Detection of β-Lactams and Chloramphenicol Residues in Raw Milk-Development and Application of an HPLC-DAD Method in Comparison with Microbial Inhibition Assays.

PubMed

Karageorgou, Eftychia; Christoforidou, Sofia; Ioannidou, Maria; Psomas, Evdoxios; Samouris, Georgios

2018-06-01

The present study was carried out to assess the detection sensitivity of four microbial inhibition assays (MIAs) in comparison with the results obtained by the High Performance Liquid Chromatography with Diode-Array Detection (HPLC-DAD) method for antibiotics of the β-lactam group and chloramphenicol in fortified raw milk samples. MIAs presented fairly good results when detecting β-lactams, whereas none were able to detect chloramphenicol at or above the permissible limits. HPLC analysis revealed high recoveries of examined compounds, whereas all detection limits observed were lower than their respective maximum residue limits (MRL) values. The extraction and clean-up procedure of antibiotics was performed by a modified matrix solid phase dispersion procedure using a mixture of Plexa by Agilent and QuEChERS as a sorbent. The HPLC method developed was validated, determining the accuracy, precision, linearity, decision limit, and detection capability. Both methods were used to monitor raw milk samples of several cows and sheep, obtained from producers in different regions of Greece, for the presence of examined antibiotic residues. Results obtained showed that MIAs could be used effectively and routinely to detect antibiotic residues in several milk types. However, in some cases, spoilage of milk samples revealed that the kits' sensitivity could be strongly affected, whereas this fact does not affect the effectiveness of HPLC-DAD analysis.

Ultrasensitive Detection of Shigella Species in Blood and Stool.

PubMed

Luo, Jieling; Wang, Jiapeng; Mathew, Anup S; Yau, Siu-Tung

2016-02-16

A modified immunosensing system with voltage-controlled signal amplification was used to detect Shigella in stool and blood matrixes at the single-digit CFU level. Inactivated Shigella was spiked in these matrixes and detected directly. The detection was completed in 78 min. Detection limits of 21 CFU/mL and 18 CFU/mL were achieved in stool and blood, respectively, corresponding to 2-7 CFUs immobilized on the detecting electrode. The outcome of the detection of extremely low bacterium concentration, i.e., below 100 CFU/mL, blood samples show a random nature. An analysis of the detection probabilities indicates the correlation between the sample volume and the success of detection and suggests that sample volume is critical for ultrasensitive detection of bacteria. The calculated detection limit is qualitatively in agreement with the empirically determined detection limit. The demonstrated ultrasensitive detection of Shigella on the single-digit CFU level suggests the feasibility of the direct detection of the bacterium in the samples without performing a culture.

DARKDROID: Exposing the Dark Side of Android Marketplaces

DTIC Science & Technology

2016-06-01

Moreover, our approaches can detect apps containing both intentional and unintentional vulnerabilities, such as unsafe code loading mechanisms and...Security, Static Analysis, Dynamic Analysis, Malware Detection , Vulnerability Scanning 16. SECURITY CLASSIFICATION OF: 17. LIMITATION OF ABSTRACT UU 18...applications in a DoD context. ................... 1 1.2.2 Develop sophisticated whole-system static analyses to detect malicious Android applications

A Review of Flow Analysis Methods for Determination of Radionuclides in Nuclear Wastes and Nuclear Reactor Coolants

DOE PAGES

Trojanowicz, Marek; Kolacinska, Kamila; Grate, Jay W.

2018-02-13

Here, the safety and security of nuclear power plant operations depend on the application of the most appropriate techniques and methods of chemical analysis, where modern flow analysis methods prevail. Nevertheless, the current status of the development of these methods is more limited than it might be expected based on their genuine advantages. The main aim of this paper is to review the automated flow analysis procedures developed with various detection methods for the nuclear energy industry. The flow analysis methods for the determination of radionuclides, that have been reported to date, are primarily focused on their environmental applications. Themore » benefits of the application of flow methods in both monitoring of the nuclear wastes and process analysis of the primary circuit coolants of light water nuclear reactors will also be discussed. The application of either continuous flow methods (CFA) or injection methods (FIA, SIA) of the flow analysis with the β–radiometric detection shortens the analysis time and improves the precision of determination due to mechanization of certain time-consuming operations of the sample processing. Compared to the radiometric detection, the mass spectrometry (MS) detection enables one to perform multicomponent analyses as well as the determination of transuranic isotopes with much better limits of detection.« less

A Review of Flow Analysis Methods for Determination of Radionuclides in Nuclear Wastes and Nuclear Reactor Coolants

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

Trojanowicz, Marek; Kolacinska, Kamila; Grate, Jay W.

Here, the safety and security of nuclear power plant operations depend on the application of the most appropriate techniques and methods of chemical analysis, where modern flow analysis methods prevail. Nevertheless, the current status of the development of these methods is more limited than it might be expected based on their genuine advantages. The main aim of this paper is to review the automated flow analysis procedures developed with various detection methods for the nuclear energy industry. The flow analysis methods for the determination of radionuclides, that have been reported to date, are primarily focused on their environmental applications. Themore » benefits of the application of flow methods in both monitoring of the nuclear wastes and process analysis of the primary circuit coolants of light water nuclear reactors will also be discussed. The application of either continuous flow methods (CFA) or injection methods (FIA, SIA) of the flow analysis with the β–radiometric detection shortens the analysis time and improves the precision of determination due to mechanization of certain time-consuming operations of the sample processing. Compared to the radiometric detection, the mass spectrometry (MS) detection enables one to perform multicomponent analyses as well as the determination of transuranic isotopes with much better limits of detection.« less

A review of flow analysis methods for determination of radionuclides in nuclear wastes and nuclear reactor coolants.

PubMed

Trojanowicz, Marek; Kołacińska, Kamila; Grate, Jay W

2018-06-01

The safety and security of nuclear power plant operations depend on the application of the most appropriate techniques and methods of chemical analysis, where modern flow analysis methods prevail. Nevertheless, the current status of the development of these methods is more limited than it might be expected based on their genuine advantages. The main aim of this paper is to review the automated flow analysis procedures developed with various detection methods for the nuclear energy industry. The flow analysis methods for the determination of radionuclides, that have been reported to date, are primarily focused on their environmental applications. The benefits of the application of flow methods in both monitoring of the nuclear wastes and process analysis of the primary circuit coolants of light water nuclear reactors will also be discussed. The application of either continuous flow methods (CFA) or injection methods (FIA, SIA) of the flow analysis with the β-radiometric detection shortens the analysis time and improves the precision of determination due to mechanization of certain time-consuming operations of the sample processing. Compared to the radiometric detection, the mass spectrometry (MS) detection enables one to perform multicomponent analyses as well as the determination of transuranic isotopes with much better limits of detection. Copyright © 2018 Elsevier B.V. All rights reserved.

Detection of contamination on selected apple cultivars using reflectance hyperspectral and multispectral analysis

NASA Astrophysics Data System (ADS)

Mehl, Patrick M.; Chao, Kevin; Kim, Moon S.; Chen, Yud-Ren

2001-03-01

Presence of natural or exogenous contaminations on apple cultivars is a food safety and quality concern touching the general public and strongly affecting this commodity market. Accumulations of human pathogens are usually observed on surface lesions of commodities. Detections of either lesions or directly of the pathogens are essential for assuring the quality and safety of commodities. We are presenting the application of hyperspectral image analysis towards the development of multispectral techniques for the detection of defects on chosen apple cultivars, such as Golden Delicious, Red Delicious, and Gala apples. Separate apple cultivars possess different spectral characteristics leading to different approaches for analysis. General preprocessing analysis with morphological treatments is followed by different image treatments and condition analysis for highlighting lesions and contaminations on the apple cultivars. Good isolations of scabs, fungal and soil contaminations and bruises are observed with hyperspectral imaging processing either using principal component analysis or utilizing the chlorophyll absorption peak. Applications of hyperspectral results to a multispectral detection are limited by the spectral capabilities of our RGB camera using either specific band pass filters and using direct neutral filters. Good separations of defects are obtained for Golden Delicious apples. It is however limited for the other cultivars. Having an extra near infrared channel will increase the detection level utilizing the chlorophyll absorption band for detection as demonstrated by the present hyperspectral imaging analysis

Radiometric Short-Term Fourier Transform analysis of photonic Doppler velocimetry recordings and detectivity limit

NASA Astrophysics Data System (ADS)

Prudhomme, G.; Berthe, L.; Bénier, J.; Bozier, O.; Mercier, P.

2017-01-01

Photonic Doppler Velocimetry is a plug-and-play and versatile diagnostic used in dynamic physic experiments to measure velocities. When signals are analyzed using a Short-Time Fourier Transform, multiple velocities can be distinguished: for example, the velocities of moving particle-cloud appear on spectrograms. In order to estimate the back-scattering fluxes of target, we propose an original approach "PDV Radiometric analysis" resulting in an expression of time-velocity spectrograms coded in power units. Experiments involving micron-sized particles raise the issue of detection limit; particle-size limit is very difficult to evaluate. From the quantification of noise sources, we derive an estimation of the spectrogram noise leading to a detectivity limit, which may be compared to the fraction of the incoming power which has been back-scattered by the particle and then collected by the probe. This fraction increases with their size. At last, some results from laser-shock accelerated particles using two different PDV systems are compared: it shows the improvement of detectivity with respect to the Effective Number of Bits (ENOB) of the digitizer.

Rapid and sensitive detection of synthetic cannabinoids AMB-FUBINACA and α-PVP using surface enhanced Raman scattering (SERS)

NASA Astrophysics Data System (ADS)

Islam, Syed K.; Cheng, Yin Pak; Birke, Ronald L.; Green, Omar; Kubic, Thomas; Lombardi, John R.

2018-04-01

The application of surface enhanced Raman scattering (SERS) has been reported as a fast and sensitive analytical method in the trace detection of the two most commonly known synthetic cannabinoids AMB-FUBINACA and alpha-pyrrolidinovalerophenone (α-PVP). FUBINACA and α-PVP are two of the most dangerous synthetic cannabinoids which have been reported to cause numerous deaths in the United States. While instruments such as GC-MS, LC-MS have been traditionally recognized as analytical tools for the detection of these synthetic drugs, SERS has been recently gaining ground in the analysis of these synthetic drugs due to its sensitivity in trace analysis and its effectiveness as a rapid method of detection. This present study shows the limit of detection of a concentration as low as picomolar for AMB-FUBINACA while for α-PVP, the limit of detection is in nanomolar concentration using SERS.

Non-volatile analysis in fruits by laser resonant ionization spectrometry: application to resveratrol (3,5,4'-trihydroxystilbene) in grapes

NASA Astrophysics Data System (ADS)

Montero, C.; Orea, J. M.; Soledad Muñoz, M.; Lobo, R. F. M.; González Ureña, A.

A laser desorption (LD) coupled with resonance-enhanced multiphoton ionisation (REMPI) and time-of-flight mass spectrometry (TOFMS) technique for non-volatile trace analysis compounds is presented. Essential features are: (a) an enhanced desorption yield due to the mixing of metal powder with the analyte in the sample preparation, (b) a high resolution, great sensitivity and low detection limit due to laser resonant ionisation and mass spectrometry detection. Application to resveratrol content in grapes demonstrated the capability of the analytical method with a sensitivity of 0.2 pg per single laser shot and a detection limit of 5 ppb.

Fast and sensitive trace analysis of malachite green using a surface-enhanced Raman microfluidic sensor.

PubMed

Lee, Sangyeop; Choi, Junghyun; Chen, Lingxin; Park, Byungchoon; Kyong, Jin Burm; Seong, Gi Hun; Choo, Jaebum; Lee, Yeonjung; Shin, Kyung-Hoon; Lee, Eun Kyu; Joo, Sang-Woo; Lee, Kyeong-Hee

2007-05-08

A rapid and highly sensitive trace analysis technique for determining malachite green (MG) in a polydimethylsiloxane (PDMS) microfluidic sensor was investigated using surface-enhanced Raman spectroscopy (SERS). A zigzag-shaped PDMS microfluidic channel was fabricated for efficient mixing between MG analytes and aggregated silver colloids. Under the optimal condition of flow velocity, MG molecules were effectively adsorbed onto silver nanoparticles while flowing along the upper and lower zigzag-shaped PDMS channel. A quantitative analysis of MG was performed based on the measured peak height at 1615 cm(-1) in its SERS spectrum. The limit of detection, using the SERS microfluidic sensor, was found to be below the 1-2 ppb level and this low detection limit is comparable to the result of the LC-Mass detection method. In the present study, we introduce a new conceptual detection technology, using a SERS microfluidic sensor, for the highly sensitive trace analysis of MG in water.

