling frequency. For the regression-model and composite methods, errors were lower when the variance in model residuals was lower. For the composite method, errors were lower when the autocorrelation in the residuals was higher. Guidelines to determine the best load estimation method based on solute concentration–discharge dynamics and diagnostics are presented, and should be applicable to other studies.

Detection of Traces of Ovalbumin and Casein in White and Red Wines by Quantitative Western Blotting.

PubMed

Meyer, Philippe; Zanetti, Simone

2015-09-01

Fining of wine with agents containing cow's milk or hen's egg white is a common and traditional procedure. In light of increasing food allergies all over the world, the presence of fining residues has been subject of intense debate. Switzerland does not make exception, and since 2009 the Federal Department of Home Affairs has modified its food regulations stating that the labels must show if traces of fining agents are present. Nevertheless, the application of this regulation is not based on an official analytical method. In this study we show that immunoblotting is an efficient technique to detect and quantify ovalbumin and casein residues in bottled wine. We showed that final filtration is an essential step to remove finings in red wine, and that overfining of white wine may result in fining residues in finished products. Finally, for the first time in Switzerland, 22 samples were taken by food safety inspectors and officially analyzed for the regional food control authority of the Canton of Vaud. These samples were allergen free, but a larger study is currently planned in collaboration with other regional authorities of Switzerland to complete these results and make a complete picture of the Swiss wine production. © 2015 Institute of Food Technologists®

Reducing detrimental electrostatic effects in Casimir-force measurements and Casimir-force-based microdevices

NASA Astrophysics Data System (ADS)

Xu, Jun; Klimchitskaya, G. L.; Mostepanenko, V. M.; Mohideen, U.

2018-03-01

It is well known that residual electrostatic forces create significant difficulties in precise measurements of the Casimir force and the wide use of Casimir-operated microdevices. We experimentally demonstrate that, with the help of Ar-ion cleaning of the surfaces, it is possible to make electrostatic effects negligibly small compared to the Casimir interaction. Our experimental setup consists of a dynamic atomic force microscope supplemented with an Ar-ion gun and argon reservoir. The residual potential difference between the Au-coated surfaces of a sphere and those of a plate was measured both before and after in situ Ar-ion cleaning. It is shown that this cleaning decreases the magnitude of the residual potential by up to an order of magnitude and makes it almost independent of the separation. The gradient of the Casimir force was measured using ordinary samples subjected to Ar-ion cleaning. The obtained results are shown to be in good agreement both with previous precision measurements using specially selected samples and with theoretical predictions of the Lifshitz theory. The conclusion is made that the suggested method of in situ Ar-ion cleaning is effective in reducing the electrostatic effects and therefore is a great resource for experiments on measuring the Casimir interaction and for Casimir-operated microdevices.

Residual stress measurement in veneering ceramic by hole-drilling.

PubMed

Mainjot, Amélie K; Schajer, Gary S; Vanheusden, Alain J; Sadoun, Michaël J

2011-05-01

Mismatch in thermal expansion properties between veneering ceramic and metallic or high-strength ceramic cores can induce residual stresses and initiate cracks when combined with functional stresses. Knowledge of the stress distribution within the veneering ceramic is a key factor for understanding and predicting chipping failures, which are well-known problems with Yttria-tetragonal-zirconia-polycrystal based fixed partial dentures. The objectives of this study are to develop a method for measuring the stress profile in veneering ceramics and to compare ceramic-fused-to-metal compounds to veneered Yttria-tetragonal-zirconia-polycrystal ceramic. The hole-drilling method, often used for engineering measurements, was adapted for use with veneering ceramic. Because of the high sensitivity needed in comparison with industrial applications, a high sensitivity electrical measurement chain was developed. All samples exhibited the same type of stress vs. depth profile, starting with compressive at the ceramic surface, decreasing with depth and becoming tensile at 0.5-1.0mm from the surface, and then becoming slightly compressive again. The zirconia samples exhibited a stress depth profile of larger magnitude. The hole drilling method was shown be a practical tool for measuring residual stresses in veneering ceramics. Copyright © 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Total sulfur determination in residues of crude oil distillation using FT-IR/ATR and variable selection methods.

PubMed

Müller, Aline Lima Hermes; Picoloto, Rochele Sogari; de Azevedo Mello, Paola; Ferrão, Marco Flores; de Fátima Pereira dos Santos, Maria; Guimarães, Regina Célia Lourenço; Müller, Edson Irineu; Flores, Erico Marlon Moraes

2012-04-01

Total sulfur concentration was determined in atmospheric residue (AR) and vacuum residue (VR) samples obtained from petroleum distillation process by Fourier transform infrared spectroscopy with attenuated total reflectance (FT-IR/ATR) in association with chemometric methods. Calibration and prediction set consisted of 40 and 20 samples, respectively. Calibration models were developed using two variable selection models: interval partial least squares (iPLS) and synergy interval partial least squares (siPLS). Different treatments and pre-processing steps were also evaluated for the development of models. The pre-treatment based on multiplicative scatter correction (MSC) and the mean centered data were selected for models construction. The use of siPLS as variable selection method provided a model with root mean square error of prediction (RMSEP) values significantly better than those obtained by PLS model using all variables. The best model was obtained using siPLS algorithm with spectra divided in 20 intervals and combinations of 3 intervals (911-824, 823-736 and 737-650 cm(-1)). This model produced a RMSECV of 400 mg kg(-1) S and RMSEP of 420 mg kg(-1) S, showing a correlation coefficient of 0.990. Copyright © 2011 Elsevier B.V. All rights reserved.

Antimicrobial residues in animal waste and water resources proximal to large-scale swine and poultry feeding operations

USGS Publications Warehouse

Campagnolo, E.R.; Johnson, K.R.; Karpati, A.; Rubin, C.S.; Kolpin, D.W.; Meyer, M.T.; Esteban, J. Emilio; Currier, R.W.; Smith, K.; Thu, K.M.; McGeehin, M.

2002-01-01

Expansion and intensification of large-scale animal feeding operations (AFOs) in the United States has resulted in concern about environmental contamination and its potential public health impacts. The objective of this investigation was to obtain background data on a broad profile of antimicrobial residues in animal wastes and surface water and groundwater proximal to large-scale swine and poultry operations. The samples were measured for antimicrobial compounds using both radioimmunoassay and liquid chromatography/electrospray ionization-mass spectrometry (LC/ESI-MS) techniques. Multiple classes of antimicrobial compounds (commonly at concentrations of >100 μg/l) were detected in swine waste storage lagoons. In addition, multiple classes of antimicrobial compounds were detected in surface and groundwater samples collected proximal to the swine and poultry farms. This information indicates that animal waste used as fertilizer for crops may serve as a source of antimicrobial residues for the environment. Further research is required to determine if the levels of antimicrobials detected in this study are of consequence to human and/or environmental ecosystems. A comparison of the radioimmunoassay and LC/ESI-MS analytical methods documented that radioimmunoassay techniques were only appropriate for measuring residues in animal waste samples likely to contain high levels of antimicrobials. More sensitive LC/ESI-MS techniques are required in environmental samples, where low levels of antimicrobial residues are more likely.

Prevalence of cannabis residues in psychiatric patients: a case study of two mental health referral hospitals in Uganda.

PubMed

Awuzu, Epaenetus A; Kaye, Emmanuel; Vudriko, Patrick

2014-01-08

Various studies have reported that abuse of cannabis is a risk factor for psychosis. The aims of this study were to determine the prevalence of delta 9-tetrahydrocanabinol (Δ(9)-THC), a major metabolite of cannabis, in psychiatric patients in Uganda, and to assess the diagnostic capacity of two referral mental health hospitals to screen patients for exposure to cannabis in Uganda. Socio-demographic characteristics of the patients were collected through questionnaires and review of medical records. Urine samples were collected from 100 patients and analyzed using Δ(9)-THC immunochromatographic kit (Standard Diagnostics(®), South Korea). Seventeen percent of the patients tested positive for Δ(9)-THC residues in their urine. There was strong association (P < 0.05) between history of previous abuse of cannabis and presence of Δ(9)-THC residues in the urine. Alcohol, cocaine, heroin, pethidine, tobacco, khat and kuber were the other substances abused in various combinations. Both referral hospitals lacked laboratory diagnostic kits for detection of cannabis in psychiatric patients. In conclusion, previous abuse of cannabis is associated with occurrence of the residues in psychiatric patients, yet referral mental health facilities in Uganda do not have the appropriate diagnostic kits for detection of cannabis residues as a basis for evidence-based psychotherapy.

Bioefficacy, dissipation kinetics and safety evaluation of selected insecticides in Allium cepa L.

PubMed

Srinivas P, Satya; Banerjee, Kaushik; Jadhav, Manjusha R; Ghaste, Manoj S; Lawande, K E

2012-01-01

This paper reports the bioefficacy of selected insecticides against thrips and their pre-harvest intervals (PHI) in onion pertaining to their recommended application rates and maximum residue limits. Profenophos, methomyl and imidacloprid showed comparatively higher bioefficacy against thrips. GC-MS and LC-MS/MS-based residue analysis methods in onion bulbs and composite matrix of bulbs+leaves were thoroughly validated. The residue data for bulb+leaves was assessed with reference to the EU-MRLs applicable for spring onion. Dimethoate was the most stable chemical with PHI of 52.5 days, followed by monocrotophos (24 days) and carbofuran (20.5 days). The PHIs of profenophos, chlorpyrifos, methomyl and cypermethrin were similar and within the range of 10-13 days. Imidacloprid and λ-cyhalothrin had similar PHI of 4.5 days. Spinosad was the fastest-degrading chemical with PHI of 2 days. The combined bioefficacy and residue dynamics information will support label-claim of these insecticides for the management of thrips in onion, help in scheduling their applications in pest management program as per relative PHIs and minimize the residue accumulations at harvest. The dietary exposure was less than the maximum permissible intake for most of the insecticides on all sampling days except for dimethoate and monocrotophos.

Multispectral Mueller polarimetric imaging detecting residual cancer and cancer regression after neoadjuvant treatment for colorectal carcinomas

NASA Astrophysics Data System (ADS)

Pierangelo, Angelo; Manhas, Sandeep; Benali, Abdelali; Fallet, Clément; Totobenazara, Jean-Laurent; Antonelli, Maria-Rosaria; Novikova, Tatiana; Gayet, Brice; De Martino, Antonello; Validire, Pierre

2013-04-01

This work is devoted to a first exploration of Mueller polarimetric imaging for the detection of residual cancer after neoadjuvant treatment for the rectum. Three samples of colorectal carcinomas treated by radiochemotherapy together with one untreated sample are analyzed ex vivo before fixation in formalin by using a multispectral Mueller polarimetric imaging system operated from 500 to 700 nm. The Mueller images, analyzed using the Lu-Chipmann decomposition, show negligible diattenuation and retardation. The nonirradiated rectum exhibits a variation of depolarization with cancer evolution stage. At all wavelengths on irradiated samples, the contrast between the footprint of the initial tumor and surrounding healthy tissue is found to be much smaller for complete tumor regression than when a residual tumor is present, even at volume fractions of the order of 5%. This high sensitivity is attributed to the modification of stromal collagen induced by the cancer. The depolarization contrast between treated cancer and healthy tissue is found to increase monotonously with the volume fraction of residual cancer in the red part of the spectrum. Polarimetric imaging is a promising technique for detecting short-time small residual cancers, which is valuable information for pathological diagnosis and patient management by clinicians.

Nutritional Composition Changes During Tempeh Gembus Processing

NASA Astrophysics Data System (ADS)

Nazaretha Sandessy Damanik, Ruth; Yanti Winda Pratiwi, Dwi; Widyastuti, Nurmasari; Rustanti, Ninik; Anjani, Gemala; Nur Afifah, Diana

2018-02-01

This paper was aimed to analyze nutritional composition during tempeh gembus processing. Processing of tempeh gembus may cause an increase or decrease in its nutritional value such as amino acids, fatty acids, vitamins, and minerals. Regardless, tempeh gembus may still be potentially beneficial to help fulfill nutrient needs. This was a descriptive study with three samples: soybeans, tofu residue, and tempeh gembus. Soybeans used were varieties of Grobogan, Central Java. Minerals identified in all three samples include sodium, calcium, potassium, phospor, and iron. Soybeans, tofu residue, and tempeh gembus each contain 34.12%, 5.40%, and 4.80% of amino acids. Saturated fatty acids were the lowest in soybeans (12.01%), marginally surpassed by tofu residue (12.41%) and tempeh gembus (12.55%). Total levels of monounsaturated fatty acids were also found in a similar pattern (34.1%, 36.5%, 36.7% respectively). In contrast, soybeans had significantly more polyunsaturated fatty acids than other samples, containing up to 43.6% in comparison with 38.29% in tofu residue and 30.18% in tempeh gembus. Overall, the nutritional profile of soybeans was generally better than tofu residue and tempeh gembus. However, fermentation process may play a role in enchancing the fatty acid profile.

[Antibiotic Residue in Environmental Water in Vietnam].