Quantitative subpixel spectral detection of targets in multispectral images. [terrestrial and planetary surfaces

NASA Technical Reports Server (NTRS)

Sabol, Donald E., Jr.; Adams, John B.; Smith, Milton O.

1992-01-01

The conditions that affect the spectral detection of target materials at the subpixel scale are examined. Two levels of spectral mixture analysis for determining threshold detection limits of target materials in a spectral mixture are presented, the cases where the target is detected as: (1) a component of a spectral mixture (continuum threshold analysis) and (2) residuals (residual threshold analysis). The results of these two analyses are compared under various measurement conditions. The examples illustrate the general approach that can be used for evaluating the spectral detectability of terrestrial and planetary targets at the subpixel scale.

Kernel-Phase Interferometry for Super-Resolution Detection of Faint Companions

NASA Astrophysics Data System (ADS)

Factor, Samuel

2016-10-01

Direct detection of close in companions (binary systems or exoplanets) is notoriously difficult. While chronagraphs and point spread function (PSF) subtraction can be used to reduce contrast and dig out signals of companions under the PSF, there are still significant limitations in separation and contrast. While non-redundant aperture masking (NRM) interferometry can be used to detect companions well inside the PSF of a diffraction limited image, the mask discards 95% of the light gathered by the telescope and thus the technique is severely flux limited. Kernel-phase analysis applies interferometric techniques similar to NRM though utilizing the full aperture. Instead of closure-phases, kernel-phases are constructed from a grid of points on the full aperture, simulating a redundant interferometer. I propose to develop my own faint companion detection pipeline which utilizes an MCMC analysis of kernel-phases. I will search for new companions in archival images from NIC1 and ACS/HRC in order to constrain binary and planet formation models at separations inaccessible to previous techniques. Using this method, it is possible to detect a companion well within the classical l/D Rayleigh diffraction limit using a fraction of the telescope time as NRM. This technique can easily be applied to archival data as no mask is needed and will thus make the detection of close in companions cheap and simple as no additional observations are needed. Since the James Webb Space Telescope (JWST) will be able to perform NRM observations, further development and characterization of kernel-phase analysis will allow efficient use of highly competitive JWST telescope time.

Fundamentals of Counting Statistics in Digital PCR: I Just Measured Two Target Copies-What Does It Mean?

PubMed

Tzonev, Svilen

2018-01-01

Current commercially available digital PCR (dPCR) systems and assays are capable of detecting individual target molecules with considerable reliability. As tests are developed and validated for use on clinical samples, the need to understand and develop robust statistical analysis routines increases. This chapter covers the fundamental processes and limitations of detecting and reporting on single molecule detection. We cover the basics of quantification of targets and sources of imprecision. We describe the basic test concepts: sensitivity, specificity, limit of blank, limit of detection, and limit of quantification in the context of dPCR. We provide basic guidelines how to determine those, how to choose and interpret the operating point, and what factors may influence overall test performance in practice.

[Quantitative spectrum analysis of characteristic gases of spontaneous combustion coal].

PubMed

Liang, Yun-Tao; Tang, Xiao-Jun; Luo, Hai-Zhu; Sun, Yong

2011-09-01

Aimed at the characteristics of spontaneous combustion gas such as a variety of gases, lou limit of detection, and critical requirement of safety, Fourier transform infrared (FTIR) spectral analysis is presented to analyze characteristic gases of spontaneous combustion In this paper, analysis method is introduced at first by combing characteristics of absorption spectra of analyte and analysis requirement. Parameter setting method, sample preparation, feature variable abstract and analysis model building are taken into consideration. The methods of sample preparation, feature abstraction and analysis model are introduced in detail. And then, eleven kinds of gases were tested with Tensor 27 spectrometer. CH4, C2H6, C3H8, iC4H10, nC4H10, C2 H4, C3 H6, C3 H2, SF6, CO and CO2 were included. The optical path length was 10 cm while the spectra resolution was set as 1 cm(-1). The testing results show that the detection limit of all analytes is less than 2 x 10(-6). All the detection limits fit the measurement requirement of spontaneous combustion gas, which means that FTIR may be an ideal instrument and the analysis method used in this paper is competent for spontaneous combustion gas measurement on line.

Fully integrated lab-on-a-disc for nucleic acid analysis of food-borne pathogens.

PubMed

Kim, Tae-Hyeong; Park, Juhee; Kim, Chi-Ju; Cho, Yoon-Kyoung

2014-04-15

This paper describes a micro total analysis system for molecular analysis of Salmonella, a major food-borne pathogen. We developed a centrifugal microfluidic device, which integrated the three main steps of pathogen detection, DNA extraction, isothermal recombinase polymerase amplification (RPA), and detection, onto a single disc. A single laser diode was utilized for wireless control of valve actuation, cell lysis, and noncontact heating in the isothermal amplification step, thereby yielding a compact and miniaturized system. To achieve high detection sensitivity, rare cells in large volumes of phosphate-buffered saline (PBS) and milk samples were enriched before loading onto the disc by using antibody-coated magnetic beads. The entire procedure, from DNA extraction through to detection, was completed within 30 min in a fully automated fashion. The final detection was carried out using lateral flow strips by direct visual observation; detection limit was 10 cfu/mL and 10(2) cfu/mL in PBS and milk, respectively. Our device allows rapid molecular diagnostic analysis and does not require specially trained personnel or expensive equipment. Thus, we expect that it would have an array of potential applications, including in the detection of food-borne pathogens, environmental monitoring, and molecular diagnostics in resource-limited settings.

Investigation of detection limits for diffuse optical tomography systems: II. Analysis of slab and cup geometry for breast imaging.

PubMed

Ziegler, Ronny; Brendel, Bernhard; Rinneberg, Herbert; Nielsen, Tim

2009-01-21

Using a statistical (chi-square) test on simulated data and a realistic noise model derived from the system's hardware we study the performance of diffuse optical tomography systems for fluorescence imaging. We compare the predicted smallest size of detectable lesions at various positions in slab and cup geometry and model how detection sensitivity depends on breast compression and lesion fluorescence contrast. Our investigation shows that lesion detection is limited by relative noise in slab geometry and by absolute noise in cup geometry.

Development of capillary electrophoresis methods for quantitative determination of taurine in vehicle system and biological media.

PubMed

da Silva, Dayse L P; Rüttinger, Hans H; Mrestani, Yahia; Baum, Walter F; Neubert, Reinhard H H

2006-06-01

CE methods have been developed for the determination of taurine in pharmaceutical formulation (microemulsion) and in biological media such as sweat. The CE system with end-column pulsed amperometric detection has been found to be an interesting method in comparison with UV and fluorescence detection for its simplicity and rapidity. A gold-disk electrode of 100 mm diameter was used as the working electrode. The effects of a field decoupler at the end of the capillary, separation voltage, injection and pressure times were investigated. A detection limit of 4 x 10(-5) mol/L was reached using integrated pulsed amperometric detection, a method successfully applied to taurine analysis of the biological samples such as sweat. For taurine analysis of oil-in-water microemulsion, fluorescence detector was the favored method, the detection limit of which was 4 x 10(-11) mol/L.

A Validation of Remotely Sensed Fires Using Ground Reports

NASA Astrophysics Data System (ADS)

Ruminski, M. G.; Hanna, J.

2007-12-01

A satellite based analysis of fire detections and smoke emissions for North America is produced daily by NOAA/NESDIS. The analysis incorporates data from the MODIS (Terra and Aqua) and AVHRR (NOAA-15/16/17) polar orbiting instruments and GOES East and West geostationary spacecraft with nominal resolutions of 1km and 4 km for the polar and geostationary platforms respectively. Automated fire detection algorithms are utilized for each of the sensors. Analysts perform a quality control procedure on the automated detects by deleting points that are deemed to be false detects and adding points that the algorithms did not detect. A limited validation of the final quality controlled product was performed using high resolution (30 m) ASTER data in the summer of 2006. Some limitations in using ASTER data are that each scene is only approximately 3600 square km, the data acquisition time is relatively constant at around 1030 local solar time and ASTER is another remotely sensed data source. This study expands on the ASTER validation by using ground reports of prescribed burns in Montana and Idaho for 2003 and 2004. It provides a non-remote sensing data source for comparison. While the ground data do not have the limitations noted above for ASTER there are still limitations. For example, even though the data set covers a much larger area (nearly 600,000 square km) than even several ASTER scenes, it still represents a single region of North America. And while the ground data are not restricted to a narrow time window, only a date is provided with each report, limiting the ability to make detailed conclusions about the detection capabilities for specific instruments, especially for the less temporally frequent polar orbiting MODIS and AVHRR sensors. Comparison of the ground data reports to the quality controlled fire analysis revealed a low rate of overall detection of 23.00% over the entire study period. Examination of the daily detection rates revealed a wide variation, with some days resulting in as little as 5 detects out of 107 reported fires while other days had as many as 84 detections out of 160 reports. Inspection of the satellite imagery from the days with very low detection rates revealed that extensive cloud cover prohibited satellite fire detection. On days when cloud cover was at a minimum, detection rates were substantially higher. An estimate of the fire size was also provided with the ground data set. Statistics will be presented for days with minimal cloud cover which will indicate the probability of detection for fires of various sizes.

Capillary zone electrophoresis for analysis of complex proteomes using an electrokinetically pumped sheath flow nanospray interface

PubMed Central

Sun, Liangliang; Zhu, Guijie; Yan, Xiaojing; Champion, Mathew M.

2014-01-01

The vast majority of proteomic studies employ reversed-phase high-performance liquid chromatography coupled with tandem mass spectrometry for analysis of the tryptic digest of a cellular lysate. This technology is quite mature, and typically provides identification of hundreds to thousands of peptides, which is used to infer the identity of hundreds to thousands of proteins. These approaches usually require milligrams to micrograms of starting material. Capillary zone electrophoresis provides an interesting alternative separation method based on a different separation mechanism than HPLC. Capillary electrophoresis received some attention for protein analysis beginning 25 years ago. Those efforts stalled because of the limited performance of the electrospray interfaces and the limited speed and sensitivity of mass spectrometers of that era. This review considers a new electrospray interface design coupled with Orbitrap Velos and linear Q-trap mass spectrometers. Capillary zone electrophoresis coupled with this interface and these detectors provides single shot detection of >1,250 peptides from an E. coli digest in less than one hour, identification of nearly 5,000 peptides from analysis of seven fractions produced by solid-phase extraction of the E. coli digest in a six hour total analysis time, low attomole detection limits for peptides generated from standard proteins, and high zeptomole detection limits for selected ion monitoring of peptides. Incorporation of an integrated on-line immobilized trypsin microreactor allows digestion and analysis of picogram amounts of a complex eukaryotic proteome. PMID:24277677

Analytical methods for the determination of urinary 2,4-dichlorophenoxyacetic acid and 2-methyl-4-chlorophenoxyacetic acid in occupationally exposed subjects and in the general population.

PubMed

Aprea, C; Sciarra, G; Bozzi, N

1997-01-01

Two methods for the quantitative analysis of 2,4-dichlorophenoxyacetic acid (2,4-D) and 2-methyl-4-chlorophenoxyacetic acid (MCPA) in urine were compared. The first was an high-performance liquid chromatography method using a C8 column with ion suppression and diode array detection. The urine extracts were first purified by solid-phase extraction (SPE) on silica capillary columns. The detection limit of the method was 15 micrograms/L for both compounds. The percentage coefficient of variation of the whole analysis evaluated at a concentration of 125.0 micrograms/L was 6.2% for 2,4-D and 6.8% for MCPA. The mean recovery of analysis was 81% for 2,4-D and 85% for MCPA. The second was a gas chromatographic (GC) method in which the compounds were first derivatized with pentafluorobenzylbromide to pentafluorobenzyl esters, which were determined with a slightly polar capillary column and electron capture detection. Before GC analysis, the urine extracts were purified by SPE on silica capillary columns. This method had a detection limit of 1 microgram/L for both compounds and a percentage coefficient of variation of the whole analysis, evaluated at a concentration of 30.0 micrograms/L, of 8% for 2,4-D, and of 5.5% for MCPA. the mean recovery was 87% for 2,4-D and 94% for MCPA. The low detection limit made the second method suitable for assaying the two herbicides in the general population. Duplicate analysis of ten urine samples from occupationally exposed subjects by the two methods gave identical results for a wide range of concentrations.

Enhancement of laser-induced breakdown spectroscopy (LIBS) Detection limit using a low-pressure and short-pulse laser-induced plasma process.

PubMed

Wang, Zhen Zhen; Deguchi, Yoshihiro; Kuwahara, Masakazu; Yan, Jun Jie; Liu, Ji Ping

2013-11-01

Laser-induced breakdown spectroscopy (LIBS) technology is an appealing technique compared with many other types of elemental analysis because of the fast response, high sensitivity, real-time, and noncontact features. One of the challenging targets of LIBS is the enhancement of the detection limit. In this study, the detection limit of gas-phase LIBS analysis has been improved by controlling the pressure and laser pulse width. In order to verify this method, low-pressure gas plasma was induced using nanosecond and picosecond lasers. The method was applied to the detection of Hg. The emission intensity ratio of the Hg atom to NO (IHg/INO) was analyzed to evaluate the LIBS detection limit because the NO emission (interference signal) was formed during the plasma generation and cooling process of N2 and O2 in the air. It was demonstrated that the enhancement of IHg/INO arose by decreasing the pressure to a few kilopascals, and the IHg/INO of the picosecond breakdown was always much higher than that of the nanosecond breakdown at low buffer gas pressure. Enhancement of IHg/INO increased more than 10 times at 700 Pa using picosecond laser with 35 ps pulse width. The detection limit was enhanced to 0.03 ppm (parts per million). We also saw that the spectra from the center and edge parts of plasma showed different features. Comparing the central spectra with the edge spectra, IHg/INO of the edge spectra was higher than that of the central spectra using the picosecond laser breakdown process.

Epidemiologic Evaluation of Measurement Data in the Presence of Detection Limits

PubMed Central

Lubin, Jay H.; Colt, Joanne S.; Camann, David; Davis, Scott; Cerhan, James R.; Severson, Richard K.; Bernstein, Leslie; Hartge, Patricia

2004-01-01

Quantitative measurements of environmental factors greatly improve the quality of epidemiologic studies but can pose challenges because of the presence of upper or lower detection limits or interfering compounds, which do not allow for precise measured values. We consider the regression of an environmental measurement (dependent variable) on several covariates (independent variables). Various strategies are commonly employed to impute values for interval-measured data, including assignment of one-half the detection limit to nondetected values or of “fill-in” values randomly selected from an appropriate distribution. On the basis of a limited simulation study, we found that the former approach can be biased unless the percentage of measurements below detection limits is small (5–10%). The fill-in approach generally produces unbiased parameter estimates but may produce biased variance estimates and thereby distort inference when 30% or more of the data are below detection limits. Truncated data methods (e.g., Tobit regression) and multiple imputation offer two unbiased approaches for analyzing measurement data with detection limits. If interest resides solely on regression parameters, then Tobit regression can be used. If individualized values for measurements below detection limits are needed for additional analysis, such as relative risk regression or graphical display, then multiple imputation produces unbiased estimates and nominal confidence intervals unless the proportion of missing data is extreme. We illustrate various approaches using measurements of pesticide residues in carpet dust in control subjects from a case–control study of non-Hodgkin lymphoma. PMID:15579415

Shifted termination assay (STA) fragment analysis to detect BRAF V600 mutations in papillary thyroid carcinomas

PubMed Central

2013-01-01

Background BRAF mutation is an important diagnostic and prognostic marker in patients with papillary thyroid carcinoma (PTC). To be applicable in clinical laboratories with limited equipment, diverse testing methods are required to detect BRAF mutation. Methods A shifted termination assay (STA) fragment analysis was used to detect common V600 BRAF mutations in 159 PTCs with DNAs extracted from formalin-fixed paraffin-embedded tumor tissue. The results of STA fragment analysis were compared to those of direct sequencing. Serial dilutions of BRAF mutant cell line (SNU-790) were used to calculate limit of detection (LOD). Results BRAF mutations were detected in 119 (74.8%) PTCs by STA fragment analysis. In direct sequencing, BRAF mutations were observed in 118 (74.2%) cases. The results of STA fragment analysis had high correlation with those of direct sequencing (p < 0.00001, κ = 0.98). The LOD of STA fragment analysis and direct sequencing was 6% and 12.5%, respectively. In PTCs with pT3/T4 stages, BRAF mutation was observed in 83.8% of cases. In pT1/T2 carcinomas, BRAF mutation was detected in 65.9% and this difference was statistically significant (p = 0.007). Moreover, BRAF mutation was more frequent in PTCs with extrathyroidal invasion than tumors without extrathyroidal invasion (84.7% versus 62.2%, p = 0.001). To prepare and run the reactions, direct sequencing required 450 minutes while STA fragment analysis needed 290 minutes. Conclusions STA fragment analysis is a simple and sensitive method to detect BRAF V600 mutations in formalin-fixed paraffin-embedded clinical samples. Virtual Slides The virtual slide(s) for this article can be found here: http://www.diagnosticpathology.diagnomx.eu/vs/5684057089135749 PMID:23883275

Improvements in an in vivo neutron activation analysis (NAA) method for the measurement of fluorine in human bone.

PubMed

Mostafaei, F; McNeill, F E; Chettle, D R; Prestwich, W V

2013-10-01

We previously published a method for the in vivo measurement of bone fluoride using neutron activation analysis (NAA) and demonstrated the utility of the technique in a pilot study of environmentally exposed people. The method involved activation of the hand in an irradiation cavity at the McMaster University Accelerator Laboratory and acquisition of the resultant γ-ray signals in a '4π' NaI(Tl) detector array of nine detectors. In this paper we describe a series of improvements to the method. This was investigated via measurement of hand simulating phantoms doped with varying levels of fluorine and fixed amounts of sodium, chlorine and calcium. Four improvements to the technique were tested since our first publication. The previously published detection limit for phantom measurements using this system was 0.66 mg F/g Ca. The accelerator irradiation and detection facilities were relocated to a new section of the laboratory and one more detector was added to the detection system. This was found to reduce the detection limit (possibly because of better detection shielding and additional detector) to 0.59 mg F/g Ca, a factor of 1.12. A new set of phantoms was developed and in this work we show that they improved the minimum detectable limit for fluoride in phantoms irradiated using neutrons produced by 2.15 MeV protons on lithium by a factor of 1.55. We compared the detection limits previously obtained using a summed signal from the nine detectors with the detection limit obtained by acquiring the spectra in anticoincidence mode for reduction of the disturbing signal from chlorine in bone. This was found to improve the ratio of the detection of fluorine to chlorine (an interfering signal) by a factor of 2.8 and the resultant minimum detection limit was found to be reduced by a factor of 1.2. We studied the effects of changing the timing of γ-ray acquisition. Our previously published data used a series of three 10 s acquisitions followed by a 300 s count. Changing the acquisition to a series of six 5 s acquisitions was found to further improve the detection limit by a factor of 1.4. We also present data showing that if the neutron dose is delivered to the phantom in a shorter time period, i.e. the dose rate is increased and irradiation shortened then the detection limit can be reduced by a further factor of 1.35.The overall improvement in detection limit by employing all of these changes was found to be a factor of 3.9. The technique now has an in phantom detection limit of 0.17 mg F/g Ca compared to a previous detection limit of 0.66 mg F/g Ca. The system can now be tested on human volunteers to see if individuals with diagnosed fluorosis can be distinguished from the general Canadian population using this technique.

Heisenberg limit for displacements with semiclassical states

NASA Astrophysics Data System (ADS)

Luis, Alfredo

2004-04-01

We analyze the quantum limit to the sensitivity of the detection of small displacements. We focus on the case of free particles and harmonic oscillators as the systems experiencing the displacement. We show that the minimum displacement detectable is proportional to the inverse of the square root of the mean value of the energy in the state experiencing the displacement (Heisenberg limit). We present a measuring scheme that reaches this limit using semiclassical states. We examine the performance of this strategy under realistic practical conditions by computing the effect of imperfections such as losses and nonunit detection efficiencies. This analysis confirms the robustness of this measuring strategy by showing that the experimental imperfections can be suitably compensated by increasing the mean energy of the input state.

Real-time detection of hazardous materials in air

NASA Astrophysics Data System (ADS)

Schechter, Israel; Schroeder, Hartmut; Kompa, Karl L.

1994-03-01

A new detection system has been developed for real-time analysis of organic compounds in ambient air. It is based on multiphoton ionization by an unfocused laser beam in a single parallel-plate device. Thus, the ionization volume can be relatively large. The amount of laser created ions is determined quantitatively from the induced total voltage drop between the biased plates (Q equals (Delta) V(DOT)C). Mass information is obtained from computer analysis of the time-dependent signal. When a KrF laser (5 ev) is used, most of the organic compounds can be ionized in a two-photon process, but none of the standard components of atmospheric air are ionized by this process. Therefore, this instrument may be developed as a `sniffer' for organic materials. The method has been applied for benzene analysis in air. The detection limit is about 10 ppb. With a simple preconcentration technique the detection limit can be decreased to the sub-ppb range. Simple binary mixtures are also resolved.

[Analysis of Arsenic Compounds in Blood and Urine by HPLC-ICP-MS].

PubMed

Lin, L; Zhang, S J; Xu, W C; Luo, R X; Ma, D; Shen, M

2018-02-01

To establish an analysis method for the detection of 6 arsenic compounds [AsC, AsB, As（Ⅲ）, DMA, MMA and As（V）] in blood and urine by high-performance liquid chromatography-inductively coupled plasma-mass spectrometry （HPLC-ICP-MS）, and apply it to real cases. Triton was used to damage cells, and then EDTA·2Na·2H2O was used to complex arsenic compounds in cells, and sonication and protein deposition by acetonitrile were performed for sample pretreatment. With the mobile phase consisted of ammonium carbonate and ultrapure water, gradient elution was performed for obtaining the arsenic compounds in samples, which were analysed by ICP-MS with Hamilton PRP-X100 column. The limits of detection in blood were 1.66-10 ng/mL, while the lower limits of quantitation in blood ranged from 5 to 30 ng/mL. The limits of detection in urine were 0.5-10 ng/mL, while the lower limits of quantitation in urine were 5-30 ng/mL. The relative standard deviation of inter-day and intra-day precisions was less than 10%. This method had been successfully applied to 3 cases. This study has established an analysis method for detecting 6 common arsenic compounds in blood and urine, which can be used to detect the arsenic compounds in the blood and urine from arsenic poisoning cases as well as the patients under arsenic treatment. Copyright© by the Editorial Department of Journal of Forensic Medicine.

Multiple-element semiquantitative analysis of one-milligram geochemical samples by D.C. arc emission spectrography

USGS Publications Warehouse

Rait, N.

1981-01-01

A modified method is described for a 1-mg sample multi-element semiquantitative spectrographic analysis. This method uses a direct-current arc source, carbon instead of graphite electrodes, and an 80% argon-20% oxygen atmosphere instead of air. Although this is a destructive method, an analysis can be made for 68 elements in all mineral and geochemical samples. Carbon electrodes have been an aid in improving the detection limits of many elements. The carbon has a greater resistance to heat conductance and develops a better tip, facilitating sample volatilization and counter balancing the cooling effect of a flow of the argon-oxygen mixture around the anode. Where such an argon-oxygen atmosphere is used instead of air, the cyanogen band lines are greatly diminished in intensity, and thus more spectral lines of analysis elements are available for use; the spectral background is also lower. The main advantage of using the carbon electrode and the 80% argon-20% oxygen atmosphere is the improved detection limits of 36 out of 68 elements. The detection limits remain the same for 23 elements, and are not as good for only nine elements. ?? 1981.

Comparative elemental analysis of fine particulate matter (PM2.5) from industrial and residential areas in Greater Cairo-Egypt by means of a multi-secondary target energy dispersive X-ray fluorescence spectrometer

NASA Astrophysics Data System (ADS)

Shaltout, Abdallah A.; Hassan, Salwa K.; Karydas, Andreas G.; Zaki, Z. I.; Mostafa, Nasser Y.; Kregsamer, Peter; Wobrauschek, Peter; Streli, Christina

2018-07-01

Fine aerosol particles with aerodynamic diameter equal or <2.5 μm (PM2.5) have been collected from industrial and residential areas of Greater Cairo, Egypt during two different seasons namely; autumn 2014 and winter 2014/2015. Energy dispersive X-ray fluorescence (EDXRF) analysis utilizing polarization geometry and three different secondary targets (CaF2, Ge, and Mo) was employed for the quantitative analysis of eighteen (18) elements in PM2.5 samples. Light elements like Na and Mg was possible to be quantified, whereas detection limits in the range of few ng m-3 were attained for the most of the detected elements. Although, the average mass concentrations of the PM2.5 collected from the residential area (27 ± 7 μg m-3) is close to the annual mean limit value, a significant number of the collected samples (33%) presented higher average mass concentrations. For the industrial location, the average mass concentration is equal to 55 ± 19 μg m-3, exceeded twofold the annual mean limit value of the European Commission. Remarkably high elemental concentrations were determined for the most of the detected elements from the industrial area samples, clearly indicating the significant influence of anthropogenic activities. The present optimized EDXRF analysis offered significantly improved analytical range and limits of detection with respect to previous similar studies, thus enhancing our knowledge and understanding on the contribution of different pollution sources.