PubMed

Harada, Kazuo

2018-01-01

　The increasing prevalence of antimicrobial resistance (AMR) has caused intractable infections worldwide. Nearly 50% of the healthy population of Southeast Asia carries extended-spectrum β-lactamase (ESBL)-producing Escherichia coli. The overuse of antimicrobial agents in the agriculture, aquaculture, and medical care sectors causes environmental pollution, facilitating the spread of AMR. However, there is a lack of data pertaining to antimicrobial residues in environmental water in such regions. We investigated a total of 49 chemicals, including β-lactams, sulfonamides, quinolones, and tetracyclines. Water samples were collected from rivers in city centers, and ponds in livestock and aquaculture farms, in Ha Noi, Thai Binh, and Can Tho in Vietnam. We detected antimicrobial agents at 87 of 111 sampling sites (78.4%). Among the target analytes, sulfamethoxazole, sulfamethazine, trimethoprim, cephalexin, and ofloxacin were detected frequently. The residual levels of each antimicrobial agent ranged from 0.1 to 10000 ng/L. Moreover, we detected multi-drug resistant E. coli in fishes sampled from these rivers, suggesting unwanted effects of antimicrobial residues in the environment.

Pesticide residue concentration in soil following conventional and Low-Input Crop Management in a Mediterranean agro-ecosystem, in Central Greece.

PubMed

Karasali, Helen; Marousopoulou, Anna; Machera, Kyriaki

2016-01-15

The present study was focused on the comparative evaluation of pesticide residues, determined in soil samples from Kopaida region, Greece before and after the implementation of Low-Input Crop Management (LCM) protocols. LCM has been suggested as an environmental friendly plant protection approach to be applied on crops growing in vulnerable to pollution ecosystems, with special focus on the site specific problems. In the case of the specific pilot area, the vulnerability was mainly related to the pollution of water bodies from agrochemicals attributed to diffuse pollution primarily from herbicides and secondarily from insecticides. A total of sixty-six soil samples, were collected and analyzed during a three-year monitoring study and the results of the determined pesticide residues were considered for the impact evaluation of applied plant protection methodology. The LCM was developed and applied in the main crops growing in the pilot area i.e. cotton, maize and industrial tomato. Herbicides active ingredients such as ethalfluralin, trifluralin, pendimethalin, S-metolachlor and fluometuron were detected in most samples at various concentrations. Ethalfluralin, which was the active ingredient present in the majority of the samples ranged from 0.01 μg g(-1) to 0.26 μg g(-1) soil dry weight. However, the amount of herbicides measured after the implementation of LCM for two cropping periods, was reduced by more than 75% in all cases. The method of analysis was based on the simultaneous extraction of the target compounds by mechanical shaking, followed by liquid chromatography mass spectrometric and gas chromatography electron capture (LC-MS/MS and GC-ECD) analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

The occurrence of pesticides and persistent organic pollutants in Italian organic honeys from different productive areas in relation to potential environmental pollution.

PubMed

Chiesa, L M; Labella, G F; Giorgi, A; Panseri, S; Pavlovic, R; Bonacci, S; Arioli, F

2016-07-01

Bee products, such as honey, are widely consumed as food and consumer interest is currently oriented towards organic foods. Regarding this, the European Commission establishes that the qualification of organic honey and other beekeeping products as being from organic production is closely bound with the characteristics of hive treatments as well as the quality of the environment. Agricultural contamination with pesticides is a challenging problem that needs to be fully addressed, in particular in the field of organic production systems. In this study, the occurrence of different classes of contaminants selected as representative of potential contamination sources were investigated in 59 organic honeys: organochlorines, OCs; organophosphates, OPs; polychlorobiphenyls, PCBs and polybromodiphenylethers, PBDEs. A method based on Accelerated Solvent Extraction with "in line" clean-up and GC-MS/MS detection was developed to detect contaminants. Residues of many pesticides were found in most of the samples investigated. The majority of honey samples contained at least one of the pesticides, even if their concentrations were found to be lower than its MRL. Diazinon, Mevinphos, Coumaphos, Chlorpyrifos and Quinoxyfen were the residues frequently detected in samples coming from the apple and citrus orchard areas. Furthermore, the results of the present study show that the presence of the residue in organic honey may also be affected by the geographical area (e.g. the presence of an agricultural system) confirming honey bee and beehive matrices as appropriate sentinels for monitoring contamination in the environment. The optimised method proved to be simple and rapid, requiring small sample sizes and minimising solvent consumption, due to the ASE having an "in line" clean-up step. Copyright © 2016 Elsevier Ltd. All rights reserved.

Analysis of pesticide residues in strawberries and soils by GC-MS/MS, LC-MS/MS and two-dimensional GC-time-of-flight MS comparing organic and integrated pest management farming.

PubMed

Fernandes, Virgínia C; Lehotay, Steven J; Geis-Asteggiante, Lucía; Kwon, Hyeyoung; Mol, Hans G J; van der Kamp, Henk; Mateus, Nuno; Domingues, Valentina F; Delerue-Matos, Cristina

2014-01-01

This study analysed 22 strawberry and soil samples after their collection over the course of 2 years to compare the residue profiles from organic farming with integrated pest management practices in Portugal. For sample preparation, we used the citrate-buffered version of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. We applied three different methods for analysis: (1) 27 pesticides were targeted using LC-MS/MS; (2) 143 were targeted using low pressure GC-tandem mass spectrometry (LP-GC-MS/MS); and (3) more than 600 pesticides were screened in a targeted and untargeted approach using comprehensive, two-dimensional gas chromatography time-of-flight mass spectrometry (GC × GC-TOF-MS). Comparison was made of the analyses using the different methods for the shared samples. The results were similar, thereby providing satisfactory confirmation of both similarly positive and negative findings. No pesticides were found in the organic-farmed samples. In samples from integrated pest management practices, nine pesticides were determined and confirmed to be present, ranging from 2 µg kg(-1) for fluazifop-p-butyl to 50 µg kg(-1) for fenpropathrin. Concentrations of residues in strawberries were less than European maximum residue limits.

On-matrix Derivatization for Dynamic Headspace Sampling of Nonvolatile Surface Residues

DOE Office of Scientific and Technical Information (OSTI.GOV)

Harvey, Scott D.; Wahl, Jon H.

2012-09-01

The goal of this study is to extend sampling by the field and laboratory emission cell (FLEC) purge-and-trap technique to applications that target nonvolatile residues. On-matrix derivatization of residues to render analytes stable and more volatile is explored to achieve this goal. Results show that on-matrix derivatizations of nerve agent hydrolysis products (monoalkyl methylphosphonic acids and methylphosphonic acid [MPA]) with diazomethane were successful on glass and painted wallboard (at the 10-µg level). It also was successful on the more difficult concrete (at the 500-µg level) and carpet (at the 20-µg level) substrates that cannot be successfully sampled using swipe techniques.more » Analysis of additional chemical warfare (CW)-associated residues can be approached by on-matrix derivatization with trifluoroacetic anhydride (TFAA). For example, amines (used as stabilizers or present as decomposition products of the nerve agent VX) or thiodiglycol (hydrolysis product of sulfur mustard) could be sampled as their TFAA derivatives from glass, painted wallboard, and concrete (at the 40-µg level), as well as carpet (at the 80-µg level) surfaces. Although the amine and thiodiglycol are semi-volatile and could be sampled directly, derivatization improves the recovery and chromatographic behavior of these analytes.« less

On-matrix derivatization for dynamic headspace sampling of nonvolatile surface residues.

PubMed

Harvey, Scott D; Wahl, Jon H

2012-09-21

The goal of this study is to extend sampling by the field and laboratory emission cell (FLEC) dynamic headspace technique to applications that target nonvolatile residues. On-matrix derivatization of residues to render analytes stable and more volatile is explored to achieve this goal. Results show that on-matrix derivatizations of nerve agent hydrolysis products (monoalkyl methylphosphonic acids and methylphosphonic acid [MPA]) with diazomethane were successful on glass and painted wallboard (at the 10-μg level). It also was successful on the more difficult concrete (at the 500-μg level) and carpet (at the 20-μg level), substrates that cannot be successfully sampled using swipe techniques. Analysis of additional chemical warfare (CW)-associated residues can be approached by on-matrix derivatization with trifluoroacetic anhydride (TFAA). For example, amines (used as stabilizers or present as decomposition products of the nerve agent VX) or thiodiglycol (hydrolysis product of sulfur mustard) could be sampled as their TFAA derivatives from glass, painted wallboard, and concrete (at the 40-μg level), as well as carpet (at the 80-μg level) surfaces. Although the amine and thiodiglycol are semi-volatile and could be sampled directly, derivatization improves the recovery and chromatographic behavior of these analytes. Copyright © 2012 Elsevier B.V. All rights reserved.

Improved lossless intra coding for H.264/MPEG-4 AVC.

PubMed

Lee, Yung-Lyul; Han, Ki-Hun; Sullivan, Gary J

2006-09-01

A new lossless intra coding method based on sample-by-sample differential pulse code modulation (DPCM) is presented as an enhancement of the H.264/MPEG-4 AVC standard. The H.264/AVC design includes a multidirectional spatial prediction method to reduce spatial redundancy by using neighboring samples as a prediction for the samples in a block of data to be encoded. In the new lossless intra coding method, the spatial prediction is performed based on samplewise DPCM instead of in the block-based manner used in the current H.264/AVC standard, while the block structure is retained for the residual difference entropy coding process. We show that the new method, based on samplewise DPCM, does not have a major complexity penalty, despite its apparent pipeline dependencies. Experiments show that the new lossless intra coding method reduces the bit rate by approximately 12% in comparison with the lossless intra coding method previously included in the H.264/AVC standard. As a result, the new method is currently being adopted into the H.264/AVC standard in a new enhancement project.

Nationwide residues of organochlorine compounds in starlings (Sturnus vulgaris), 1976

USGS Publications Warehouse

White, D.H.

1979-01-01

Organochlorine pesticide and PCB residues in starlings from 126 sites within the contiguous 48 states were monitored during fall 1976. The average nationwide level of DDE and PCBs has increased significantly since 1974, but the number of sites reporting PCB residues has decreased fivefold. Dieldrin residues have remained unchanged since 1974. Highest DDE levels occurred in samples from parts of Arizona, Arkansas, California, Louisiana, and New Mexico.

Depletion of eugenol residues from the skin-on fillet tissue of rainbow trout exposed to 14C-labeled eugenol

USGS Publications Warehouse

Meinertz, Jeffery R.; Schreier, Theresa M.; Porcher, Scott T.; Smerud, Justin R.; Gaikowski, Mark P.

2014-01-01

The U.S. is lagging in access to an approved immediate-release sedative, i.e. a compound that can be safely and effectively used to sedate fish and has no withdrawal period. AQUI-S® 20E (10% active ingredient, eugenol) is under investigation as an immediate-release sedative for freshwater finfish. Because of its investigational status, data are needed to characterize the depletion, distribution, and identity of AQUI-S® 20E residues in fillet tissue. Rainbow trout (Oncorhynchus mykiss) were exposed to uniformly ring labeled 14C-eugenol at a nominal concentration of 10 mg/L for 60 min in 18 °C water. Fish (n = 6) were sampled immediately after the exposure (0 min) then at 30, 60, 120, and 240 min. Eugenol concentrations and characterization of 14C residues in the fillet tissue were determined by high pressure liquid chromatography and flow-through liquid scintillation counting techniques. Total 14C-residue burdens in fillet tissue were determined by tissue oxidation and static liquid scintillation counting techniques. Maximum eugenol and 14C-eugenol equivalent residue concentrations in the fillet tissue were measured immediately after the exposure (44.5 and 38.8 μg/g, respectively). Eugenol was the primary 14C-residue (> 90% of all 14C-residues) in extracts from fillet tissue taken from fish sampled immediately after the exposure (0 min) and from fish sampled at 30 and 60 min after the exposure. The depletion of 14C-eugenol residues from the fillet tissue was rapid (t1/2 = 26.25 min) after transferring the exposed fish to fresh flowing water.

The disappearance rate and risk assessment of thiacloprid residues in Asian pear using liquid chromatography confirmed with tandem mass spectrometry.

PubMed

Kabir, Md Humayun; Abd El-Aty, A M; Rahman, Md Musfiqur; Kim, Sung-Woo; Choi, Jeong-Heui; Lee, Young-Jun; Truong, Lieu T B; Lee, Kang-Bong; Kim, Mi-Ra; Shin, Ho-Chul; Shim, Jae-Han

2017-05-01

This study was undertaken to quantify the residue levels and propose the dissipation kinetics of thiacloprid formulated as suspension concentrate in field-incurred Asian pears grown under two different open-field conditions. Samples were extracted with 20% distilled water in acetonitrile; partitioned with brine water and dichloromethane; and purified with a Florisil solid phase extraction cartridge. The analyte was identified with an LC ultraviolet detector, and field-incurred samples were confirmed using LC-MS/MS. The calibration curve was linear over the range 0.05-5.0 mg/L with a satisfactory coefficient of determination (R 2  = 0.9994). The limits of detection and limits of quantification (LOQ) were 0.003 and 0.01 mg/kg, respectively. The recovery rate fortified to blank samples at LOQ, 10× LOQ, and the maximum residue limit (MRL) were between 73.7 and 86.2% with relative standard deviation ≤9.0%. The residual concentrations at both sites were considerably lower than the MRL (0.7 mg/kg) set by the Korean Ministry of Food Drug Safety, with biological half-lives of 5.0 and 7.4 days, for sites 1 and 2, respectively. From the pre-harvest residue limit curve, it was predicted that if the residues were <1.13 or 1.40 mg/kg 10 days before harvest, the residue level would be lower than the MRL during harvest. Risk assessment on day 0 showed an acceptable daily intake (%) of 13.0% and 11.0% for sites 1 and site 2, respectively, which indicates that the residual amounts are not hazardous to the Korean population. Copyright © 2016 John Wiley & Sons, Ltd.