Acetylcholinesterase Immobilized on Magnetic Beads for Pesticides Detection: Application to Olive Oil Analysis

PubMed Central

Ben Oujji, Najwa; Bakas, Idriss; Istamboulié, Georges; Ait-Ichou, Ihya; Ait-Addi, Elhabib; Rouillon, Régis; Noguer, Thierry

2012-01-01

This work presents the development of bioassays and biosensors for the detection of insecticides widely used in the treatment of olive trees. The systems are based on the covalent immobilisation of acetylcholinesterase on magnetic microbeads using either colorimetry or amperometry as detection technique. The magnetic beads were immobilised on screen-printed electrodes or microtitration plates and tested using standard solutions and real samples. The developed devices showed good analytical performances with limits of detection much lower than the maximum residue limit tolerated by international regulations, as well as a good reproducibility and stability. PMID:22969377

Detection Of Malware Collusion With Static Dependence Analysis On Inter-App Communication

DTIC Science & Technology

2016-12-08

DETECTION OF MALWARE COLLUSION WITH STATIC DEPENDENCE ANALYSIS ON INTER-APP COMMUNICATION VIRGINIA TECH DECEMBER 2016 FINAL TECHNICAL REPORT... DEPENDENCE ANALYSIS ON INTER-APP COMMUNICATION 5a. CONTRACT NUMBER FA8750-15-2-0076 5b. GRANT NUMBER N/A 5c. PROGRAM ELEMENT NUMBER 61101E 6. AUTHOR(S...exploited. 15. SUBJECT TERMS Malware Collusion; Inter-App Communication; Static Dependence Analysis 16. SECURITY CLASSIFICATION OF: 17. LIMITATION OF

Automatic rectum limit detection by anatomical markers correlation.

PubMed

Namías, R; D'Amato, J P; del Fresno, M; Vénere, M

2014-06-01

Several diseases take place at the end of the digestive system. Many of them can be diagnosed by means of different medical imaging modalities together with computer aided detection (CAD) systems. These CAD systems mainly focus on the complete segmentation of the digestive tube. However, the detection of limits between different sections could provide important information to these systems. In this paper we present an automatic method for detecting the rectum and sigmoid colon limit using a novel global curvature analysis over the centerline of the segmented digestive tube in different imaging modalities. The results are compared with the gold standard rectum upper limit through a validation scheme comprising two different anatomical markers: the third sacral vertebra and the average rectum length. Experimental results in both magnetic resonance imaging (MRI) and computed tomography colonography (CTC) acquisitions show the efficacy of the proposed strategy in automatic detection of rectum limits. The method is intended for application to the rectum segmentation in MRI for geometrical modeling and as contextual information source in virtual colonoscopies and CAD systems. Copyright © 2014 Elsevier Ltd. All rights reserved.

Toward Intelligent Software Defect Detection

NASA Technical Reports Server (NTRS)

Benson, Markland J.

2011-01-01

Source code level software defect detection has gone from state of the art to a software engineering best practice. Automated code analysis tools streamline many of the aspects of formal code inspections but have the drawback of being difficult to construct and either prone to false positives or severely limited in the set of defects that can be detected. Machine learning technology provides the promise of learning software defects by example, easing construction of detectors and broadening the range of defects that can be found. Pinpointing software defects with the same level of granularity as prominent source code analysis tools distinguishes this research from past efforts, which focused on analyzing software engineering metrics data with granularity limited to that of a particular function rather than a line of code.

Resonant photoacoustic cell for pulsed laser analysis of gases at high temperature

NASA Astrophysics Data System (ADS)

Sorvajärvi, Tapio; Manninen, Albert; Toivonen, Juha; Saarela, Jaakko; Hernberg, Rolf

2009-12-01

A new approach to high temperature gas analysis by means of photoacoustic (PA) spectroscopy is presented. The transverse modes of the resonant PA cell were excited with a pulsed laser and detected with a microphone. Changes in the properties of the PA cell resulting from a varying temperature are discussed and considered when processing the PA signal. The feasibility of the proposed method was demonstrated by studying PA response from saturated vapor of potassium chloride (KCl) in the temperature range extending from 410 to 691 °C. The PA spectrum, the detection limit, and the signal saturation of KCl vapor are discussed. At 245 nm excitation wavelength and 300 μJ pulse energy, the achieved detection limit for KCl is 15 ppb.

Progressive data transmission for anatomical landmark detection in a cloud.

PubMed

Sofka, M; Ralovich, K; Zhang, J; Zhou, S K; Comaniciu, D

2012-01-01

In the concept of cloud-computing-based systems, various authorized users have secure access to patient records from a number of care delivery organizations from any location. This creates a growing need for remote visualization, advanced image processing, state-of-the-art image analysis, and computer aided diagnosis. This paper proposes a system of algorithms for automatic detection of anatomical landmarks in 3D volumes in the cloud computing environment. The system addresses the inherent problem of limited bandwidth between a (thin) client, data center, and data analysis server. The problem of limited bandwidth is solved by a hierarchical sequential detection algorithm that obtains data by progressively transmitting only image regions required for processing. The client sends a request to detect a set of landmarks for region visualization or further analysis. The algorithm running on the data analysis server obtains a coarse level image from the data center and generates landmark location candidates. The candidates are then used to obtain image neighborhood regions at a finer resolution level for further detection. This way, the landmark locations are hierarchically and sequentially detected and refined. Only image regions surrounding landmark location candidates need to be trans- mitted during detection. Furthermore, the image regions are lossy compressed with JPEG 2000. Together, these properties amount to at least 30 times bandwidth reduction while achieving similar accuracy when compared to an algorithm using the original data. The hierarchical sequential algorithm with progressive data transmission considerably reduces bandwidth requirements in cloud-based detection systems.

Nanoporous Glass Integrated in Volumetric Bar-Chart Chip for Point-of-Care Diagnostics of Non-Small Cell Lung Cancer.

PubMed

Li, Ying; Xuan, Jie; Song, Yujun; Qi, Wenjin; He, Bangshun; Wang, Ping; Qin, Lidong

2016-01-26

Point-of-care (POC) testing has the potential to enable rapid, low-cost, and large-scale screening. POC detection of a multiplexed biomarker panel can facilitate the early diagnosis of non-small cell lung cancer (NSCLC) and, thus, may allow for more timely surgical intervention for life-saving treatment. Herein, we report the nanoporous glass (NPG) integrated volumetric bar-chart chip (V-Chip) for POC detection of the three NSCLC biomarkers CEA, CYFRA 21-1, and SCCA, by the naked eye. The 3D nanostructures in the NPG membrane efficiently increase the number of binding sites for antibodies and decrease the diffusion distance between antibody and antigen, enabling the low detection limit and rapid analysis time of the NPG-V-Chip. We utilized the NPG-V-Chip to test the NSCLC biomarker panel and found that the limit of detection can reach 50 pg/mL (10-fold improvement over the original V-Chip), and the total assay time can be decreased from 4 to 0.5 h. We then detected CEA in 21 serum samples from patients with common cancers, and the on-chip results showed good correlation with the clinical results. We further assayed 10 lung cancer samples using the device and confirmed the results obtained using conventional ELISA methods. In summary, the NPG-V-Chip platform has the ability of multiplex, low detection limit, low cost, lack of need for accessory equipment, and rapid analysis time, which may render the V-Chip a useful platform for quantitative POC detection in resource-limited settings and personalized diagnostics.

Integrated Multi-process Microfluidic Systems for Automating Analysis

PubMed Central

Yang, Weichun; Woolley, Adam T.

2010-01-01

Microfluidic technologies have been applied extensively in rapid sample analysis. Some current challenges for standard microfluidic systems are relatively high detection limits, and reduced resolving power and peak capacity compared to conventional approaches. The integration of multiple functions and components onto a single platform can overcome these separation and detection limitations of microfluidics. Multiplexed systems can greatly increase peak capacity in multidimensional separations and can increase sample throughput by analyzing many samples simultaneously. On-chip sample preparation, including labeling, preconcentration, cleanup and amplification, can all serve to speed up and automate processes in integrated microfluidic systems. This paper summarizes advances in integrated multi-process microfluidic systems for automated analysis, their benefits and areas for needed improvement. PMID:20514343

Detection of semi-volatile organic compounds in permeable ...

EPA Pesticide Factsheets

Abstract The Edison Environmental Center (EEC) has a research and demonstration permeable parking lot comprised of three different permeable systems: permeable asphalt, porous concrete and interlocking concrete permeable pavers. Water quality and quantity analysis has been ongoing since January, 2010. This paper describes a subset of the water quality analysis, analysis of semivolatile organic compounds (SVOCs) to determine if hydrocarbons were in water infiltrated through the permeable surfaces. SVOCs were analyzed in samples collected from 11 dates over a 3 year period, from 2/8/2010 to 4/1/2013.Results are broadly divided into three categories: 42 chemicals were never detected; 12 chemicals (11 chemical test) were detected at a rate of less than 10% or less; and 22 chemicals were detected at a frequency of 10% or greater (ranging from 10% to 66.5% detections). Fundamental and exploratory statistical analyses were performed on these latter analyses results by grouping results by surface type. The statistical analyses were limited due to low frequency of detections and dilutions of samples which impacted detection limits. The infiltrate data through three permeable surfaces were analyzed as non-parametric data by the Kaplan-Meier estimation method for fundamental statistics; there were some statistically observable difference in concentration between pavement types when using Tarone-Ware Comparison Hypothesis Test. Additionally Spearman Rank order non-parame

Analysis of metalaxyl racemate using high performance liquid chromatography coupled with four kinds of detectors.

PubMed

Chen, Tao; Fan, Jun; Gao, Ruiqi; Wang, Tai; Yu, Ying; Zhang, Weiguang

2016-10-07

Chiral stationary phase-high performance liquid chromatography coupled with various detectors has been one of most commonly used methods for analysis and separation of chiral compounds over the past decades. Various detectors exhibit different characteristics in qualitative and quantitative studies under different chromatographic conditions. Herein, a comparative evaluation of HPLC coupled with ultraviolet, optical rotation, refractive index, and evaporative light scattering detectors has been conducted for qualitative and quantitative analyses of metalaxyl racemate. Effects of separation conditions on the peak area ratio between two enantiomers, including sample concentration, column temperature, mobile phase composition, as well as flow rate, have been investigated in detail. In addition, the limits of detection, the limits of quantitation, quantitative range and precision for these two enantiomers by using four detectors have been also studied. As indicated, the chromatographic separation conditions have been slight effects on ultraviolet and refractive index detections and the peak area ratio between two enantiomers remains almost unchanged, but the evaporative light scattering detection has been significantly affected by the above-mentioned chromatographic conditions and the corresponding peak area ratios varied greatly. Moreover, the limits of detection, the limits of quantitation, and the quantitative ranges of two enantiomers with UV detection were remarkably lower by 1-2 magnitudes than the others. Copyright © 2016 Elsevier B.V. All rights reserved.

Computerized Lung Sound Analysis as diagnostic aid for the detection of abnormal lung sounds: a systematic review and meta-analysis

PubMed Central

Gurung, Arati; Scrafford, Carolyn G; Tielsch, James M; Levine, Orin S; Checkley, William

2011-01-01

Rationale The standardized use of a stethoscope for chest auscultation in clinical research is limited by its inherent inter-listener variability. Electronic auscultation and automated classification of recorded lung sounds may help prevent some these shortcomings. Objective We sought to perform a systematic review and meta-analysis of studies implementing computerized lung sounds analysis (CLSA) to aid in the detection of abnormal lung sounds for specific respiratory disorders. Methods We searched for articles on CLSA in MEDLINE, EMBASE, Cochrane Library and ISI Web of Knowledge through July 31, 2010. Following qualitative review, we conducted a meta-analysis to estimate the sensitivity and specificity of CLSA for the detection of abnormal lung sounds. Measurements and Main Results Of 208 articles identified, we selected eight studies for review. Most studies employed either electret microphones or piezoelectric sensors for auscultation, and Fourier Transform and Neural Network algorithms for analysis and automated classification of lung sounds. Overall sensitivity for the detection of wheezes or crackles using CLSA was 80% (95% CI 72–86%) and specificity was 85% (95% CI 78–91%). Conclusions While quality data on CLSA are relatively limited, analysis of existing information suggests that CLSA can provide a relatively high specificity for detecting abnormal lung sounds such as crackles and wheezes. Further research and product development could promote the value of CLSA in research studies or its diagnostic utility in clinical setting. PMID:21676606

Computerized lung sound analysis as diagnostic aid for the detection of abnormal lung sounds: a systematic review and meta-analysis.

PubMed

Gurung, Arati; Scrafford, Carolyn G; Tielsch, James M; Levine, Orin S; Checkley, William

2011-09-01

The standardized use of a stethoscope for chest auscultation in clinical research is limited by its inherent inter-listener variability. Electronic auscultation and automated classification of recorded lung sounds may help prevent some of these shortcomings. We sought to perform a systematic review and meta-analysis of studies implementing computerized lung sound analysis (CLSA) to aid in the detection of abnormal lung sounds for specific respiratory disorders. We searched for articles on CLSA in MEDLINE, EMBASE, Cochrane Library and ISI Web of Knowledge through July 31, 2010. Following qualitative review, we conducted a meta-analysis to estimate the sensitivity and specificity of CLSA for the detection of abnormal lung sounds. Of 208 articles identified, we selected eight studies for review. Most studies employed either electret microphones or piezoelectric sensors for auscultation, and Fourier Transform and Neural Network algorithms for analysis and automated classification of lung sounds. Overall sensitivity for the detection of wheezes or crackles using CLSA was 80% (95% CI 72-86%) and specificity was 85% (95% CI 78-91%). While quality data on CLSA are relatively limited, analysis of existing information suggests that CLSA can provide a relatively high specificity for detecting abnormal lung sounds such as crackles and wheezes. Further research and product development could promote the value of CLSA in research studies or its diagnostic utility in clinical settings. Copyright © 2011 Elsevier Ltd. All rights reserved.

Detection of proteolytic activity by covalent tethering of fluorogenic substrates in zymogram gels.

PubMed

Deshmukh, Ameya A; Weist, Jessica L; Leight, Jennifer L

2018-05-01

Current zymographic techniques detect only a subset of known proteases due to the limited number of native proteins that have been optimized for incorporation into polyacrylamide gels. To address this limitation, we have developed a technique to covalently incorporate fluorescently labeled, protease-sensitive peptides using an azido-PEG3-maleimide crosslinker. Peptides incorporated into gels enabled measurement of MMP-2, -9, -14, and bacterial collagenase. Sensitivity analysis demonstrated that use of peptide functionalized gels could surpass detection limits of current techniques. Finally, electrophoresis of conditioned media from cultured cells resulted in the appearance of several proteolytic bands, some of which were undetectable by gelatin zymography. Taken together, these results demonstrate that covalent incorporation of fluorescent substrates can greatly expand the library of detectable proteases using zymographic techniques.

Laboratory evaluation of a field-portable sealed source X-ray fluorescence spectrometer for determination of metals in air filter samples.

PubMed

Lawryk, Nicholas J; Feng, H Amy; Chen, Bean T

2009-07-01

Recent advances in field-portable X-ray fluorescence (FP XRF) spectrometer technology have made it a potentially valuable screening tool for the industrial hygienist to estimate worker exposures to airborne metals. Although recent studies have shown that FP XRF technology may be better suited for qualitative or semiquantitative analysis of airborne lead in the workplace, these studies have not extensively addressed its ability to measure other elements. This study involved a laboratory-based evaluation of a representative model FP XRF spectrometer to measure elements commonly encountered in workplace settings that may be collected on air sample filter media, including chromium, copper, iron, manganese, nickel, lead, and zinc. The evaluation included assessments of (1) response intensity with respect to location on the probe window, (2) limits of detection for five different filter media, (3) limits of detection as a function of analysis time, and (4) bias, precision, and accuracy estimates. Teflon, polyvinyl chloride, polypropylene, and mixed cellulose ester filter media all had similarly low limits of detection for the set of elements examined. Limits of detection, bias, and precision generally improved with increasing analysis time. Bias, precision, and accuracy estimates generally improved with increasing element concentration. Accuracy estimates met the National Institute for Occupational Safety and Health criterion for nearly all the element and concentration combinations. Based on these results, FP XRF spectrometry shows potential to be useful in the assessment of worker inhalation exposures to other metals in addition to lead.

Demonstration and Evaluation of Solid Phase Microextraction for the Assessment of Bioavailability and Contaminant Mobility. ESTCP Cost and Performance Report

DTIC Science & Technology

2012-08-01

subsequent chemical analysis (into acetonitrile for high-performance liquid chromatography [ HPLC ] analysis or hexane for gas chromatography [GC... analysis ) is rapid and complete. In this work, PAHs were analyzed by Waters 2795 HPLC with fluorescent detection (USEPA Method 8310) and PCBs were...detection limits by direct water injection versus SPME with PDMS and coefficient of variation and correlation coefficient for SPME. Analysis by HPLC

Kernel-Phase Interferometry for Super-Resolution Detection of Faint Companions

NASA Astrophysics Data System (ADS)

Factor, Samuel M.; Kraus, Adam L.

2017-06-01

Direct detection of close in companions (exoplanets or binary systems) is notoriously difficult. While coronagraphs and point spread function (PSF) subtraction can be used to reduce contrast and dig out signals of companions under the PSF, there are still significant limitations in separation and contrast near λ/D. Non-redundant aperture masking (NRM) interferometry can be used to detect companions well inside the PSF of a diffraction limited image, though the mask discards ˜ 95% of the light gathered by the telescope and thus the technique is severely flux limited. Kernel-phase analysis applies interferometric techniques similar to NRM to a diffraction limited image utilizing the full aperture. Instead of non-redundant closure-phases, kernel-phases are constructed from a grid of points on the full aperture, simulating a redundant interferometer. I have developed a new, easy to use, faint companion detection pipeline which analyzes kernel-phases utilizing Bayesian model comparison. I demonstrate this pipeline on archival images from HST/NICMOS, searching for new companions in order to constrain binary formation models at separations inaccessible to previous techniques. Using this method, it is possible to detect a companion well within the classical λ/D Rayleigh diffraction limit using a fraction of the telescope time as NRM. Since the James Webb Space Telescope (JWST) will be able to perform NRM observations, further development and characterization of kernel-phase analysis will allow efficient use of highly competitive JWST telescope time. As no mask is needed, this technique can easily be applied to archival data and even target acquisition images (e.g. from JWST), making the detection of close in companions cheap and simple as no additional observations are needed.

Simultaneous analysis of six aldehyde-DNA adducts in salivary DNA of nonsmokers and smokers using stable isotope dilution liquid chromatography electrospray ionization-tandem mass spectrometry.

PubMed

Li, Xiangyu; Liu, Lujuan; Wang, Hongjuan; Chen, Jian; Zhu, Beibei; Chen, Huan; Hou, Hongwei; Hu, Qingyuan

2017-08-15

A stable method, using isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS), to simultaneously determine six aldehyde-DNA adducts was developed and applied to the analysis of human salivary DNA samples. The detection limit of these six DNA adducts was in the range of 0.006-0.014ng/mL and that of the quantification limit was 0.017-0.026ng/mL. The intra-day and inter-day precision of all aldehyde-DNA adducts was <10%. The analysis was completed within 25min. Additionally, a noninvasive technique was used to collect the DNA samples from human saliva. The new method was successfully applied for the analysis of salivary DNA of nonsmokers and smokers. Five aldehyde-DNA adducts were detected in both smoker and nonsmoker salivary DNA, while α-Acr-dG was not detected in all the samples. Among these detected DNA adducts, no significant differences were found between smoker and nonsmoker (p>0.05). This may due to the individual detoxifying differences or environmental and endogenous exposure. Our study provides a rapid and selective method to simultaneously detect six aldehyde-DNA adducts and to assess potential DNA damage induced by aldehydes. Copyright © 2017 Elsevier B.V. All rights reserved.

USE OF TRANSCRIPTIONAL COUPLING AND KEGG PATHWAY ANALYSIS OF GLOBAL GENE EXPRESSION TO REVEAL TRANSCRIPTIONAL CHANGES BETWEEN STATIONARY- AND LOG-PHASE SALMONELLA TYPHIMURIUM LT2

EPA Science Inventory

DNA microarray analysis is plagued by a lack of data reproducibility and by limits to the detectability of transcripts by hybridization. To mitigate these limitations, we employed transcriptional coupling within the S. typhimurium genome. This genome has 2664 transcriptionally co...

Capillary electrophoresis with laser-induced fluorescence detection: a sensitive method for monitoring extracellular concentrations of amino acids in the periaqueductal grey matter.

PubMed

Bergquist, J; Vona, M J; Stiller, C O; O'Connor, W T; Falkenberg, T; Ekman, R

1996-03-01

The use of capillary electrophoresis with laser-induced fluorescence detection (CE-LIF) for the analysis of microdialysate samples from the periaqueductal grey matter (PAG) of freely moving rats is described. By employing 3-(4-carboxybenzoyl)-2-quinoline-carboxaldehyde (CBQCA) as a derivatization agent, we simultaneously monitored the concentrations of 8 amino acids (arginine, glutamine, valine, gamma-amino-n-butyric acid (GABA), alanine, glycine, glutamate, and aspartate), with nanomolar and subnanomolar detection limits. Two of the amino acids (GABA and glutamate) were analysed in parallel by conventional high-performance liquid chromatography (HPLC) in order to directly compare the two analytical methods. Other CE methods for analysis of microdialysate have been previously described, and this improved method offers greater sensitivity, ease of use, and the possibility to monitor several amino acids simultaneously. By using this technique together with an optimised form of microdialysis technique, the tiny sample consumption and the improved detection limits permit the detection of fast and transient transmitter changes.

Selective counting and sizing of single virus particles using fluorescent aptamer-based nanoparticle tracking analysis.

PubMed

Szakács, Zoltán; Mészáros, Tamás; de Jonge, Marien I; Gyurcsányi, Róbert E

2018-05-30

Detection and counting of single virus particles in liquid samples are largely limited to narrow size distribution of viruses and purified formulations. To address these limitations, here we propose a calibration-free method that enables concurrently the selective recognition, counting and sizing of virus particles as demonstrated through the detection of human respiratory syncytial virus (RSV), an enveloped virus with a broad size distribution, in throat swab samples. RSV viruses were selectively labeled through their attachment glycoproteins (G) with fluorescent aptamers, which further enabled their identification, sizing and counting at the single particle level by fluorescent nanoparticle tracking analysis. The proposed approach seems to be generally applicable to virus detection and quantification. Moreover, it could be successfully applied to detect single RSV particles in swab samples of diagnostic relevance. Since the selective recognition is associated with the sizing of each detected particle, this method enables to discriminate viral elements linked to the virus as well as various virus forms and associations.

Portable TXRF Spectrometer with 10{sup -11}g Detection Limit and Portable XRF Spectromicroscope with Sub-mm Spatial Resolution

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

Kunimura, Shinsuke; Hatakeyama, So; Sasaki, Nobuharu

A portable total reflection X-ray fluorescence (TXRF) spectrometer that we have developed is applied to trace elemental analysis of water solutions. Although a 5 W X-ray tube is used in the portable TXRF spectrometer, detection limits of several ppb are achieved for 3d transition metal elements and trace elements in a leaching solution of soils, a leaching solution of solder, and alcoholic beverages are detected. Portable X-ray fluorescence (XRF) spectromicroscopes with a 1 W X-ray tube and an 8 W X-ray tube are also presented. Using the portable XRF spectromicroscope with the 1 W X-ray tube, 93 ppm of Crmore » is detected with an about 700 {mu}m spatial resolution. Spatially resolved elemental analysis of a mug painted with blue, red, green, and white is performed using the two portable spectromicroscopes, and the difference in elemental composition at each paint is detected.« less

Analysis of Urinary Metabolites of Nerve and Blister Chemical Warfare Agents

DTIC Science & Technology

2014-08-01

of CWAs. The analysis methods use UHPLC-MS/MS in Multiple Reaction Monitoring ( MRM ) mode to enhance the selectivity and sensitivity of the method...Chromatography Mass Spectrometry LOD Limit Of Detection LOQ Limit of Quantitation MRM Multiple Reaction Monitoring MSMS Tandem mass...urine [1]. Those analysis methods use UHPLC- MS/MS in Multiple Reaction Monitoring ( MRM ) mode to enhance the selectivity and sensitivity of the method

Qualitative analysis of seized cocaine samples using desorption electrospray ionization- mass spectrometry (DESI-MS).