Successive monitoring surveys of selected banned and restricted pesticide residues in vegetables from the northwest region of China from 2011 to 2013.

PubMed

Yu, Yan; Hu, Senke; Yang, Yuxuan; Zhao, Xiaodan; Xue, Jianjun; Zhang, Jinghua; Gao, Song; Yang, Aimin

2017-08-02

A wide range of pesticides is applied for crop protection in vegetable cultivation in China. Regulation of pesticide maximum residue limits (MRLs) in vegetables is established but not fully enforced. And pesticide residues in vegetables were not well monitored. This study conducted the monitoring surveys from 2011 to 2013 to investigate the pesticides in vegetables in the northwest region of China. A multi-residue gas chromatography/mass spectrometry method (GC/MS) was used in determination of pesticides in vegetable samples. The χ 2 test was used to compare the concentration of pesticide residues. A total of 32 pesticide residues were detected in 518 samples from 20 types of vegetables in this study. 7.7% of the detected pesticide residues exceeded the MRLs. The percentages of residues that exceeded the MRLs for leafy, melon and fruit, and root vegetables were 11.2%, 5.1%, and 1.6%, respectively. There was no seasonal difference in the proportion of samples that exceeded the MRLs in different vegetables. A total of 84.3% (27/32) pesticides were detected at concentrations that exceeded MRLs. And of the 27 pesticides that exceeded the MRLs, 11 (40.7%) were banned for use in agriculture. The most frequently detected pesticides were Malathion (9.4%), Dichlorvos (8.7%), and Dimethoate (8.1%). The observed high rate of pesticides detected and high incidence of pesticide detection exceeding their MRLs in the commonly consumed vegetables indicated that the Good Agricultural Practices (GAP) may not be well followed. The management of pesticide use and control should be improved. Well-developed training programs should be initiated to improve pesticide application knowledge for farmers.

Insecticide residues in Australian plague locusts (Chortoicetes terminifera Walker) after ultra-low volume aerial application of the organophosphorus insecticide fenitrothion.

PubMed

Story, Paul G; Mineau, Pierre; Mullié, Wim C

2013-12-01

The need for locust control throughout eastern Australia during spring 2010 provided an opportunity to quantify residues of the organophosphorus insecticide fenitrothion on nymphs of the Australian plague locust, Chortoicetes terminifera Walker. Residues were collected across the different physiological states--live, dead, and debilitated (characterized by ease of capture, erratic hopping, and the inability to remain upright)--of locust nymphs observed following exposure to fenitrothion. The time course of residue depletion for 72 h after spraying was quantified, and residue-per-unit dose values in the present study were compared with previous research. Fenitrothion residue-per-unit dose values ranged from 0.2 µg/g to 31.2 µg/g (mean ± standard error [SE] = 6.3 ± 1.3 µg/g) in live C. terminifera nymps, from 0.5 µg/g to 25.5 µg/g (7.8 ± 1.3 µg/g) in debilitated nymphs, and from 2.3 µg/g to 39.8 µg/g (16.5 ± 2.8 µg/g) in dead nymphs. Residues of the oxidative derivative of fenitrothion, fenitrooxon, were generally below the limit of quantitation for the analysis (0.02 µg/g), with 2 exceptions--1 live and 1 debilitated sample returned residues at the limit of quantitation. The results of the present study suggest that sampling of acridids for risk assessment should include mimicking predatory behavior and be over a longer time course (preferably 3-24 h postspray) than sampling of vegetation (typically 1-2 h postspray) and that current regulatory frameworks may underestimate the risk of pesticides applied for locust or grasshopper control. © 2013 SETAC.

A Novel Immunoassay Test System for Detection of Modified Allergen Residues Present in Almond-, Cashew-, Coconut-, Hazelnut-, and Soy-Based Nondairy Beverages.

PubMed

Masiri, Jongkit; Benoit, Lora; Meshgi, Mahzad; Day, Jeffrey; Nadala, Cesar; Samadpour, Mansour

2016-09-01

A growing number of plant-based milk substitutes have become commercially available, providing an array of options for consumers with dietary restrictions. Though several of these products rival cow's milk in terms of their nutritional profiles, beverages prepared with soy and tree nuts can be a significant concern to consumers because of potential contamination with food allergens. Adding to this concern is the fact that allergen residues from plant-based beverages are modified during manufacturing, thereby decreasing the sensitivity of antibody-based detection methods. Consequently, many commercially available allergen detection kits are less effective for allergens derived from nondairy milk substitutes. To address this limitation, we developed a panel of polyclonal antibodies directed against the modified proteins present in almond, cashew, coconut, hazelnut, and soy milks and incorporated them into rapid lateral flow immunoassay tests configured in both sandwich and competitive format. The tests had robust detection capabilities when used with a panel of various brand-name products, with a sensitivity of 1 ppm and selectivity values of 3 to 5 ppm in nondairy beverages. Minimal cross-reactivity to extracts prepared from common commodities was observed. The development of a highly sensitive and rapid test specifically designed to detect trace quantities of highly modified allergen residues in plant-based, dairy-free beverages will aid food manufacturers and regulatory agencies in monitoring products for these modified allergens when testing environmental and food samples.

Comparison of screening-level and Monte Carlo approaches for wildlife food web exposure modeling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pastorok, R.; Butcher, M.; LaTier, A.

1995-12-31

The implications of using quantitative uncertainty analysis (e.g., Monte Carlo) and site-specific tissue residue data for wildlife exposure modeling were examined with data on trace elements at the Clark Fork River Superfund Site. Exposure of white-tailed deer, red fox, and American kestrel was evaluated using three approaches. First, a screening-level exposure model was based on conservative estimates of exposure parameters, including estimates of dietary residues derived from bioconcentration factors (BCFs) and soil chemistry. A second model without Monte Carlo was based on site-specific data for tissue residues of trace elements (As, Cd, Cu, Pb, Zn) in key dietary species andmore » plausible assumptions for habitat spatial segmentation and other exposure parameters. Dietary species sampled included dominant grasses (tufted hairgrass and redtop), willows, alfalfa, barley, invertebrates (grasshoppers, spiders, and beetles), and deer mice. Third, the Monte Carlo analysis was based on the site-specific residue data and assumed or estimated distributions for exposure parameters. Substantial uncertainties are associated with several exposure parameters, especially BCFS, such that exposure and risk may be greatly overestimated in screening-level approaches. The results of the three approaches are compared with respect to realism, practicality, and data gaps. Collection of site-specific data on trace elements concentrations in plants and animals eaten by the target wildlife receptors is a cost-effective way to obtain realistic estimates of exposure. Implications of the results for exposure and risk estimates are discussed relative to use of wildlife exposure modeling and evaluation of remedial actions at Superfund sites.« less

Determination of regulatory ionophore coccidiostat residues in feedstuffs at carry-over levels by liquid chromatography-mass spectrometry

PubMed Central

Stramenga, Arianna; Colagrande, Maria Novella; Campana, Guido; Scortichini, Giampiero; Migliorati, Giacomo; Compagnone, Dario

2017-01-01

In this study samples of feedstuffs were collected from different feed mills and animal farms located in central Italy and analyzed for ionophore coccidiostat residues at carry-over levels by liquid chromatography-mass spectrometry. Since unavoidable cross-contamination of feedstuffs may occur during their production as well as distribution and storage, the collection of samples covered all these different stages. Residues of lasalocid, monensin, salinomycin and maduramicin were detected in 32.4% of samples, both at production and storage level. The maximum content for unavoidable carry-over set by Regulation (EU) No 574/2011 was exceeded in 11.3% of samples. The variability of the results highlighted the different approach of each investigated feed business operator to avoid any cross-contamination in non-target feed. The method developed in this study can be able to detect ionophore coccidiostats at low concentrations consequent to carry-over. PMID:28792977

Contamination profiles, mass loadings, and sewage epidemiology of neuropsychiatric and illicit drugs in wastewater and river waters from a community in the Midwestern United States.

PubMed

Skees, Allie J; Foppe, Katelyn S; Loganathan, Bommanna; Subedi, Bikram

2018-08-01

In this study, residues of the neuropsychiatric and illicit drugs including stimulants, opioids, hallucinogens, antischizophrenics, sedatives, and antidepressants were determined in influent and effluent samples from a small wastewater treatment plant, a receiving creek, and river waters in the Four Rivers region of the Midwestern United States. Nineteen neuropsychiatric drugs, eight illicit drugs, and three metabolites of illicit drugs were detected and quantitated in the water samples using HPLC-MS/MS. Residual concentrations of the drugs varied from below the detection limit to sub-μg/L levels. The source of residual cocaine and benzoylecgonine in wastewater is primarily from human consumption of cocaine rather than direct disposal. Wastewater based epidemiology is utilized to estimate the community usage of drugs based on the concentration of drug residues in wastewater, wastewater inflow, and the population served by the centralized wastewater treatment plant. The per-capita consumption rate of methamphetamine (1740 mg/d/1000 people) and amphetamine (970 mg/d/1000 people) found in this study were the highest reported per-capita consumption rates in the USA. Antidepressant venlafaxine found to have the highest environmental emission from the WWTP (333 ± 160 mg/d/1000 people) followed by citalopram (132 ± 60.2 mg/d/1000 people), methamphetamine (111 ± 43.6 mg/d/1000 people), and hydrocodone (108 ± 90.1 mg/d/1000 people). Bee Creek, an immediate receiving water body, is found to be a source of several neuropsychiatric and illicit drugs including methamphetamine, methadone, alprazolam, oxazepam, temazepam, carbamazepine, venlafaxine, citalopram, sertraline, oxycodone, and hydrocodone (p < 0.036) in the Clarks River. Copyright © 2018 Elsevier B.V. All rights reserved.

Magnetic graphene dispersive solid phase extraction combining high performance liquid chromatography for determination of fluoroquinolones in foods.

PubMed

He, Xin; Wang, Geng Nan; Yang, Kun; Liu, Hui Zhi; Wu, Xia Jun; Wang, Jian Ping

2017-04-15

In this study, a magnetic graphene-based dispersive solid phase extraction method was developed that was combined with high performance liquid chromatography to determine the residues of fluoroquinolone drugs in foods of animal origin. During the experiments, several parameters possible influencing the extraction performance were optimized (amount of magnetic graphene, sample pH, extraction time and elution solution). This extraction method showed high absorption capacities (>6800ng) and high enrichment factors (68-79-fold) for seven fluoroquinolones. Furthermore, this absorbent could be reused for at least 40 times. The limits of detection were in the range of 0.05-0.3ng/g, and the recoveries from the standards fortified blank samples (bovine milk, chicken muscle and egg) were in the range of 82.4-108.5%. Therefore, this method could be used as a simple and sensitive tool to determine the residues of fluoroquinolones in foods of animal origin. Copyright © 2016 Elsevier Ltd. All rights reserved.

Residual stresses investigations in composite samples by speckle interferometry and specimen repositioning

NASA Astrophysics Data System (ADS)

Baldi, Alfonso; Jacquot, Pierre

2003-05-01

Graphite-epoxy laminates are subjected to the "incremental hole-drilling" technique in order to investigate the residual stresses acting within each layer of the composite samples. In-plane speckle interferometry is used to measure the displacement field created by each drilling increment around the hole. Our approach features two particularities (1) we rely on the precise repositioning of the samples in the optical set-up after each new boring step, performed by means of a high precision, numerically controlled milling machine in the workshop; (2) for each increment, we acquire three displacement fields, along the length, the width of the samples, and at 45°, using a single symmetrical double beam illumination and a rotary stage holding the specimens. The experimental protocol is described in detail and the experimental results are presented, including a comparison with strain gages. Speckle interferometry appears as a suitable method to respond to the increasing demand for residual stress determination in composite samples.

Predictive equations for total lung capacity and residual volume calculated from radiographs in a random sample of the Michigan population.