PubMed

Stojanovska, Natasha; Tahtouh, Mark; Kelly, Tamsin; Beavis, Alison; Fu, Shanlin

2015-05-01

Desorption electrospray ionization - mass spectrometry (DESI-MS) is a useful technique for the qualitative analysis of compounds found in seized drug material. In this study, DESI-MS was utilized in the screening analysis of illicit cocaine samples. The technique was also applied to the geographical origin determination of these samples. The limit of detection was determined to be 24.3 µg (or 3.47 µg/mm(2) ) and the analysis time was less than 1 minute per sample. The intra-day and inter-day precision for the detection of cocaine was 11 % and 42 %, respectively; therefore the quantitative data provided by DESI-MS was limited in its use for accurate determination of cocaine concentration in a sample. Using the quadrupole time-of-flight (QTOF) mass spectrometer, the presence of cocaine and impurities detected were confirmed by accurate tandem MS data. The qualitative chemical profiles obtained using DESI-MS were compared to two popular analysis techniques, GC-MS and LC-MS. The effects of a range of adulterants including caffeine, procaine, levamisole, lignocaine, paracetamol, and atropine on the detectability of cocaine were also investigated. It was found that the addition of these adulterants in a cocaine sample did not prevent the detection of the analyte itself (there was slight enhancement in some samples), which was useful in drug detection. The detection of truxillines in the seized samples by DESI-MS aided in the preliminary determination of geographical origin, i.e., Bolivian, Peruvian or Colombian leaf origin. The application of DESI-MS to the qualitative analysis and screening of seized cocaine samples demonstrates the potential and applicability of the technique to the fast chemical profiling of illicit samples. Copyright © 2014 John Wiley & Sons, Ltd.

Development and validation of an universal interface for compound-specific stable isotope analysis of chlorine (37Cl/35Cl) by GC-high-temperature conversion (HTC)-MS/IRMS.

PubMed

Renpenning, Julian; Hitzfeld, Kristina L; Gilevska, Tetyana; Nijenhuis, Ivonne; Gehre, Matthias; Richnow, Hans-Hermann

2015-03-03

A universal application of compound-specific isotope analysis of chlorine was thus far limited by the availability of suitable analysis techniques. In this study, gas chromatography in combination with a high-temperature conversion interface (GC-HTC), converting organic chlorine in the presence of H2 to gaseous HCl, was coupled to a dual-detection system, combining an ion trap mass spectrometer (MS) and isotope-ratio mass spectrometer (IRMS). The combination of the MS/IRMS detection enabled a detailed characterization, optimization, and online monitoring of the high-temperature conversion process via ion trap MS as well as a simultaneous chlorine isotope analysis by the IRMS. Using GC-HTC-MS/IRMS, chlorine isotope analysis at optimized conversion conditions resulted in very accurate isotope values (δ(37)Cl(SMOC)) for measured reference material with known isotope composition, including chlorinated ethylene, chloromethane, hexachlorocyclohexane, and trichloroacetic acids methyl ester. Respective detection limits were determined to be <15 nmol Cl on column with achieved precision of <0.3‰.

Microbial Diagnostic Microarrays for the Detection and Typing of Food- and Water-Borne (Bacterial) Pathogens

PubMed Central

Kostić, Tanja; Sessitsch, Angela

2011-01-01

Reliable and sensitive pathogen detection in clinical and environmental (including food and water) samples is of greatest importance for public health. Standard microbiological methods have several limitations and improved alternatives are needed. Most important requirements for reliable analysis include: (i) specificity; (ii) sensitivity; (iii) multiplexing potential; (iv) robustness; (v) speed; (vi) automation potential; and (vii) low cost. Microarray technology can, through its very nature, fulfill many of these requirements directly and the remaining challenges have been tackled. In this review, we attempt to compare performance characteristics of the microbial diagnostic microarrays developed for the detection and typing of food and water pathogens, and discuss limitations, points still to be addressed and issues specific for the analysis of food, water and environmental samples. PMID:27605332

Nonparametric rank regression for analyzing water quality concentration data with multiple detection limits.

PubMed

Fu, Liya; Wang, You-Gan

2011-02-15

Environmental data usually include measurements, such as water quality data, which fall below detection limits, because of limitations of the instruments or of certain analytical methods used. The fact that some responses are not detected needs to be properly taken into account in statistical analysis of such data. However, it is well-known that it is challenging to analyze a data set with detection limits, and we often have to rely on the traditional parametric methods or simple imputation methods. Distributional assumptions can lead to biased inference and justification of distributions is often not possible when the data are correlated and there is a large proportion of data below detection limits. The extent of bias is usually unknown. To draw valid conclusions and hence provide useful advice for environmental management authorities, it is essential to develop and apply an appropriate statistical methodology. This paper proposes rank-based procedures for analyzing non-normally distributed data collected at different sites over a period of time in the presence of multiple detection limits. To take account of temporal correlations within each site, we propose an optimal linear combination of estimating functions and apply the induced smoothing method to reduce the computational burden. Finally, we apply the proposed method to the water quality data collected at Susquehanna River Basin in United States of America, which clearly demonstrates the advantages of the rank regression models.

Nanotechnology: moving from microarrays toward nanoarrays.

PubMed

Chen, Hua; Li, Jun

2007-01-01

Microarrays are important tools for high-throughput analysis of biomolecules. The use of microarrays for parallel screening of nucleic acid and protein profiles has become an industry standard. A few limitations of microarrays are the requirement for relatively large sample volumes and elongated incubation time, as well as the limit of detection. In addition, traditional microarrays make use of bulky instrumentation for the detection, and sample amplification and labeling are quite laborious, which increase analysis cost and delays the time for obtaining results. These problems limit microarray techniques from point-of-care and field applications. One strategy for overcoming these problems is to develop nanoarrays, particularly electronics-based nanoarrays. With further miniaturization, higher sensitivity, and simplified sample preparation, nanoarrays could potentially be employed for biomolecular analysis in personal healthcare and monitoring of trace pathogens. In this chapter, it is intended to introduce the concept and advantage of nanotechnology and then describe current methods and protocols for novel nanoarrays in three aspects: (1) label-free nucleic acids analysis using nanoarrays, (2) nanoarrays for protein detection by conventional optical fluorescence microscopy as well as by novel label-free methods such as atomic force microscopy, and (3) nanoarray for enzymatic-based assay. These nanoarrays will have significant applications in drug discovery, medical diagnosis, genetic testing, environmental monitoring, and food safety inspection.

Nonlethal evaluation of the physiological health of unionid mussels: Method for biopsy and glycogen analysis

USGS Publications Warehouse

Naimo, T.J.; Damschen, E.D.; Rada, R.G.; Monroe, E.M.

1998-01-01

In long-lived unionid mussels, many short-term measures of growth are of limited value. Changes in physiological condition may be an early indication of stress, because the increased energy demand associated with stress often results in a depletion of glycogen reserves, the principal storage form of carbohydrates in unionid mussels. Our goal was to nonlethally extract tissue from freshwater mussels and then to develop a rapid and dependable method for the analysis of glycogen in the tissue extracts. A biopsy technique was developed to remove between 5 and 10 mg of food tissue in Amblema plicata plicata. The survival rate did not differ between biopsied and non-biopsied mussels during a 581-d observation period, demonstrating that the biopsy technique will allow nonlethal evaluation of the physiological condition of individual mussels through measurement of changes in contaminant, genetic, and biochemical indicators in tissue. We also modified the standard alkaline digestion and phenol-sulfuric acid analysis of glycogen for use on the small samples of biopsied tissue and to reduce analysis time and cost. We present quality control data, including method detection limits and estimates of precision and bias. The modified analytical method is rapid and accurate and has a method detection limit of 0.014 mg glycogen. Glycogen content in the biopsied samples was well above the method detection limit; it ranged from 0.09 to 0.36 mg, indicating that the method should be applicable to native mussels.

Cycling temperature capillary electrophoresis: A quantitative, fast and inexpensive method to detect mutations in mixed populations of human mitochondrial DNA.

PubMed

Refinetti, Paulo; Morgenthaler, Stephan; Ekstrøm, Per O

2016-07-01

Cycling temperature capillary electrophoresis has been optimised for mutation detection in 76% of the mitochondrial genome. The method was tested on a mixed sample and compared to mutation detection by next generation sequencing. Out of 152 fragments 90 were concordant, 51 discordant and in 11 were semi-concordant. Dilution experiments show that cycling capillary electrophoresis has a detection limit of 1-3%. The detection limit of routine next generation sequencing was in the ranges of 15 to 30%. Cycling temperature capillary electrophoresis detect and accurate quantify mutations at a fraction of the cost and time required to perform a next generation sequencing analysis. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

Detection of silver nanoparticles in seawater at ppb levels using UV-visible spectrophotometry with long path cells.

PubMed

Lodeiro, Pablo; Achterberg, Eric P; El-Shahawi, Mohammad S

2017-03-01

Silver nanoparticles (AgNPs) are emerging contaminants that are difficult to detect in natural waters. UV-visible spectrophotometry is a simple technique that allows detection of AgNPs through analysis of their characteristic surface plasmon resonance band. The detection limit for nanoparticles using up to 10cm path length cuvettes with UV-visible spectrophotometry is in the 0.1-10ppm range. This detection limit is insufficiently low to observe AgNPs in natural environments. Here we show how the use of capillary cells with an optical path length up to 200cm, forms an excellent technique for rapid detection and quantification of non-aggregated AgNPs at ppb concentrations in complex natural matrices such as seawater. Copyright © 2016 Elsevier B.V. All rights reserved.

THE USE AND LIMITATIONS OF DETECTION AND QUANTITATION LIMITS IN ENVIRONMENTAL ANALYSIS

EPA Science Inventory

Site assessment, remediation and compliance monitoring require the routine determination of the concentration of regulated substances in environmental samples. Each measurement methodology providing the concentration determinations, is required to specify key data quality elemen...

One-step liquid-liquid extraction of cocaine from urine samples for gas chromatographic analysis.

PubMed

Farina, Marcelo; Yonamine, Maurício; Silva, Ovandir A

2002-07-17

An improved technique for cocaine extraction from urine samples for gas chromatographic (GC) analysis is described. Employing a simple liquid-liquid extraction (LLE) of cocaine with a mixture of ethyl ether:isopropanol (9:1) the method presents a mean recovery of 74.49%. Limit of detection (LOD) and limit of quantification (LOQ) were 5 and 20 ng/ml, respectively. The method is highly precise (coefficient of variation (CV) <8%) and linear from 20 to 2000 ng/ml. It can he applied to detect the presence of cocaine in urine as a marker of its recent use in drug abuse treatment protocols.

Concentrations of platinum group elements in 122 U.S. coal samples

USGS Publications Warehouse

Oman, C.L.; Finkelman, R.B.; Tewalt, S.J.

1997-01-01

Analysis of more than 13,000 coal samples by semi-quantitative optical emission spectroscopy (OES) indicates that concentrations of the platinum group elements (iridium, palladium, platinum, osmium, rhodium, and ruthenium) are less than 1 ppm in the ash, the limit of detection for this method of analysis. In order to accurately determine the concentration of the platinum group elements (PGE) in coal, additional data were obtained by inductively coupled plasma mass spectroscopy, an analytical method having part-per-billion (ppb) detection limits for these elements. These data indicate that the PGE in coal occur in concentrations on the order of 1 ppb or less.

Rapid Determination of Lymphogranuloma Venereum Serovars of Chlamydia trachomatis by Quantitative High-Resolution Melt Analysis (HRMA)

PubMed Central

Stevens, Matthew P.; Garland, Suzanne M.; Zaia, Angelo M.; Tabrizi, Sepehr N.

2012-01-01

A quantitative high-resolution melt analysis assay was developed to differentiate lymphogranuloma venereum-causing serovars of Chlamydia trachomatis (L1 to L3) from other C. trachomatis serovars (D to K). The detection limit of this assay is approximately 10 copies per reaction, comparable to the limits of other quantitative-PCR-based methods. PMID:22933594

Photoelectrochemical detection of benzaldehyde in foodstuffs

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

LaCourse, W.R.; Krull, I.S.

Photoelectrochemical detection (PED) coupled with high performance liquid chromatography was used to quantitatively determine benzaldehyde in extracts, beverages, and foodstuffs. Photoelectrochemical detection is responsive to alkyl and aryl ketones and aldehydes and offers the advantages of 2-3 orders of magnitude linearity, 5-1-ng limits of detection, and a high degree of selectivity without chemical derivatization. This is the first application of the PED to sample analysis.

Electrochemistry and Spectroelectrochemistry of Luminescent Europium Complexes

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

Lines, Amanda M.; Wang, Zheming; Clark, Sue B.