PubMed Central

Kilburn, K H; Warshaw, R H; Thornton, J C; Thornton, K; Miller, A

1992-01-01

BACKGROUND: Published predicted values for total lung capacity and residual volume are often based on a small number of subjects and derive from different populations from predicted spirometric values. Equations from the only two large studies gave smaller predicted values for total lung capacity than the smaller studies. A large number of subjects have been studied from a population which has already provided predicted values for spirometry and transfer factor for carbon monoxide. METHODS: Total lung capacity was measured from standard posteroanterior and lateral chest radiographs and forced vital capacity by spirometry in a population sample of 771 subjects. Prediction equations were developed for total lung capacity (TLC), residual volume (RV) and RV/TLC in two groups--normal and total. Subjects with signs or symptoms of cardiopulmonary disease were combined with the normal subjects and equations for all subjects were also modelled. RESULTS: Prediction equations for TLC and RV in non-smoking normal men and women were square root transformations which included height and weight but not age. They included a coefficient for duration of smoking in current smokers. The predictive equation for RV/TLC included weight, age, age and duration of smoking for current smokers and ex-smokers of both sexes. For the total population the equations took the same form but the height coefficients and constants were slightly different. CONCLUSION: These population based prediction equations for TLC, RV and RV/TLC provide reference standards in a population that has provided reference standards for spirometry and single breath transfer factor for carbon monoxide. PMID:1412094

Expression and Functional Properties of an Anti-Triazophos High-Affinity Single-Chain Variable Fragment Antibody with Specific Lambda Light Chain

PubMed Central

Liu, Rui; Liang, Xiao; Xiang, Dandan; Guo, Yirong; Liu, Yihua; Zhu, Guonian

2016-01-01

Triazophos is a widely used organophosphorous insecticide that has potentially adverse effects to organisms. In the present study, a high-affinity single-chain variable fragment (scFv) antibody with specific lambda light chain was developed for residue monitoring. First, the specific variable regions were correctly amplified from a hybridoma cell line 8C10 that secreted monoclonal antibody (mAb) against triazophos. The regions were then assembled as scFv via splicing by overlap extension polymerase chain reaction. Subsequently, the recombinant anti-triazophos scFv-8C10 was successfully expressed in Escherichia coli strain HB2151 in soluble form, purified through immobilized metal ion affinity chromatography, and verified via Western blot and peptide mass fingerprinting analyses. Afterward, an indirect competitive enzyme-linked immunosorbent assay was established based on the purified anti-triazophos scFv-8C10 antibody. The assay exhibited properties similar to those based on the parent mAb, with a high sensitivity (IC50 of 1.73 ng/mL) to triazophos and no cross reaction for other organophosphorus pesticides; it was reliable in detecting triazophos residues in spiked water samples. Moreover, kinetic measurement using a surface plasmon resonance biosensor indicated that the purified scFv-8C10 antibody had a high affinity of 1.8 × 10−10 M and exhibited good binding stability. Results indicated that the recombinant high-affinity scFv-8C10 antibody was an effective detection material that would be promising for monitoring triazophos residues in environment samples. PMID:27338340

Observation of residues in tissues of chickens exposed to low dietary concentrations of chloramphenicol.

PubMed

Rejtharová, Martina; Rejthar, Libor; Čačková, Katarína; Bureš, Jiří; Vernerová, Eva; Hera, Alfred

2017-04-01

To investigate potential residues in tissues arising from naturally occurring low levels of chloramphenicol in plant material, feeding studies were conducted with chickens. A common chicken feed was prepared containing 0, 10, 50 and 200 μg kg -1 chloramphenicol and levels were confirmed by LC-MS/MS. Four separate groups of broiler chickens, eight animals in each group, were fed all their 35-day life with this contaminated feed. They were allowed ad libitum access to this feed and fresh water. After slaughtering the chickens, the residues in muscle and liver tissues were determined using GC/MS-NCI method. No residues were detected in tissues of animals from groups fed with feed containing 0, 10 or 50 µg kg -1 . Low chloramphenicol residual concentrations were observed in a few of the muscle samples obtained from the group of chickens fed with feed containing chloramphenicol in added concentration 200 µg kg -1 . No residues were detected in the remaining samples of this group. These results indicate that when residues of chloramphenicol are detected it is in all probability through illegal use.

Fruit and vegetable intake and their pesticide residues in relation to semen quality among men from a fertility clinic

PubMed Central

Chiu, Y.H.; Afeiche, M.C.; Gaskins, A.J.; Williams, P.L.; Petrozza, J.C.; Tanrikut, C.; Hauser, R.; Chavarro, J.E.

2015-01-01

STUDY QUESTION Is consumption of fruits and vegetables with high levels of pesticide residues associated with lower semen quality? SUMMARY ANSWER Consumption of fruits and vegetables with high levels of pesticide residues was associated with a lower total sperm count and a lower percentage of morphologically normal sperm among men presenting to a fertility clinic. WHAT IS KNOWN ALREADY Occupational and environmental exposure to pesticides is associated with lower semen quality. Whether the same is true for exposure through diet is unknown. STUDY DESIGN, SIZE, DURATION Men enrolled in the Environment and Reproductive Health (EARTH) Study, an ongoing prospective cohort at an academic medical fertility center. Male partners (n = 155) in subfertile couples provided 338 semen samples during 2007–2012. PARTICIPANTS/MATERIALS, SETTING, METHODS Semen samples were collected over an 18-month period following diet assessment. Sperm concentration and motility were evaluated by computer-aided semen analysis (CASA). Fruits and vegetables were categorized as containing high or low-to-moderate pesticide residues based on data from the annual United States Department of Agriculture Pesticide Data Program. Linear mixed models were used to analyze the association of fruit and vegetable intake with sperm parameters accounting for within-person correlations across repeat samples while adjusting for potential confounders. MAIN RESULTS AND THE ROLE OF CHANCE Total fruit and vegetable intake was unrelated to semen quality parameters. High pesticide residue fruit and vegetable intake, however, was associated with poorer semen quality. On average, men in highest quartile of high pesticide residue fruit and vegetable intake (≥1.5 servings/day) had 49% (95% confidence interval (CI): 31%, 63%) lower total sperm count and 32% (95% CI: 7%, 58%) lower percentage of morphologically normal sperm than men in the lowest quartile of intake (<0.5 servings/day) (P, trend = 0.003 and 0.02, respectively). Low-to-moderate pesticide residue fruit and vegetable intake was associated with a higher percentage of morphologically normal sperm (P, trend = 0.04). LIMITATIONS, REASONS FOR CAUTION Surveillance data, rather than individual pesticide assessment, was used to assess the pesticide residue status of fruits and vegetables. CASA is a useful method for clinical evaluation but may be considered less favorable for accurate semen analysis in the research setting. Owing to the observational nature of the study, confirmation is required by interventional studies as well. WIDER IMPLICATIONS OF THE FINDINGS To our knowledge, this is the first report on the consumption of fruits and vegetables with high levels of pesticide residue in relation to semen quality. Further confirmation of these findings is warranted. STUDY FUNDING/COMPETING INTEREST(S) Supported by National Institutes of Health grants ES009718, ES022955, ES000002, P30 DK046200 and Ruth L. Kirschstein National Research Service Award T32 DK007703-16. None of the authors has any conflicts of interest to declare. PMID:25824023

Fruit and vegetable intake and their pesticide residues in relation to semen quality among men from a fertility clinic.

PubMed

Chiu, Y H; Afeiche, M C; Gaskins, A J; Williams, P L; Petrozza, J C; Tanrikut, C; Hauser, R; Chavarro, J E

2015-06-01

Is consumption of fruits and vegetables with high levels of pesticide residues associated with lower semen quality? Consumption of fruits and vegetables with high levels of pesticide residues was associated with a lower total sperm count and a lower percentage of morphologically normal sperm among men presenting to a fertility clinic. Occupational and environmental exposure to pesticides is associated with lower semen quality. Whether the same is true for exposure through diet is unknown. Men enrolled in the Environment and Reproductive Health (EARTH) Study, an ongoing prospective cohort at an academic medical fertility center. Male partners (n = 155) in subfertile couples provided 338 semen samples during 2007-2012. Semen samples were collected over an 18-month period following diet assessment. Sperm concentration and motility were evaluated by computer-aided semen analysis (CASA). Fruits and vegetables were categorized as containing high or low-to-moderate pesticide residues based on data from the annual United States Department of Agriculture Pesticide Data Program. Linear mixed models were used to analyze the association of fruit and vegetable intake with sperm parameters accounting for within-person correlations across repeat samples while adjusting for potential confounders. Total fruit and vegetable intake was unrelated to semen quality parameters. High pesticide residue fruit and vegetable intake, however, was associated with poorer semen quality. On average, men in highest quartile of high pesticide residue fruit and vegetable intake (≥1.5 servings/day) had 49% (95% confidence interval (CI): 31%, 63%) lower total sperm count and 32% (95% CI: 7%, 58%) lower percentage of morphologically normal sperm than men in the lowest quartile of intake (<0.5 servings/day) (P, trend = 0.003 and 0.02, respectively). Low-to-moderate pesticide residue fruit and vegetable intake was associated with a higher percentage of morphologically normal sperm (P, trend = 0.04). Surveillance data, rather than individual pesticide assessment, was used to assess the pesticide residue status of fruits and vegetables. CASA is a useful method for clinical evaluation but may be considered less favorable for accurate semen analysis in the research setting. Owing to the observational nature of the study, confirmation is required by interventional studies as well. To our knowledge, this is the first report on the consumption of fruits and vegetables with high levels of pesticide residue in relation to semen quality. Further confirmation of these findings is warranted. Supported by National Institutes of Health grants ES009718, ES022955, ES000002, P30 DK046200 and Ruth L. Kirschstein National Research Service Award T32 DK007703-16. None of the authors has any conflicts of interest to declare. © The Author 2015. Published by Oxford University Press on behalf of the European Society of Human Reproduction and Embryology. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Neonicotinoid Insecticide Residues in Surface Water and Soil Associated with Commercial Maize (Corn) Fields in Southwestern Ontario

PubMed Central

Schaafsma, Arthur; Limay-Rios, Victor; Baute, Tracey; Smith, Jocelyn; Xue, Yingen

2015-01-01

Neonicotinoid insecticides have come under scrutiny for their potential unintended effects on non-target organisms, particularly pollinators in agro-ecosystems. As part of a larger study of neonicotinoid residues associated with maize (corn) production, 76 water samples within or around the perimeter of 18 commercial maize fields and neighbouring apiaries were collected in 5 maize-producing counties of southwestern Ontario. Residues of clothianidin (mean = 2.28, max. = 43.60 ng/mL) and thiamethoxam (mean = 1.12, max. = 16.50 ng/mL) were detected in 100 and 98.7% of the water samples tested, respectively. The concentration of total neonicotinoid residues in water within maize fields increased six-fold during the first five weeks after planting, and returned to pre-plant levels seven weeks after planting. However, concentrations in water sampled from outside the fields were similar throughout the sampling period. Soil samples from the top 5 cm of the soil profile were also collected in these fields before and immediately following planting. The mean total neonicotinoid residue was 4.02 (range 0.07 to 20.30) ng/g, for samples taken before planting, and 9.94 (range 0.53 to 38.98) ng/g, for those taken immediately after planting. Two soil samples collected from within an conservation area contained detectable (0.03 and 0.11 ng/g) concentrations of clothianidin. Of three drifted snow samples taken, the drift stratum containing the most wind-scoured soil had 0.16 and 0.20 ng/mL mainly clothianidin in the melted snow. The concentration was at the limit of detection (0.02 ng/mL) taken across the entire vertical profile. With the exception of one sample, water samples tested had concentrations below those reported to have acute, chronic or sublethal effects to honey bees. Our results suggest that neonicotinoids may move off-target by wind erosion of contaminated soil. These results are informative to risk assessment models for other non-target species in maize agro-ecosytems. PMID:25710560

Degradation kinetics and safety evaluation of buprofezin residues in grape (Vitis vinifera L.) and three different soils of India.

PubMed

Oulkar, Dasharath P; Banerjee, Kaushik; Patil, Sangram H; Upadhyay, Ajay K; Taware, Praveen B; Deshmukh, Madhukar B; Adsule, Pandurang G

2009-02-01

This work was undertaken to determine the preharvest interval (PHI) of buprofezin to minimize its residues in grapes and thereby ensure consumer safety and avoid possible non-compliance in terms of residue violations in export markets. Furthermore, the residue dynamics in three grapevine soils of India was explored to assess its environmental safety. Residues dissipated following non-linear two-compartment first + first-order kinetics. In grapes, the PHI was 31 days at both treatments (312.5 and 625 g a.i. ha(-1)), with the residues below the maximum permissible intake even 1 h after foliar spraying. Random sampling of 5 kg comprising small bunchlets (8-10 berries) collected from a 1 ha area gave satisfactory homogeneity and representation of the population. A survey on the samples harvested after the PHI from supervised vineyards that received treatment at the recommended dose showed residues below the maximum residue limit (MRL) of 0.02 mg kg(-1) applicable for the European Union. In soil, the degradation rate was fastest in clay soil, followed by sandy loam and silty clay, with a half-life within 16 days in all the soils. The recommendation of the PHI proved to be effective in minimizing buprofezin residues in grapes. Thus, this work is of high practical significance to the domestic and export grape industry of India to ensure safety compliance in respect of buprofezin residues, keeping in view the requirements of international trade.

Nonlinear vibrational microscopy

DOEpatents

Holtom, Gary R.; Xie, Xiaoliang Sunney; Zumbusch, Andreas

2000-01-01

The present invention is a method and apparatus for microscopic vibrational imaging using coherent Anti-Stokes Raman Scattering or Sum Frequency Generation. Microscopic imaging with a vibrational spectroscopic contrast is achieved by generating signals in a nonlinear optical process and spatially resolved detection of the signals. The spatial resolution is attained by minimizing the spot size of the optical interrogation beams on the sample. Minimizing the spot size relies upon a. directing at least two substantially co-axial laser beams (interrogation beams) through a microscope objective providing a focal spot on the sample; b. collecting a signal beam together with a residual beam from the at least two co-axial laser beams after passing through the sample; c. removing the residual beam; and d. detecting the signal beam thereby creating said pixel. The method has significantly higher spatial resolution then IR microscopy and higher sensitivity than spontaneous Raman microscopy with much lower average excitation powers. CARS and SFG microscopy does not rely on the presence of fluorophores, but retains the resolution and three-dimensional sectioning capability of confocal and two-photon fluorescence microscopy. Complementary to these techniques, CARS and SFG microscopy provides a contrast mechanism based on vibrational spectroscopy. This vibrational contrast mechanism, combined with an unprecedented high sensitivity at a tolerable laser power level, provides a new approach for microscopic investigations of chemical and biological samples.

A novel multiplexed fluorescence polarisation immunoassay based on a recombinant bi-specific single-chain diabody for simultaneous detection of fluoroquinolones and sulfonamides in milk.

PubMed

Chen, Min; Wen, Kai; Tao, Xiaoqi; Ding, Shuangyang; Xie, Jie; Yu, Xuezhi; Li, Jiancheng; Xia, Xi; Wang, Yang; Xie, Sanlei; Jiang, Haiyang

2014-01-01

Major research efforts are focusing on the development of simultaneous multiplexed immunoassays. In this study, a novel dual-binding fluorescence polarisation immunoassay (DB-FPIA) using a broad-specificity bi-specific single-chain diabody (scDb) and two fluorescent-labelled tracers (sulfamethoxypyridazine-fluorescein isothiocyanate (SMP-FITC) and sarafloxacin-Texas Red (SAR-TR)) with different excitation and emission wavelengths was developed for simultaneous and high-throughput detection of 19 fluoroquinolones (FQs) and 13 sulfonamides (SAs) at the maximum residue limits in milk samples. Recoveries for spiked milk samples were from 76.4% to 128.4%, with a relative standard deviation lower than 13.9%. The developed DB-FPIA was then applied to field samples, followed by confirmation by LC-MS/MS. All three instances in which FQs and SAs were present at concentrations near or above the assay limit of detection were identified as positive by the developed DB-FPIA, demonstrating that the method is suitable for rapid screening of FQs and SAs contamination. The novel methodology combines the advantage of the FPIA and the broad sensitivity of scDb and shows great promise for fast multi-analyte screening of low-molecular weight chemical residues in food samples.

Determination of Pesticides Residues in Cucumbers Grown in Greenhouse and the Effect of Some Procedures on Their Residues.

PubMed

Leili, Mostafa; Pirmoghani, Amin; Samadi, Mohammad Taghi; Shokoohi, Reza; Roshanaei, Ghodratollah; Poormohammadi, Ali

2016-11-01

The objective of this study was to determine the residual concentrations of ethion and imidacloprid in cucumbers grown in greenhouse. The effect of some simple processing procedures on both ethion and imidacloprid residues were also studied. Ten active greenhouses that produce cucumber were randomly selected. Ethion and imidacloprid as the most widely used pesticides were measured in cucumber samples of studied greenhouses. Moreover, the effect of storing, washing, and peeling as simple processing procedures on both ethion and imidacloprid residues were investigated. One hour after pesticide application; the maximum residue levels (MRLs) of ethion and imidacloprid were higher than that of Codex standard level. One day after pesticide application, the levels of pesticides were decreased about 35 and 31% for ethion and imidacloprid, respectively, which still were higher than the MRL. Washing procedure led to about 51 and 42.5% loss in ethion and imidacloprid residues, respectively. Peeling procedure also led to highest loss of 93.4 and 63.7% in ethion and imidacloprid residues, respectively. The recovery for both target analytes was in the range between 88 and 102%. The residue values in collected samples one hour after pesticides application were higher than standard value. The storing, washing, and peeling procedures lead to the decrease of pesticide residues in greenhouse cucumbers. Among them, the peeling procedure has the greatest impact on residual reduction. Therefore, these procedures can be used as simple and effective processing techniques for reducing and removing pesticides from greenhouse products before their consumption.

Minimization of spurious strains by using a Si bent-perfect-crystal monochromator: neutron surface strain scanning of a shot-peened sample

NASA Astrophysics Data System (ADS)

Rebelo Kornmeier, Joana; Gibmeier, Jens; Hofmann, Michael

2011-06-01

Neutron strain measurements are critical at the surface. When scanning close to a sample surface, aberration peak shifts arise due to geometrical and divergence effects. These aberration peak shifts can be of the same order as the peak shifts related to residual strains. In this study it will be demonstrated that by optimizing the horizontal bending radius of a Si (4 0 0) monochromator, the aberration peak shifts from surface effects can be strongly reduced. A stress-free sample of fine-grained construction steel, S690QL, was used to find the optimal instrumental conditions to minimize aberration peak shifts. The optimized Si (4 0 0) monochromator and instrument settings were then applied to measure the residual stress depth gradient of a shot-peened SAE 4140 steel sample to validate the effectiveness of the approach. The residual stress depth profile is in good agreement with results obtained by x-ray diffraction measurements from an international round robin test (BRITE-EURAM-project ENSPED). The results open very promising possibilities to bridge the gap between x-ray diffraction and conventional neutron diffraction for non-destructive residual stress analysis close to surfaces.

Determination of 10 sulfonamide residues in meat samples by liquid chromatography with ultraviolet detection.

PubMed

Di Sabatino, Marcello; Di Pietra, Anna Maria; Benfenati, Luigi; Di Simone, Bruno

2007-01-01

A liquid chromatography (LC) method is described for the simultaneous determination of 10 commonly used sulfonamide drug residues in meat. The 10 sulfonamide drugs of interest were sulfadiazine, sulfathiazole, sulfamerazine, sulfadimidine, sulfamethizole, sulfamonomethoxine, sulfachloropyridazine, sulfadoxine, sulfadimethoxine, and sulfaquinoxaline. The residues were extracted with acetone-chloroform (1 + 1). Sulfonamides were quantitatively retained in the extracting solution and afterwards eluted from a cation-exchanger solid-phase extraction cartridge with a solution of methanol-aqueous ammonia. The solution was dried, reconstituted with 5 mL methanol and filtered before analysis by LC-ultraviolet using a C18 column with a mobile phase gradient of potassium dihydrogen phosphate buffer, pH 2.5, and methanol-acetonitrile (30 + 70, v/v). The method was applied to cattle, swine, chicken, and sheep muscle tissues. The validation was performed with a fortified cattle meat sample at level of 100 ppb, which is the administrative maximum residue limit for sulfonamides in the European Union. The limit of quantitation for all sulfonamides was between 3 and 14 ppb. Recovery was evaluated for different meat matrixes. The mean recovery values were between 66.3% for pork meat samples and 71.5% for cattle meat samples.

Assessment of pesticide contamination in soil samples from an intensive horticulture area, using ultrasonic extraction and gas chromatography-mass spectrometry.

PubMed

Gonçalves, C; Alpendurada, M F

2005-03-15

In order to reduce the amount of sample to be collected and the time consumed in the analytical process, a broad range of analytes should be preferably considered in the same analytical procedure. A suitable methodology for pesticide residue analysis in soil samples was developed based on ultrasonic extraction (USE) and gas chromatography-mass spectrometry (GC-MS). For this study, different classes of pesticides were selected, both recent and old persistent molecules: parent compounds and degradation products, namely organochlorine, organophosphorous and pyrethroid insecticides, triazine and acetanilide herbicides and other miscellaneous pesticides. Pesticide residues could be detected in the low- to sub-ppb range (0.05-7.0mugkg(-1)) with good precision (7.5-20.5%, average 13.7% R.S.D.) and extraction efficiency (69-118%, average 88%) for the great majority of analytes. This methodology has been applied in a monitoring program of soil samples from an intensive horticulture area in Póvoa de Varzim, North of Portugal. The pesticides detected in four sampling programs (2001/2002) were the following: lindane, dieldrin, endosulfan, endosulfan sulfate, 4,4'-DDE, 4,4'-DDD, atrazine, desethylatrazine, alachlor, dimethoate, chlorpyrifos, pendimethalin, procymidone and chlorfenvinphos. Pesticide contamination was investigated at three depths and in different soil and crop types to assess the influence of soil characteristics and trends over time.

Deposition and residues of azoxystrobin and imidacloprid on greenhouse lettuce with implications for human consumption.

PubMed

Itoiz, Eva Sevigné; Fantke, Peter; Juraske, Ronnie; Kounina, Anna; Vallejo, Assumpció Antón

2012-11-01

Lettuce greenhouse experiments were carried out from March to June 2011 in order to analyze how pesticides behave from the time of application until their intake via human consumption taking into account the primary distribution of pesticides, field dissipation, and post-harvest processing. In addition, experimental conditions were used to evaluate a new dynamic plant uptake model comparing its results with the experimentally derived residues. One application of imidacloprid and two of azoxystrobin were conducted. For evaluating primary pesticide distribution, two approaches based on leaf area index and vegetation cover were used and results were compared with those obtained from a tracer test. High influence of lettuce density, growth stage and type of sprayer was observed in primary distribution showing that low densities or early growth stages implied high losses of pesticides on soil. Washed and unwashed samples of lettuce were taken and analyzed from application to harvest to evaluate removal of pesticides by food processing. Results show that residues found on the Spanish preharvest interval days were in all cases below officially set maximum residue limits, although it was observed that time between application and harvest is as important for residues as application amounts. An overall reduction of 40-60% of pesticides residues was obtained from washing lettuce. Experimentally derived residues were compared with modeled residues and deviate from 1.2 to 1.4 for imidacloprid and azoxystrobin, respectively, presenting good model predictions. Resulting human intake fractions range from 0.045 kg(intake) kg(applied)(-1) for imidacloprid to 0.14 kg(intake) kg(applied)(-1) for azoxystrobin. Copyright © 2012 Elsevier Ltd. All rights reserved.

Agricultural chemicals in groundwater of the midwestern United States: Relations to land use

USGS Publications Warehouse

Kolpin, D.W.

1997-01-01

To determine the relations between land use and concentrations of selected agricultural chemicals (nitrate, atrazine residue [atrazine (2-chloro-4-ethylamino-6-isopropylamino-s-triazine) + deethylatrazinc (2-amino-4-chloro-6-isopropylamino-s-triazine) + deisopropylatrazine (2-amino-4-chloro-6-ethylamino-s-triazine)], and alachlor residue [alachlor, [2-chloro-2′,6′-diethyl-N-(methoxymethyl) acetanilide] + alachlor ethanesulfonic acid (alachlor-ESA; 2-[(2,6-diethylphenyl)(methoxymethyl)amino]-2-oxoethanesulfonic acid)] in groundwater, detailed land use information based on accurate measurements from aerial photographs for the 1991 growing season was obtained within a 2-km radius surrounding 100 wells completed in near-surface unconsolidated aquifers in the midwestern USA. The most significant land use factors to the agricultural chemicals examined were: nitrate (amount of irrigated crop production, positive relation), atrazine residue (amount of irrigated crop production, positive relation), and alachlor residue (amount of highly erodible land, inverse relation). The investigation of smaller buffer sizes (size of circular area around sampled wells) proved insightful for this study. Additional land use factors having significant relations to all three agricultural chemicals were identified using these smaller buffer radii. The most significant correlations (correlation maxima) generally occurred at ≤500-m for nitrate and ≥1000-m for atrazine residue and alachlor residue. An attempt to improve the statistical relations to land use by taking hydrologic considerations into account (removing land outside the estimated most probable recharge area from the statistical analysis) was not as successful as anticipated. Only 45% of the nitrate, 32% of the atrazine residue, and 20% of the alachlor residue correlations were improved by a consideration of the estimated most probable recharge area.

Ten year regeneration of southern Appalachian hardwood clearcuts after controlling residual trees

Treesearch

P.M. Zaldivar-Garcia; D.T. Tew

1991-01-01

Two upland hardwood stands were clearcut in 1978 and three treatments to control the unmerchantable and/or cull trees were applied. The treatments applied to the residual trees were chainsaw felling, herbicide injection, and a control, where residual trees were left standing. Regeneration was sampled 10 years after the cutting.

Noble Gases in the Hamlet Meteorite (LL4)

NASA Astrophysics Data System (ADS)

Amari, S.; Sabe, Y.; Shiraishi, T.; Matsuda, J.

2014-09-01

We analyzed noble gases in a bulk sample and an HF-HCl residue of Hamlet (LL4). The Xe composition of the residue shows that no diamond is contained in the residue. The 20Ne/22Ne ratio of Hamlet Ne-Q has been determined to be 11.0 ± 0.5.

40 CFR 141.533 - What data must my system collect to calculate a disinfection profile?

Code of Federal Regulations, 2014 CFR

2014-07-01

... at each residual disinfectant concentration sampling point during peak hourly flow; (b) If your system uses chlorine, the pH of the disinfected water at each residual disinfectant concentration...; and (d) The residual disinfectant concentration(s) (“C”) of the water before or at the first customer...

40 CFR 141.533 - What data must my system collect to calculate a disinfection profile?

Code of Federal Regulations, 2013 CFR

2013-07-01

... at each residual disinfectant concentration sampling point during peak hourly flow; (b) If your system uses chlorine, the pH of the disinfected water at each residual disinfectant concentration...; and (d) The residual disinfectant concentration(s) (“C”) of the water before or at the first customer...