Fast, cost effective, and robust means of detecting and quantifying lanthanides are needed for supporting more efficient tracking within the nuclear, medicinal, and industrial fields. Spectroelectrochemistry (SEC) is a powerful technique combining electrochemistry and spectroscopy that can meet those needs. The primary limitation of SEC as a detection method for lanthanides is their low molar absorptivity in absorbance based measurements and low emission intensities in fluorescence based measurements; both lead to high limits of detection. These limitations can be circumvented by complexing the lanthanides with sensitizing ligands that enhance fluorescence, thereby dropping the limits of detection. Complexation may also stabilizemore » the metal ions in solution and improve the electrochemical reversibility, or Nernstian behavior, of the redox couples. To demonstrate this concept, studies were completed using europium in complexes with four different sensitizing ligands. Initial work indicates Eu in the four complexes studied does display the necessary characteristics for SEC analysis, which was successfully and reproducibly applied to all Eu complexes.« less

Network hydraulics inclusion in water quality event detection using multiple sensor stations data.

PubMed

Oliker, Nurit; Ostfeld, Avi

2015-09-01

Event detection is one of the current most challenging topics in water distribution systems analysis: how regular on-line hydraulic (e.g., pressure, flow) and water quality (e.g., pH, residual chlorine, turbidity) measurements at different network locations can be efficiently utilized to detect water quality contamination events. This study describes an integrated event detection model which combines multiple sensor stations data with network hydraulics. To date event detection modelling is likely limited to single sensor station location and dataset. Single sensor station models are detached from network hydraulics insights and as a result might be significantly exposed to false positive alarms. This work is aimed at decreasing this limitation through integrating local and spatial hydraulic data understanding into an event detection model. The spatial analysis complements the local event detection effort through discovering events with lower signatures by exploring the sensors mutual hydraulic influences. The unique contribution of this study is in incorporating hydraulic simulation information into the overall event detection process of spatially distributed sensors. The methodology is demonstrated on two example applications using base runs and sensitivity analyses. Results show a clear advantage of the suggested model over single-sensor event detection schemes. Copyright © 2015 Elsevier Ltd. All rights reserved.

Detection of Salmonella enterica Serovar Typhimurium by Using a Rapid, Array-Based Immunosensor

PubMed Central

Taitt, Chris Rowe; Shubin, Yura S.; Angel, Roselina; Ligler, Frances S.

2004-01-01

The multianalyte array biosensor (MAAB) is a rapid analysis instrument capable of detecting multiple analytes simultaneously. Rapid (15-min), single-analyte sandwich immunoassays were developed for the detection of Salmonella enterica serovar Typhimurium, with a detection limit of 8 × 104 CFU/ml; the limit of detection was improved 10-fold by lengthening the assay protocol to 1 h. S. enterica serovar Typhimurium was also detected in the following spiked foodstuffs, with minimal sample preparation: sausage, cantaloupe, whole liquid egg, alfalfa sprouts, and chicken carcass rinse. Cross-reactivity tests were performed with Escherichia coli and Campylobacter jejuni. To determine whether the MAAB has potential as a screening tool for the diagnosis of asymptomatic Salmonella infection of poultry, chicken excretal samples from a private, noncommercial farm and from university poultry facilities were tested. While the private farm excreta gave rise to signals significantly above the buffer blanks, none of the university samples tested positive for S. enterica serovar Typhimurium without spiking; dose-response curves of spiked excretal samples from university-raised poultry gave limits of detection of 8 × 103 CFU/g. PMID:14711637

Kinetic Modeling of Accelerated Stability Testing Enabled by Second Harmonic Generation Microscopy.

PubMed

Song, Zhengtian; Sarkar, Sreya; Vogt, Andrew D; Danzer, Gerald D; Smith, Casey J; Gualtieri, Ellen J; Simpson, Garth J

2018-04-03

The low limits of detection afforded by second harmonic generation (SHG) microscopy coupled with image analysis algorithms enabled quantitative modeling of the temperature-dependent crystallization of active pharmaceutical ingredients (APIs) within amorphous solid dispersions (ASDs). ASDs, in which an API is maintained in an amorphous state within a polymer matrix, are finding increasing use to address solubility limitations of small-molecule APIs. Extensive stability testing is typically performed for ASD characterization, the time frame for which is often dictated by the earliest detectable onset of crystal formation. Here a study of accelerated stability testing on ritonavir, a human immunodeficiency virus (HIV) protease inhibitor, has been conducted. Under the condition for accelerated stability testing at 50 °C/75%RH and 40 °C/75%RH, ritonavir crystallization kinetics from amorphous solid dispersions were monitored by SHG microscopy. SHG microscopy coupled by image analysis yielded limits of detection for ritonavir crystals as low as 10 ppm, which is about 2 orders of magnitude lower than other methods currently available for crystallinity detection in ASDs. The four decade dynamic range of SHG microscopy enabled quantitative modeling with an established (JMAK) kinetic model. From the SHG images, nucleation and crystal growth rates were independently determined.

SU-E-T-144: Effective Analysis of VMAT QA Generated Trajectory Log Files for Medical Accelerator Predictive Maintenance

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

Able, CM; Baydush, AH; Nguyen, C

Purpose: To determine the effectiveness of SPC analysis for a model predictive maintenance process that uses accelerator generated parameter and performance data contained in trajectory log files. Methods: Each trajectory file is decoded and a total of 131 axes positions are recorded (collimator jaw position, gantry angle, each MLC, etc.). This raw data is processed and either axis positions are extracted at critical points during the delivery or positional change over time is used to determine axis velocity. The focus of our analysis is the accuracy, reproducibility and fidelity of each axis. A reference positional trace of the gantry andmore » each MLC is used as a motion baseline for cross correlation (CC) analysis. A total of 494 parameters (482 MLC related) were analyzed using Individual and Moving Range (I/MR) charts. The chart limits were calculated using a hybrid technique that included the use of the standard 3σ limits and parameter/system specifications. Synthetic errors/changes were introduced to determine the initial effectiveness of I/MR charts in detecting relevant changes in operating parameters. The magnitude of the synthetic errors/changes was based on: TG-142 and published analysis of VMAT delivery accuracy. Results: All errors introduced were detected. Synthetic positional errors of 2mm for collimator jaw and MLC carriage exceeded the chart limits. Gantry speed and each MLC speed are analyzed at two different points in the delivery. Simulated Gantry speed error (0.2 deg/sec) and MLC speed error (0.1 cm/sec) exceeded the speed chart limits. Gantry position error of 0.2 deg was detected by the CC maximum value charts. The MLC position error of 0.1 cm was detected by the CC maximum value location charts for every MLC. Conclusion: SPC I/MR evaluation of trajectory log file parameters may be effective in providing an early warning of performance degradation or component failure for medical accelerator systems.« less

ON COMPUTING UPPER LIMITS TO SOURCE INTENSITIES

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

Kashyap, Vinay L.; Siemiginowska, Aneta; Van Dyk, David A.

2010-08-10

A common problem in astrophysics is determining how bright a source could be and still not be detected in an observation. Despite the simplicity with which the problem can be stated, the solution involves complicated statistical issues that require careful analysis. In contrast to the more familiar confidence bound, this concept has never been formally analyzed, leading to a great variety of often ad hoc solutions. Here we formulate and describe the problem in a self-consistent manner. Detection significance is usually defined by the acceptable proportion of false positives (background fluctuations that are claimed as detections, or Type I error),more » and we invoke the complementary concept of false negatives (real sources that go undetected, or Type II error), based on the statistical power of a test, to compute an upper limit to the detectable source intensity. To determine the minimum intensity that a source must have for it to be detected, we first define a detection threshold and then compute the probabilities of detecting sources of various intensities at the given threshold. The intensity that corresponds to the specified Type II error probability defines that minimum intensity and is identified as the upper limit. Thus, an upper limit is a characteristic of the detection procedure rather than the strength of any particular source. It should not be confused with confidence intervals or other estimates of source intensity. This is particularly important given the large number of catalogs that are being generated from increasingly sensitive surveys. We discuss, with examples, the differences between these upper limits and confidence bounds. Both measures are useful quantities that should be reported in order to extract the most science from catalogs, though they answer different statistical questions: an upper bound describes an inference range on the source intensity, while an upper limit calibrates the detection process. We provide a recipe for computing upper limits that applies to all detection algorithms.« less

Trueness, Precision, and Detectability for Sampling and Analysis of Organic Species in Airborne Particulate Matter

EPA Science Inventory

Recovery. precision, limits of detection and quantitation, blank levels, calibration linearity, and agreement with certified reference materials were determined for two classes of organic components of airborne particulate matter, polycyclic aromatic hydrocarbons and hopanes usin...

Rapid and sensitive detection of canine parvovirus type 2 by recombinase polymerase amplification.

PubMed

Wang, Jianchang; Liu, Libing; Li, Ruiwen; Wang, Jinfeng; Fu, Qi; Yuan, Wanzhe

2016-04-01

A novel recombinase polymerase amplification (RPA)-based method for detection of canine parvovirus type 2 (CPV-2) was developed. Sensitivity analysis showed that the detection limit of RPA was 10 copies of CPV-2 genomic DNA. RPA amplified both CPV-2a and -2b DNA but did not amplify the template of other important dog viruses (CCoV, PRV or CDV), demonstrating high specificity. The method was further validated with 57 canine fecal samples. An outstanding advantage of RPA is that it is an isothermal reaction and can be performed in a water bath, making RPA a potential alternative method for CPV-2 detection in resource-limited settings.

Multi-modality analysis of glucose aqueous solution using photoacoustic and dielectric spectroscopy for non-invasive glucose monitoring

NASA Astrophysics Data System (ADS)

Tajima, Takuro; Tanaka, Yujiro; Nakamura, Masahito; Seyama, Michiko

2017-03-01

Quantitative analysis of glucose using conventional optical spectroscopy suffers from a lack of repeatability due to high optical scattering in skin tissue. Here we present a multi-modality analysis of glucose aqueous solution using photoacoustic spectroscopy (PAS) and broadband dielectric spectroscopy (BDS). These techniques involve the direct detection of the acoustic and electromagnetic waves propagating through or reflecting from tissue without their being scattered. They therefore have potential for better tolerance to the variation of scattering. For PAS, to differentiate signals induced by water absorption, we select another laser wavelength (1.38 μm) that exhibits the same absorbance for water at 1.61 μm. Furthermore, one of the two photoacoustic signals is used to normalize the variations of acoustic properties in differential signal. Measured results for glucose solutions (0-2 g/dL) showed that the differential signal has a sensitivity of 1.61%/g·dL-1 and a detection limit of 120 mg/dL. We also tested glucose detection with BDS (500 MHz to 50 GHz) by detecting glucose hydration bonding at around 10-20 GHz. Using a partial least square analysis and first derivation on broadband spectra, we obtained an RMS error 19 mg/dL and a detection limit of 59 mg/dL. Using both the low-scattering ultrasonic and microwave detection techniques, we successfully captured the glucose footprint in the physiological range.

Application of principal component regression and partial least squares regression in ultraviolet spectrum water quality detection

NASA Astrophysics Data System (ADS)

Li, Jiangtong; Luo, Yongdao; Dai, Honglin

2018-01-01

Water is the source of life and the essential foundation of all life. With the development of industrialization, the phenomenon of water pollution is becoming more and more frequent, which directly affects the survival and development of human. Water quality detection is one of the necessary measures to protect water resources. Ultraviolet (UV) spectral analysis is an important research method in the field of water quality detection, which partial least squares regression (PLSR) analysis method is becoming predominant technology, however, in some special cases, PLSR's analysis produce considerable errors. In order to solve this problem, the traditional principal component regression (PCR) analysis method was improved by using the principle of PLSR in this paper. The experimental results show that for some special experimental data set, improved PCR analysis method performance is better than PLSR. The PCR and PLSR is the focus of this paper. Firstly, the principal component analysis (PCA) is performed by MATLAB to reduce the dimensionality of the spectral data; on the basis of a large number of experiments, the optimized principal component is extracted by using the principle of PLSR, which carries most of the original data information. Secondly, the linear regression analysis of the principal component is carried out with statistic package for social science (SPSS), which the coefficients and relations of principal components can be obtained. Finally, calculating a same water spectral data set by PLSR and improved PCR, analyzing and comparing two results, improved PCR and PLSR is similar for most data, but improved PCR is better than PLSR for data near the detection limit. Both PLSR and improved PCR can be used in Ultraviolet spectral analysis of water, but for data near the detection limit, improved PCR's result better than PLSR.