40 CFR 141.533 - What data must my system collect to calculate a disinfection profile?

Code of Federal Regulations, 2011 CFR

2011-07-01

... at each residual disinfectant concentration sampling point during peak hourly flow; (b) If your system uses chlorine, the pH of the disinfected water at each residual disinfectant concentration...; and (d) The residual disinfectant concentration(s) (“C”) of the water before or at the first customer...

40 CFR 141.533 - What data must my system collect to calculate a disinfection profile?

Code of Federal Regulations, 2012 CFR

2012-07-01

... at each residual disinfectant concentration sampling point during peak hourly flow; (b) If your system uses chlorine, the pH of the disinfected water at each residual disinfectant concentration...; and (d) The residual disinfectant concentration(s) (“C”) of the water before or at the first customer...

Enhanced Cleaning of Genesis Solar Wind Sample 61348 for Film Residue Removal

NASA Technical Reports Server (NTRS)

Allums, K. K.; Gonzalez, C. P.; Kuhlman, K. R.; Allton, J. H.

2015-01-01

The Genesis mission returned to Earth on September 8, 2004, experiencing a nonnominal reentry. During the recovery of the collector materials from the capsule, many of the collector fragments were placed on the adhesive protion of post-it notes to prevent the fragments from moving during transport back to Johnson Space Center. This unknowingly provided an additional contaminate that would prove difficult to remove with the limited chemistries allowed in the Genesis Curation Laboratory. Generally when collector material samples are prepared for allocation to PIs, the samples are cleaned front side only with Ultra-Pure Water (UPW) via megasonic dispersion to the collector surface to remove crash debris and contamination. While this cleaning method works well on samples that were not placed on post-its during recovery, it has caused movement of the residue on the back of the sample to be deposited on the front in at least two examples. Therefore, samples placed on the adhesive portion on post-it note, require enhanced cleaning methods since post-it residue has proved resistant to UPW cleaning.

Research results: preserving newborn blood samples.

PubMed

Lewis, Michelle Huckaby; Scheurer, Michael E; Green, Robert C; McGuire, Amy L

2012-11-07

Retention and use, without explicit parental permission, of residual dried blood samples from newborn screening has generated public controversy over concerns about violations of family privacy rights and loss of parental autonomy. The public debate about this issue has included little discussion about the destruction of a potentially valuable public resource that can be used for research that may yield improvements in public health. The research community must advocate for policies and infrastructure that promote retention of residual dried blood samples and their use in biomedical research.

Pesticide Residues on Three Cut Flower Species and Potential Exposure of Florists in Belgium.

PubMed

Toumi, Khaoula; Vleminckx, Christiane; van Loco, Joris; Schiffers, Bruno

2016-09-23

In order to assess the prevalence of pesticide contamination and the risk of florists' exposure when handling cut flowers, sampling and analysis of 90 bouquets of the most commonly sold cut flowers in Belgium (50 bouquets of roses; 20 of gerberas, and 20 of chrysanthemums) were carried out. The bouquets were collected from 50 florists located in the seven largest cities of Belgium (Antwerp, Brussels, Charleroi, Ghent, Leuven, Liege, and Namur) and from five supermarkets located in the different regions. To have a better understanding of the route of exposure and professional practices a questionnaire was also addressed to a group of 25 florists who volunteered to take part in the survey. All florists were interviewed individually when collecting the questionnaire. The residual pesticide deposit values on cut flowers were determined in an accredited laboratory using a multi-residue (QuEChERS Quick Easy Cheap Effective Rugged Safe) method and a combination of gas chromatography (GC) and liquid chormatograhphy (LC) analysis. A total of 107 active substances were detected from all samples; i.e., an average of about 10 active substances per bouquet. The most severely contaminated bouquet accumulated a total concentration of residues up to 97 mg/kg. Results show that roses are the most contaminated cut flowers; with an average of 14 substances detected per sample and a total concentration per rose sample of 26 mg/kg. Some active substances present an acute toxicity (acephate, methiocarb, monocrotophos, methomyl, deltamethrin, etc.) and exposure can generate a direct effect on the nervous system of florists. Nevertheless, fungicides (dodemorph, propamocarb, and procymidone) were the most frequently detected in samples and had the highest maximum concentrations out of all the active substances analysed. Dodemorph was the most frequently detected substance with the highest maximum concentration (41.9 mg/kg) measured in the rose samples. It appears from the survey that, despite being exposed to high deposits of residues, florists usually do not protect themselves from contact with residues even if they spend several hours handling cut flowers and preparing bouquets (from 2 to 6 h/day, depending on the time of year and/or selling periods) daily. Bad habits (eating, drinking, or smoking at work) and absence of personal protective equipment of most florists also increase the risk of contact with pesticide residues.

Pesticide Residues on Three Cut Flower Species and Potential Exposure of Florists in Belgium

PubMed Central

Toumi, Khaoula; Vleminckx, Christiane; van Loco, Joris; Schiffers, Bruno

2016-01-01

In order to assess the prevalence of pesticide contamination and the risk of florists’ exposure when handling cut flowers, sampling and analysis of 90 bouquets of the most commonly sold cut flowers in Belgium (50 bouquets of roses; 20 of gerberas, and 20 of chrysanthemums) were carried out. The bouquets were collected from 50 florists located in the seven largest cities of Belgium (Antwerp, Brussels, Charleroi, Ghent, Leuven, Liege, and Namur) and from five supermarkets located in the different regions. To have a better understanding of the route of exposure and professional practices a questionnaire was also addressed to a group of 25 florists who volunteered to take part in the survey. All florists were interviewed individually when collecting the questionnaire. The residual pesticide deposit values on cut flowers were determined in an accredited laboratory using a multi-residue (QuEChERS Quick Easy Cheap Effective Rugged Safe) method and a combination of gas chromatography (GC) and liquid chormatograhphy (LC) analysis. A total of 107 active substances were detected from all samples; i.e., an average of about 10 active substances per bouquet. The most severely contaminated bouquet accumulated a total concentration of residues up to 97 mg/kg. Results show that roses are the most contaminated cut flowers; with an average of 14 substances detected per sample and a total concentration per rose sample of 26 mg/kg. Some active substances present an acute toxicity (acephate, methiocarb, monocrotophos, methomyl, deltamethrin, etc.) and exposure can generate a direct effect on the nervous system of florists. Nevertheless, fungicides (dodemorph, propamocarb, and procymidone) were the most frequently detected in samples and had the highest maximum concentrations out of all the active substances analysed. Dodemorph was the most frequently detected substance with the highest maximum concentration (41.9 mg/kg) measured in the rose samples. It appears from the survey that, despite being exposed to high deposits of residues, florists usually do not protect themselves from contact with residues even if they spend several hours handling cut flowers and preparing bouquets (from 2 to 6 h/day, depending on the time of year and/or selling periods) daily. Bad habits (eating, drinking, or smoking at work) and absence of personal protective equipment of most florists also increase the risk of contact with pesticide residues. PMID:27669276

Residues of Malathion and Metabolites in and on the Cotton Leaf vs. Toxicity to the Boll Weevil

Treesearch

D.A. Wolfenbarger

2002-01-01

Malathion was applied at 12 and 16 oz [A.l.]/a to cotton near Mercedes, TX, in 1995 and sampled on 0, 2, 4 and 6 d posttreatment to determine residues of malathion, malaoxon, and iso-malathion. Residues were then compared to determine toxicity to boll weevil, Anthonomus grandis Boheman. Residues of malathion comprised 99% of the leaf washes and 100% of the leaf...

Transcriptomic markers meet the real world: finding diagnostic signatures of corticosteroid treatment in commercial beef samples

PubMed Central

2012-01-01

Background The use of growth-promoters in beef cattle, despite the EU ban, remains a frequent practice. The use of transcriptomic markers has already proposed to identify indirect evidence of anabolic hormone treatment. So far, such approach has been tested in experimentally treated animals. Here, for the first time commercial samples were analyzed. Results Quantitative determination of Dexamethasone (DEX) residues in the urine collected at the slaughterhouse was performed by Liquid Chromatography-Mass Spectrometry (LC-MS). DNA-microarray technology was used to obtain transcriptomic profiles of skeletal muscle in commercial samples and negative controls. LC-MS confirmed the presence of low level of DEX residues in the urine of the commercial samples suspect for histological classification. Principal Component Analysis (PCA) on microarray data identified two clusters of samples. One cluster included negative controls and a subset of commercial samples, while a second cluster included part of the specimens collected at the slaughterhouse together with positives for corticosteroid treatment based on thymus histology and LC-MS. Functional analysis of the differentially expressed genes (3961) between the two groups provided further evidence that animals clustering with positive samples might have been treated with corticosteroids. These suspect samples could be reliably classified with a specific classification tool (Prediction Analysis of Microarray) using just two genes. Conclusions Despite broad variation observed in gene expression profiles, the present study showed that DNA-microarrays can be used to find transcriptomic signatures of putative anabolic treatments and that gene expression markers could represent a useful screening tool. PMID:23110699

Susceptibility-matched plugs for microcoil NMR probes

NASA Astrophysics Data System (ADS)

Kc, Ravi; Gowda, Yashas N.; Djukovic, Danijel; Henry, Ian D.; Park, Gregory H. J.; Raftery, Daniel

2010-07-01

For mass-limited samples, the residual sample volume outside the detection coil is an important concern, as is good base line resolution. Here, we present the construction and evaluation of magnetic susceptibility-matched plugs for microcoil NMR sample cells which address these issues. Mixed-epoxy glue and ultem tube plugs that have susceptibility values close to those of perfluorocarbon FC-43 (fluorinert) and copper were used in small volume (0.5-2 μL) and larger volume (15-20 μL) thin glass capillary sample cells. Using these plugs, the sample volume efficiency (i.e. ratio of active volume to total sample volume in the microcoil NMR cell) was improved by 6-12-fold without sensitivity and resolution trade-offs. Comparison with laser etched or heat etched microcoil sample cells is provided. The approaches described are potentially useful in metabolomics for biomarkers detection in mass limited biological samples.

Susceptibility-matched plugs for microcoil NMR probes.

PubMed

Kc, Ravi; Gowda, Yashas N; Djukovic, Danijel; Henry, Ian D; Park, Gregory H J; Raftery, Daniel

2010-07-01

For mass-limited samples, the residual sample volume outside the detection coil is an important concern, as is good base line resolution. Here, we present the construction and evaluation of magnetic susceptibility-matched plugs for microcoil NMR sample cells which address these issues. Mixed-epoxy glue and ultem tube plugs that have susceptibility values close to those of perfluorocarbon FC-43 (fluorinert) and copper were used in small volume (0.5-2 microL) and larger volume (15-20 microL) thin glass capillary sample cells. Using these plugs, the sample volume efficiency (i.e. ratio of active volume to total sample volume in the microcoil NMR cell) was improved by 6-12-fold without sensitivity and resolution trade-offs. Comparison with laser etched or heat etched microcoil sample cells is provided. The approaches described are potentially useful in metabolomics for biomarkers detection in mass limited biological samples. Copyright (c) 2010 Elsevier Inc. All rights reserved.

Susceptibility-matched plugs for microcoil NMR probes

PubMed Central

Kc, Ravi; Gowda, Yashas N.; Djukovic, Danijel; Henry, Ian D; Park, Gregory H J; Raftery, Daniel

2010-01-01

For mass limited samples, the residual sample volume outside the detection coil is an important concern, as is good base line resolution. Here, we present the construction and evaluation of magnetic susceptibility-matched plugs for microcoil NMR sample cells which address these issues. Mixed-epoxy glue and ultem tube plugs that have susceptibility values close to those of perfluorocarbon FC-43 (fluorinert) and copper were used in small volume (0.5 to 2 μL) and larger volume (15 to 20 μL) thin glass capillary sample cells. Using these plugs, the sample volume efficiency (i.e. ratio of active volume to total sample volume in the microcoil NMR cell) was improved by 6 to 12 fold without sensitivity and resolution trade-offs. Comparison with laser etched or heat etched microcoil sample cells is provided. The approaches described are potentially useful in metabolomics for biomarkers detection in mass limited biological samples. PMID:20510638

Short communication: use of the BetaStar Plus assay for detection of ceftiofur antimicrobial residues in milk from individual cows following intramammary treatment for mastitis.

PubMed

Grooms, D L; Norby, B; Grooms, K E; Jagodzinski, E N; Erskine, R J; Halbert, L W; Coetzee, J F; Wulf, L; Rice, J A

2015-09-01

Development and use of on-farm assays to detect antimicrobial residues in milk is important to reduce the risk of violative residues in marketed milk. The objective of this study was to evaluate the effectiveness of a lateral-flow immunodiagnostic assay (BetaStar Plus, Neogen Corp., Lansing, MI) in detecting ceftiofur residues in milk from individual cows treated for mastitis. This assay is currently approved by the US Federal Drug Administration (FDA) for detecting β-lactam residues in commingled milk. Forty-five dairy cows with clinical mastitis from 4 dairy farms were enrolled and treated intramammary with 125 mg of ceftiofur hydrochloride (Spectramast LC, Zoetis, Madison, NJ) according to the manufacturer's label recommendation. Composite milk samples were collected (A) before first intramammary antimicrobial treatment, (B) before the last intramammary antimicrobial treatment, (C) the last milking of the product-labeled milk withhold, (D) the first milking after the product-labeled milk withhold had been met, and (E) 72 h after the product-labeled milk withhold had been met. Samples were tested using the BetaStar Plus assay within 48 h of collection. Parallel samples were analyzed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and for somatic cell count and milk components. The BetaStar Plus assay identified 6.7, 60.0, 46.7, 22.2, and 6.7% positive samples at each of the respective time points. The assay had sensitivity and specificity of 100 and 84.7%, respectively, compared with liquid chromatography-tandem mass spectrometry analysis using FDA published residue tolerance levels for ceftiofur (or ceftiofur metabolites) as a threshold. The BetaStar Plus assay could be useful for detecting ceftiofur residues in milk from individual cows following intramammary treatment for mastitis before the milk is shipped for processing. Copyright © 2015 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

15N CSA tensors and 15N-1H dipolar couplings of protein hydrophobic core residues investigated by static solid-state NMR

NASA Astrophysics Data System (ADS)

Vugmeyster, Liliya; Ostrovsky, Dmitry; Fu, Riqiang

2015-10-01

In this work, we assess the usefulness of static 15N NMR techniques for the determination of the 15N chemical shift anisotropy (CSA) tensor parameters and 15N-1H dipolar splittings in powder protein samples. By using five single labeled samples of the villin headpiece subdomain protein in a hydrated lyophilized powder state, we determine the backbone 15N CSA tensors at two temperatures, 22 and -35 °C, in order to get a snapshot of the variability across the residues and as a function of temperature. All sites probed belonged to the hydrophobic core and most of them were part of α-helical regions. The values of the anisotropy (which include the effect of the dynamics) varied between 130 and 156 ppm at 22 °C, while the values of the asymmetry were in the 0.32-0.082 range. The Leu-75 and Leu-61 backbone sites exhibited high mobility based on the values of their temperature-dependent anisotropy parameters. Under the assumption that most differences stem from dynamics, we obtained the values of the motional order parameters for the 15N backbone sites. While a simple one-dimensional line shape experiment was used for the determination of the 15N CSA parameters, a more advanced approach based on the ;magic sandwich; SAMMY pulse sequence (Nevzorov and Opella, 2003) was employed for the determination of the 15N-1H dipolar patterns, which yielded estimates of the dipolar couplings. Accordingly, the motional order parameters for the dipolar interaction were obtained. It was found that the order parameters from the CSA and dipolar measurements are highly correlated, validating that the variability between the residues is governed by the differences in dynamics. The values of the parameters obtained in this work can serve as reference values for developing more advanced magic-angle spinning recoupling techniques for multiple labeled samples.

Bomb swab: Can trace explosive particle sampling and detection be improved?

PubMed

Fisher, Danny; Zach, Raya; Matana, Yossef; Elia, Paz; Shustack, Shiran; Sharon, Yarden; Zeiri, Yehuda

2017-11-01

The marked increase in international terror in recent years requires the development of highly efficient methods to detect trace amounts of explosives at airports, border crossings and check points. The preferred analytical method worldwide is the ion mobility spectrometry (IMS) that is capable of detecting most explosives at the nano-gram level. Sample collection for the IMS analysis is based on swabbing of a passenger's belongings to collect possible explosive residues. The present study examines a wide range of issues related to swab-based particle collection and analysis, in the hope of gaining deeper understanding into this technique that will serve to improve the detection process. The adhesion of explosive particles to three typical materials, plastic, metal and glass, were measured using atomic force microscopy (AFM). We found that a strong contribution of capillary forces to adhesion on glass and metal surfaces renders these substrates more promising materials upon which to find and collect explosive residues. The adhesion of explosives to different swipe materials was also examined. Here we found that Muslin, Nomex ® and polyamide membrane surfaces are the most promising materials for use as swipes. Subsequently, the efficiency of multiple swipe use - for collecting explosive residues from a glass surface using Muslin, Nomex ® and Teflon™ swipes - was examined. The study suggests that swipes used in about 5-10 "sampling and analysis cycles" have higher efficiency as compared to new unused swipes. The reason for this behavior was found to be related to the increased roughness of the swipe surface following a few swab measurements. Lastly, GC-MS analysis was employed to examine the nature of contaminants collected by the three types of swipe. The relative amounts of different contaminants are reported. The existence and interference of these contaminants have to be considered in relation to the detection efficiency of the various explosives by the IMS. Copyright © 2017 Elsevier B.V. All rights reserved.

Laboratory measurements of emissions of nonmethane volatile organic compounds from biomass burning in Chinese crop residues

NASA Astrophysics Data System (ADS)

Inomata, S.; Tanimoto, H.; PAN, X.; Taketani, F.; Komazaki, Y.; Miyakawa, T.; Kanaya, Y.; Wang, Z.

2014-12-01

The emission factors (EFs) of volatile organic compounds (VOCs) from the burning of Chinese crop residue were investigated as a function of modified combustion efficiency by the laboratory experiments. The VOCs including acetonitrile, aldehydes/ketones, furan, and aromatic hydrocarbons were monitored by proton-transfer-reaction mass spectrometry. Two samples, wheat straw and rape plant, were burned in dry conditions and for some experiments wheat straw was burned under wet conditions. We compared the present data to the field data reported by Kudo et al. [2014]. The agreement between the field and laboratory data was obtained for aromatics for relatively more smoldering data of dry samples but the field data were slightly underestimated compared with the laboratory data for oxygenated VOCs (OVOCs) and acetonitrile. When the EFs from the burning of wet samples were investigated, the underestimations for OVOCs and acetonitrile were improved compared with the data of dry samples. It may be a property of the burning of crop residue in the region of high temperature and high humidity that some inside parts of piled crop residue and/or the crop residue facing on the ground are still wet. But the ratios for acetic acid/glycolaldehyde was still lower than 1. This may suggest that strong loss processes of acetic acid/glycolaldehyde are present in the fresh plume.Kudo S., H. Tanimoto, S. Inomata, S. Saito, X. L. Pan, Y. Kanaya, F. Taketani, Z. F. Wang, H. Chen, H. Dong, M. Zhang, and K. Yamaji (2014), Emissions of nonmethane volatile organic compounds from open crop residue burning in Yangtze River Delta region, China, J. Geophys. Res. Atmos., 119, 7684-7698, doi: 10.1002/2013JD021044.

Determination of linuron and related compounds in soil by microwave-assisted solvent extraction and reversed-phase liquid chromatography with UV detection.

PubMed

Molins, C; Hogendoorn, E A; Dijkman, E; Heusinkveld, H A; Baumann, R A

2000-02-11

The combination of microwave-assisted solvent extraction (MASE) and reversed-phase liquid chromatography (RPLC) with UV detection has been investigated for the efficient determination of phenylurea herbicides in soils involving the single-residue method (SRM) approach (linuron) and the multi-residue method (MRM) approach (monuron, monolinuron, isoproturon, metobromuron, diuron and linuron). Critical parameters of MASE, viz, extraction temperature, water content and extraction solvent were varied in order to optimise recoveries of the analytes while simultaneously minimising co-extraction of soil interferences. The optimised extraction procedure was applied to different types of soil with an organic carbon content of 0.4-16.7%. Besides freshly spiked soil samples, method validation included the analysis of samples with aged residues. A comparative study between the applicability of RPLC-UV without and with the use of column switching for the processing of uncleaned extracts, was carried out. For some of the tested analyte/matrix combinations the one-column approach (LC mode) is feasible. In comparison to LC, coupled-column LC (LC-LC mode) provides high selectivity in single-residue analysis (linuron) and, although less pronounced in multi-residue analysis (all six phenylurea herbicides), the clean-up performance of LC-LC improves both time of analysis and sample throughput. In the MRM approach the developed procedure involving MASE and LC-LC-UV provided acceptable recoveries (range, 80-120%) and RSDs (<12%) at levels of 10 microg/kg (n=9) and 50 microg/kg (n=7), respectively, for most analyte/matrix combinations. Recoveries from aged residue samples spiked at a level of 100 microg/kg (n=7) ranged, depending of the analyte/soil type combination, from 41-113% with RSDs ranging from 1-35%. In the SRM approach the developed LC-LC procedure was applied for the determination of linuron in 28 sandy soil samples collected in a field study. Linuron could be determined in soil with a limit of quantitation of 10 microg/kg.

Comparing generalized ensemble methods for sampling of systems with many degrees of freedom

DOE PAGES

Lincoff, James; Sasmal, Sukanya; Head-Gordon, Teresa

2016-11-03

Here, we compare two standard replica exchange methods using temperature and dielectric constant as the scaling variables for independent replicas against two new corresponding enhanced sampling methods based on non-equilibrium statistical cooling (temperature) or descreening (dielectric). We test the four methods on a rough 1D potential as well as for alanine dipeptide in water, for which their relatively small phase space allows for the ability to define quantitative convergence metrics. We show that both dielectric methods are inferior to the temperature enhanced sampling methods, and in turn show that temperature cool walking (TCW) systematically outperforms the standard temperature replica exchangemore » (TREx) method. We extend our comparisons of the TCW and TREx methods to the 5 residue met-enkephalin peptide, in which we evaluate the Kullback-Leibler divergence metric to show that the rate of convergence between two independent trajectories is faster for TCW compared to TREx. Finally we apply the temperature methods to the 42 residue amyloid-β peptide in which we find non-negligible differences in the disordered ensemble using TCW compared to the standard TREx. All four methods have been made available as software through the OpenMM Omnia software consortium.« less

Multi-residue screening of prioritised human pharmaceuticals, illicit drugs and bactericides in sediments and sludge.

PubMed

Langford, Katherine H; Reid, Malcolm; Thomas, Kevin V

2011-08-01

A robust multi-residue method was developed for the analysis of a selection of pharmaceutical compounds, illicit drugs and personal care product bactericides in sediments and sludges. Human pharmaceuticals were selected for analysis in Scottish sewage sludge and freshwater sediments based on prescription, physico-chemical and occurrence data. The method was suitable for the analysis of the selected illicit drugs amphetamine, benzoylecgonine, cocaine, and methamphetamine, the pharmaceuticals atenolol, bendroflumethiazide, carbamazepine, citalopram, diclofenac, fluoxetine, ibuprofen, and salbutamol, and the bactericides triclosan and triclocarban in sewage sludge and freshwater sediment. The method provided an overall recovery of between 56 and 128%, RSDs of between 2 and 19% and LODs of between 1 and 50 ng g(-1). Using the methodology the human pharmaceuticals atenolol, carbamazepine and citalopram and the bactericides triclosan and triclocarban were detected in Scottish sewage sludge. The illicit drugs cocaine, its metabolite benzoylecgonine, amphetamine and methamphetamine were not detected in any of the samples analysed. Triclosan and triclocarban were present at the highest concentrations with triclocarban detected in all but one sample and showing a pattern of co-occurrence in both sludge and sediment samples.

Determination of Chlortetracycline Residues, Antimicrobial Activity and Presence of Resistance Genes in Droppings of Experimentally Treated Broiler Chickens.

PubMed

Cornejo, Javiera; Yevenes, Karina; Avello, Constanza; Pokrant, Ekaterina; Maddaleno, Aldo; Martin, Betty San; Lapierre, Lisette

2018-05-25

Tetracyclines are important antimicrobial drugs for poultry farming that are actively excreted via feces and urine. Droppings are one of the main components in broiler bedding, which is commonly used as an organic fertilizer. Therefore, bedding becomes an unintended carrier of antimicrobial residues into the environment and may pose a highly significant threat to public health. For this depletion study, 60 broiler chickens were treated with 20% chlortetracycline (CTC) under therapeutic conditions. Concentrations of CTC and 4-epi-CTC were then determined in their droppings. Additionally, this work also aimed to detect the antimicrobial activity of these droppings and the phenotypic susceptibility to tetracycline in E. coli isolates, as well as the presence of tet(A) , tet(B) , and tet(G) resistance genes. CTC and 4-epi-CTC concentrations that were found ranged from 179.5 to 665.8 µg/kg. Based on these data, the depletion time for chicken droppings was calculated and set at 69 days. All samples presented antimicrobial activity, and a resistance to tetracyclines was found in bacterial strains that were isolated from these samples. Resistance genes tet(A) and tet(B) were also found in these samples.

On-line approaches for the determination of residues and contaminants in complex samples.

PubMed

Fumes, Bruno Henrique; Andrade, Mariane Aissa; Franco, Maraíssa Silva; Lanças, Fernando Mauro

2017-01-01

The determination of residues and contaminants in complex matrices such as in the case of food, environmental, and biological samples requires a combination of several steps to succeed in the aimed goal. At least three independent steps are integrated to provide the best available situation to deal with such matrices: (1) a sample preparation technique is employed to isolate the target compounds from the rest of the matrix; (2) a chromatographic (second) step further "purifies" the isolated compounds from the co-extracted matrix interferences; (3) a spectroscopy-based device acts as chromatographic detector (ideally containing a tandem high-resolution mass analyzer) for the qualitative and quantitative analysis. These techniques can be operated in different modes including the off-line and the on-line modes. The present report focus the on-line coupling techniques aiming the determination of analytes present in complex matrices. The fundamentals of these approaches as well as the most common set ups are presented and discussed, as well as a review on the recent applications of these two approaches to the fields of bioanalytical, environmental, and food analysis are critically discussed. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparing generalized ensemble methods for sampling of systems with many degrees of freedom.

PubMed

Lincoff, James; Sasmal, Sukanya; Head-Gordon, Teresa

2016-11-07

We compare two standard replica exchange methods using temperature and dielectric constant as the scaling variables for independent replicas against two new corresponding enhanced sampling methods based on non-equilibrium statistical cooling (temperature) or descreening (dielectric). We test the four methods on a rough 1D potential as well as for alanine dipeptide in water, for which their relatively small phase space allows for the ability to define quantitative convergence metrics. We show that both dielectric methods are inferior to the temperature enhanced sampling methods, and in turn show that temperature cool walking (TCW) systematically outperforms the standard temperature replica exchange (TREx) method. We extend our comparisons of the TCW and TREx methods to the 5 residue met-enkephalin peptide, in which we evaluate the Kullback-Leibler divergence metric to show that the rate of convergence between two independent trajectories is faster for TCW compared to TREx. Finally we apply the temperature methods to the 42 residue amyloid-β peptide in which we find non-negligible differences in the disordered ensemble using TCW compared to the standard TREx. All four methods have been made available as software through the OpenMM Omnia software consortium (http://www.omnia.md/).

Development of a quantum dot-based immunochromatography test strip for rapid screening of oxytetracycline and 4-epi-oxytetracycline in edible animal tissues.

PubMed

Xie, Yong; Zhang, Lei; Yang, Xian; Le, Tao

2017-03-01

A rapid and sensitive immunochromatographic test strip (ICTS) was developed in a competitive format with the quantum dot-conjugated monoclonal antibody specifically to determine the residues of oxytetracycline (OTC) and its metabolite 4-epi-oxytetracycline (4-epi-OTC). Using an ICTS reader, the 50% inhibition concentration (IC 50 ) was found to be 3.41 ± 0.29 ng ml - 1 of OTC in phosphate-buffered saline samples and the detection limit was 0.44 ± 0.05 ng ml - 1 . The visual cut-off level of the ICTS is 25 ng ml - 1 . The recoveries from tissue samples spiked with OTC of 50-600 μg kg - 1 were 74.2-107.2%, with coefficients of variation below 15%. The method was used to analyse incurred tissue samples, and there was good correlation (R 2  = 0.999) between the ICTS and high-performance liquid chromatography. These results indicate that ICTS is suitable for the rapid and quantitative detection of OTC and 4-epi-OTC residues in edible animal tissues.

Matrix Effect Evaluation and Method Validation of Azoxystrobin and Difenoconazole Residues in Red Flesh Dragon Fruit (Hylocereus polyrhizus) Matrices Using QuEChERS Sample Preparation Methods Followed by LC-MS/MS Determination.

PubMed

Noegrohati, Sri; Hernadi, Elan; Asviastuti, Syanti

2018-06-01

Production of red flesh dragon fruit (Hylocereus polyrhizus) was hampered by Colletotrichum sp. Pre-harvest application of azoxystrobin and difenoconazole mixture is recommended, therefore, a selective and sensitive multi residues analytical method is required in monitoring and evaluating the commodity's safety. LC-MS/MS is a well-established analytical technique for qualitative and quantitative determination in complex matrices. However, this method is hurdled by co-eluted coextractives interferences. This work evaluated the pH effect of acetate buffered and citrate buffered QuEChERS sample preparation in their effectiveness of matrix effect reduction. Citrate buffered QuEChERS proved to produce clean final extract with relative matrix effect 0.4%-0.7%. Method validation of the selected sample preparation followed by LC-MS/MS for whole dragon fruit, flesh and peel matrices fortified at 0.005, 0.01, 0.1 and 1 g/g showed recoveries 75%-119%, intermediate repeatability 2%-14%. The expanded uncertainties were 7%-48%. Based on the international acceptance criteria, this method is valid.

Milk and plasma disposition of thymol following intramammary administration of a phytoceutical mastitis treatment.

PubMed

McPhee, C S; Anderson, K L; Yeatts, J L; Mason, S E; Barlow, B M; Baynes, R E

2011-04-01

Despite the recent growth of the organic dairy industry, organic producers and veterinarians have limited information when choosing mastitis treatments for animals in organic dairy production. Organic producers commonly administer homeopathic or other plant-based products without having research evaluating the efficacy of these products and using estimated or no withholding times to treat mastitis and other health problems in their herds. In this pilot study, we attempted to identify several active ingredients of Phyto-Mast (Penn Dutch Cow Care, Narvon, PA), a plant-based mastitis treatment used on organic dairy farms, and to quantify the product residue in milk and plasma after intramammary administration. We developed an assay to quantify thymol (one of the active ingredients in Phyto-Mast) in milk and plasma using gas chromatography and mass spectrometry (GC-MS). Thymol is a volatile aromatic compound with antiinflammatory properties. As a model for dairy cows, 5 healthy, lactating alpine dairy goats were given 5 mL of Phyto-Mast per udder half. For 10 d following treatment, we analyzed blood and milk samples for thymol residues using GC-MS. The GC-MS assay was very sensitive for thymol detection, to a concentration of 0.01 μg/mL in plasma. Using thymol as a marker, Phyto-Mast was detectable and quantifiable in plasma beginning with the 15-min posttreatment sample, but was no longer detectable in the 4-h posttreatment sample. Thymol residues were only detected in the 12-h posttreatment milk sample. An inflammatory response was not evident in the udder following phytoceutical administration. Although this study provides information about the elimination of thymol, the product contains several other active chemicals, which may have different pharmacokinetic behaviors. Further analysis and additional study animals will help to determine a milk withholding time for Phyto-Mast. Given the recent growth of the organic dairy industry, understanding the pharmacokinetics of therapeutics used in organic production and developing accurate withholding recommendations will help to ensure milk safety. Copyright © 2011 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Molecular identification of polymers and anthropogenic particles extracted from oceanic water and fish stomach - A Raman micro-spectroscopy study.

PubMed

Ghosal, Sutapa; Chen, Michael; Wagner, Jeff; Wang, Zhong-Min; Wall, Stephen

2018-02-01

Pacific Ocean trawl samples, stomach contents of laboratory-raised fish as well as fish from the subtropical gyres were analyzed by Raman micro-spectroscopy (RMS) to identify polymer residues and any detectable persistent organic pollutants (POP). The goal was to access specific molecular information at the individual particle level in order to identify polymer debris in the natural environment. The identification process was aided by a laboratory generated automated fluorescence removal algorithm. Pacific Ocean trawl samples of plastic debris associated with fish collection sites were analyzed to determine the types of polymers commonly present. Subsequently, stomach contents of fish from these locations were analyzed for ingested polymer debris. Extraction of polymer debris from fish stomach using KOH versus ultrapure water were evaluated to determine the optimal method of extraction. Pulsed ultrasonic extraction in ultrapure water was determined to be the method of choice for extraction with minimal chemical intrusion. The Pacific Ocean trawl samples yielded primarily polyethylene (PE) and polypropylene (PP) particles >1 mm, PE being the most prevalent type. Additional microplastic residues (1 mm - 10 μm) extracted by filtration, included a polystyrene (PS) particle in addition to PE and PP. Flame retardant, deca-BDE was tentatively identified on some of the PP trawl particles. Polymer residues were also extracted from the stomachs of Atlantic and Pacific Ocean fish. Two types of polymer related debris were identified in the Atlantic Ocean fish: (1) polymer fragments and (2) fragments with combined polymer and fatty acid signatures. In terms of polymer fragments, only PE and PP were detected in the fish stomachs from both locations. A variety of particles were extracted from oceanic fish as potential plastic pieces based on optical examination. However, subsequent RMS examination identified them as various non-plastic fragments, highlighting the importance of chemical analysis in distinguishing between polymer and non-polymer residues. Copyright © 2017 Elsevier Ltd. All rights reserved.

Effect of temperature (cooking and freezing) on the concentration of oxytetracycline residue in experimentally induced birds

PubMed Central

Vivienne, Ezenduka Ekene; Josephine, Okorie-kanu Onyinye; Anaelom, Nwanta John

2018-01-01

Aim: The objective of this study was to determine the effect of varying temperatures (different cooking methods and freezing) on the concentration of oxytetracycline (OTC) residues in tissues of broiler birds. Materials and Methods: Fifty, 5-week-old birds were purchased and acclimatized for 3 weeks while being fed antibiotic-free feed and water. Four birds were then tested for residue and in the absence; the remaining birds were injected intramuscularly with oxytetracycline at its therapeutic dose. Muscle and liver samples of the treated birds were harvested and checked for OTC residues before subjecting them to boiling, microwaving, and roasting. The three plate test was used for the residue detection. Result: OTC was detected at both pH 6.0 and pH 7.2 but not detected at pH 8.0. Roasting and boiling significantly reduced the concentration of oxytetracycline in muscle by 53.6% and 69.6%, respectively, at pH 6.0, microwaving reduced the concentration by 49.1% but was not statistically significant. The same pattern was followed at pH 7.2 with reduction of 34.3%, 53.2%, and 67.7% for microwaved, roasted, and boiled. For the liver tissues, there was a significant reduction in the concentration for both pH: 6.0 (57.75%, 79.75%, and 89%; pH 7.2 (48.06%, 79.6%, and 88.79%) for boiled, microwaved, and roasted samples. Boiling had a greater reduction effect for muscle samples while roasting had a greater reduction in liver samples at both pHs. Freezing at −10°C had no effect on the concentration of OTC even after 9 days. Conclusion: The significant reduction of OTC concentration by cooking indicates that consumers may not be at risk of the effects of OTC residues in meat, but microwaving meat may not reduce the concentration below the maximum residue limit if the initial concentration is very high. Therefore, routine monitoring of drug residues in farms and abattoirs is still advocated. PMID:29657398

Influence of variable selection on partial least squares discriminant analysis models for explosive residue classification

NASA Astrophysics Data System (ADS)

De Lucia, Frank C., Jr.; Gottfried, Jennifer L.

2011-02-01

Using a series of thirteen organic materials that includes novel high-nitrogen energetic materials, conventional organic military explosives, and benign organic materials, we have demonstrated the importance of variable selection for maximizing residue discrimination with partial least squares discriminant analysis (PLS-DA). We built several PLS-DA models using different variable sets based on laser induced breakdown spectroscopy (LIBS) spectra of the organic residues on an aluminum substrate under an argon atmosphere. The model classification results for each sample are presented and the influence of the variables on these results is discussed. We found that using the whole spectra as the data input for the PLS-DA model gave the best results. However, variables due to the surrounding atmosphere and the substrate contribute to discrimination when the whole spectra are used, indicating this may not be the most robust model. Further iterative testing with additional validation data sets is necessary to determine the most robust model.

Development, validation and determination of multiclass pesticide residues in cocoa beans using gas chromatography and liquid chromatography tandem mass spectrometry.

PubMed

Zainudin, Badrul Hisyam; Salleh, Salsazali; Mohamed, Rahmat; Yap, Ken Choy; Muhamad, Halimah

2015-04-01

An efficient and rapid method for the analysis of pesticide residues in cocoa beans using gas and liquid chromatography-tandem mass spectrometry was developed, validated and applied to imported and domestic cocoa beans samples collected over 2 years from smallholders and Malaysian ports. The method was based on solvent extraction method and covers 26 pesticides (insecticides, fungicides, and herbicides) of different chemical classes. The recoveries for all pesticides at 10 and 50 μg/kg were in the range of 70-120% with relative standard deviations of less than 20%. Good selectivity and sensitivity were obtained with method limit of quantification of 10 μg/kg. The expanded uncertainty measurements were in the range of 4-25%. Finally, the proposed method was successfully applied for the routine analysis of pesticide residues in cocoa beans via a monitoring study where 10% of them was found positive for chlorpyrifos, ametryn and metalaxyl. Copyright © 2014 Elsevier Ltd. All rights reserved.

A novel method for the identification of inorganic and organic gunshot residue particles of lead-free ammunitions from the hands of shooters using scanning laser ablation-ICPMS and Raman micro-spectroscopy.

PubMed

Abrego, Zuriñe; Grijalba, Nagore; Unceta, Nora; Maguregui, Maite; Sanchez, Alicia; Fernández-Isla, Alberto; Goicolea, M Aranzazu; Barrio, Ramón J

2014-12-07

A method based on scanning laser ablation and inductively coupled plasma-mass spectrometry (SLA-ICPMS) and Raman micro-spectroscopy for the detection and identification of compounds consistent with gunshot residue particles (GSR) has been developed. The method has been applied to the characterization of particles resulting from the discharge of firearms using lead-free ammunition. Modified tape lifts were used to collect the inorganic and organic residues from skin surfaces in a single sample. Using SLA-ICPMS, aggregates related to the composition of the ammunition, such as Cu-Zn-Sn, Zr-Sr, Cu-Zn, Al-Ti, or Al-Sr-Zr were detected, but this composition is only consistent with GSR from lead-free ammunitions. Additional evidence was provided by micro-Raman spectroscopy, which identified the characteristic organic groups of the particles as centralite, diphenylamine or their nitrated derivatives, which are indicative of GSR.