Anodic Stripping Voltammetry with Pencil Graphite Electrode for Determination of Chromium (III)

NASA Astrophysics Data System (ADS)

Wyantuti, S.; Hafidza, R. A.; Ishmayana, S.; Hartati, Y. W.

2017-02-01

Chromium is required as micronutrient that has roles in insulin metabolism and blood glucose level regulation. Chromium (III) deficiency can cause hyperglycemia and glycosuria. However, a high amount of chromium in body can cause allergic reaction, organ damage, and even death because of its toxicity. Chromium is commonly used in steel industries. Simultaneously with the development of industry, the waste disposal that can endanger environment also increased. Therefore, a sensitive and specific analysis method for chromium detection is required. Stripping voltammetry is one of the voltammetric methods that is commonly used for heavy metal analysis due to the very low limit of detection (sub ppb). The present study was conducted to develop an analysis method for chromium (III) determination using pencil graphite electrode. Quantitative determination was performed for chromium (III) which measured at -0.8 to +1.0 V with deposition time for 60 s and 50 mV/s scan rate. Stripping voltammetric analysis of chromium (III) using pencil graphite electrode gave linear range at 12.5 to 75 ppm with limit of detection of 0.31 ppm.

Enzymatic digestion and selective quantification of underivatised delta-9-tetrahydrocannabinol and cocaine in human hair using gas chromatography-mass spectrometry.

PubMed

Breidi, Salah Eddine; Barker, James; Petróczi, Andrea; Naughton, Declan P

2012-01-01

Gas chromatography-mass spectrometric (GC-MS) methods for drug analysis routinely employ derivatising reagents. The aim of this paper was to develop a method for the analysis of two recreational drugs, delta-9-tetrahydrocannabinol (Δ(9)-THC) and cocaine in hair samples using GC-MS, without prior derivatisation, thus allowing the sample to be reanalysed in its original form. An enzymatic digestion technique was also developed. Ten hair samples, that were known positive for either Δ(9)-THC and/or cocaine, were enzymatically digested, extracted, and then analysed by GC-MS. All samples measured contained Δ(9)-THC and one sample contained cocaine. The limits of detection (LOD) and quantification (LOQ) were 0.02 ng/mg and 0.05 ng/mg, respectively, for cocaine and 0.015 ng/mg and 0.02 ng/mg, respectively, for Δ(9)-THC. The wide detection window, ease of direct analysis by GC-MS, lower detection limits of underivatised samples, and the stability of drugs using this technique may offer an improved method of analysis.

Enzymatic Digestion and Selective Quantification of Underivatised Delta-9-Tetrahydrocannabinol and Cocaine in Human Hair Using Gas Chromatography-Mass Spectrometry

PubMed Central

Breidi, Salah Eddine; Barker, James; Petróczi, Andrea; Naughton, Declan P.

2012-01-01

Gas chromatography-mass spectrometric (GC-MS) methods for drug analysis routinely employ derivatising reagents. The aim of this paper was to develop a method for the analysis of two recreational drugs, delta-9-tetrahydrocannabinol (Δ9-THC) and cocaine in hair samples using GC-MS, without prior derivatisation, thus allowing the sample to be reanalysed in its original form. An enzymatic digestion technique was also developed. Ten hair samples, that were known positive for either Δ9-THC and/or cocaine, were enzymatically digested, extracted, and then analysed by GC-MS. All samples measured contained Δ9-THC and one sample contained cocaine. The limits of detection (LOD) and quantification (LOQ) were 0.02 ng/mg and 0.05 ng/mg, respectively, for cocaine and 0.015 ng/mg and 0.02 ng/mg, respectively, for Δ9-THC. The wide detection window, ease of direct analysis by GC-MS, lower detection limits of underivatised samples, and the stability of drugs using this technique may offer an improved method of analysis. PMID:22567573

Quantile regression for the statistical analysis of immunological data with many non-detects.

PubMed

Eilers, Paul H C; Röder, Esther; Savelkoul, Huub F J; van Wijk, Roy Gerth

2012-07-07

Immunological parameters are hard to measure. A well-known problem is the occurrence of values below the detection limit, the non-detects. Non-detects are a nuisance, because classical statistical analyses, like ANOVA and regression, cannot be applied. The more advanced statistical techniques currently available for the analysis of datasets with non-detects can only be used if a small percentage of the data are non-detects. Quantile regression, a generalization of percentiles to regression models, models the median or higher percentiles and tolerates very high numbers of non-detects. We present a non-technical introduction and illustrate it with an implementation to real data from a clinical trial. We show that by using quantile regression, groups can be compared and that meaningful linear trends can be computed, even if more than half of the data consists of non-detects. Quantile regression is a valuable addition to the statistical methods that can be used for the analysis of immunological datasets with non-detects.

Herbicide Orange Site Characterization Study Naval Construction Battalion Center

DTIC Science & Technology

1987-01-01

U.S. Testing Laboratories for analysis. Over 200 additional analyses were performed for a variety of quality assurance criteria. The resultant data...TABLE 9. NCBC PERFORMANCE AUDIT SAMPLE ANALYSIS SUNMARYa (SERIES 1) TCDD Sppb ) Reported Detection Relative b Sample Number Concentration Limit...limit rather than estimating the variance of the results. The sample results were transformed using the natural logarithm. The Shapiro-Wilk W test

Stripping analysis of nanomolar perchlorate in drinking water with a voltammetric ion-selective electrode based on thin-layer liquid membrane.

PubMed

Kim, Yushin; Amemiya, Shigeru

2008-08-01

A highly sensitive analytical method is required for the assessment of nanomolar perchlorate contamination in drinking water as an emerging environmental problem. We developed the novel approach based on a voltammetric ion-selective electrode to enable the electrochemical detection of "redox-inactive" perchlorate at a nanomolar level without its electrolysis. The perchlorate-selective electrode is based on the submicrometer-thick plasticized poly(vinyl chloride) membrane spin-coated on the poly(3-octylthiophene)-modified gold electrode. The liquid membrane serves as the first thin-layer cell for ion-transfer stripping voltammetry to give low detection limits of 0.2-0.5 nM perchlorate in deionized water, commercial bottled water, and tap water under a rotating electrode configuration. The detection limits are not only much lower than the action limit (approximately 246 nM) set by the U.S. Environmental Protection Agency but also are comparable to the detection limits of the most sensitive analytical methods for detecting perchlorate, that is, ion chromatography coupled with a suppressed conductivity detector (0.55 nM) or electrospray ionization mass spectrometry (0.20-0.25 nM). The mass transfer of perchlorate in the thin-layer liquid membrane and aqueous sample as well as its transfer at the interface between the two phases were studied experimentally and theoretically to achieve the low detection limits. The advantages of ion-transfer stripping voltammetry with a thin-layer liquid membrane against traditional ion-selective potentiometry are demonstrated in terms of a detection limit, a response time, and selectivity.

Methods for the preparation and analysis of solids and suspended solids for methylmercury

USGS Publications Warehouse

DeWild, John F.; Olund, Shane D.; Olson, Mark L.; Tate, Michael T.

2004-01-01

This report presents the methods and method performance data for the determination of methylmercury concentrations in solids and suspended solids. Using the methods outlined here, the U.S. Geological Survey's Wisconsin District Mercury Laboratory can consistently detect methylmercury in solids and suspended solids at environmentally relevant concentrations. Solids can be analyzed wet or freeze dried with a minimum detection limit of 0.08 ng/g (as-processed). Suspended solids must first be isolated from aqueous matrices by filtration. The minimum detection limit for suspended solids is 0.01 ng per filter resulting in a minimum reporting limit ranging from 0.2 ng/L for a 0.05 L filtered volume to 0.01 ng/L for a 1.0 L filtered volume. Maximum concentrations for both matrices can be extended to cover nearly any amount of methylmercury by limiting sample size.

Suspended Microchannel Resonators for Ultralow Volume Universal Detection

PubMed Central

Son, Sungmin; Grover, William H.; Burg, Thomas P.; Manalis, Scott R.

2008-01-01

Universal detectors that maintain high sensitivity as the detection volume is reduced to the subnanoliter scale can enhance the utility of miniaturized total analysis systems (μ-TAS). Here the unique scaling properties of the suspended microchannel resonator (SMR) are exploited to show universal detection in a 10 pL analysis volume with a density detection limit of ∼1 μg/cm3 (10 Hz bandwidth) and a dynamic range of 6 decades. Analytes with low UV extinction coefficients such as polyethylene glycol (PEG) 8 kDa, glucose, and glycine are measured with molar detection limits of 0.66, 13.5, and 31.6 μM, respectively. To demonstrate the potential for real-time monitoring, gel filtration chromatography was used to separate different molecular weights of PEG as the SMR acquired a chromatogram by measuring the eluate density. This work suggests that the SMR could offer a simple and sensitive universal detector for various separation systems from liquid chromatography to capillary electrophoresis. Moreover, since the SMR is itself a microfluidic channel, it can be directly integrated into μ-TAS without compromising overall performance. PMID:18489125

Reporter gene bioassays in environmental analysis.

PubMed

Köhler, S; Belkin, S; Schmid, R D

2000-01-01

In parallel to the continuous development of increasingly more sophisticated physical and chemical analytical technologies for the detection of environmental pollutants, there is a progressively more urgent need also for bioassays which report not only on the presence of a chemical but also on its bioavailability and its biological effects. As a partial fulfillment of that need, there has been a rapid development of biosensors based on genetically engineered bacteria. Such microorganisms typically combine a promoter-operator, which acts as the sensing element, with reporter gene(s) coding for easily detectable proteins. These sensors have the ability to detect global parameters such as stress conditions, toxicity or DNA-damaging agents as well as specific organic and inorganic compounds. The systems described in this review, designed to detect different groups of target chemicals, vary greatly in their detection limits, specificity, response times and more. These variations reflect on their potential applicability which, for most of the constructs described, is presently rather limited. Nevertheless, present trends promise that additional improvements will make microbial biosensors an important tool for future environmental analysis.

Eye movements during change detection: implications for search constraints, memory limitations, and scanning strategies.

PubMed

Zelinsky, G J

2001-02-01

Search, memory, and strategy constraints on change detection were analyzed in terms of oculomotor variables. Observers viewed a repeating sequence of three displays (Scene 1-->Mask-->Scene 2-->Mask...) and indicated the presence-absence of a changing object between Scenes 1 and 2. Scenes depicted real-world objects arranged on a surface. Manipulations included set size (one, three, or nine items) and the orientation of the changing objects (similar or different). Eye movements increased with the number of potentially changing objects in the scene, with this set size effect suggesting a relationship between change detection and search. A preferential fixation analysis determined that memory constraints are better described by the operation comparing the pre- and postchange objects than as a capacity limitation, and a scanpath analysis revealed a change detection strategy relying on the peripheral encoding and comparison of display items. These findings support a signal-in-noise interpretation of change detection in which the signal varies with the similarity of the changing objects and the noise is determined by the distractor objects and scene background.

A novel vacuum spectrometer for total reflection x-ray fluorescence analysis with two exchangeable low power x-ray sources for the analysis of low, medium, and high Z elements in sequence

NASA Astrophysics Data System (ADS)

Wobrauschek, P.; Prost, J.; Ingerle, D.; Kregsamer, P.; Misra, N. L.; Streli, C.

2015-08-01

The extension of the detectable elemental range with Total Reflection X-ray Fluorescence (TXRF) analysis is a challenging task. In this paper, it is demonstrated how a TXRF spectrometer is modified to analyze elements from carbon to uranium. Based on the existing design of a vacuum TXRF spectrometer with a 12 specimen sample changer, the following components were renewed: the silicon drift detector with 20 mm2 active area and having a special ultra-thin polymer window allowing the detection of elements from carbon upwards. Two exchangeable X-ray sources guarantee the efficient excitation of both low and high Z elements. These X-ray sources were two light-weighted easily mountable 35 W air-cooled low-power tubes with Cr and Rh anodes, respectively. The air cooled tubes and the Peltier-cooled detector allowed to construct a transportable tabletop spectrometer with compact dimensions, as neither liquid nitrogen cooling for the detector nor a water cooling circuit and a bulky high voltage generator for the X-ray tubes are required. Due to the excellent background conditions as a result of the TXRF geometry, detection limits of 150 ng for C, 12 ng for F, and 3.3 ng for Na have been obtained using Cr excitation in vacuum. For Rh excitation, the detection limits of 90 pg could be achieved for Sr. Taking 10 to 20 μl of sample volume, extrapolated detection limits in the ng/g (ppb) range are resulting in terms of concentration.

Direct liquid chromatography method for the simultaneous quantification of hydroxytyrosol and tyrosol in red wines.

PubMed

Piñeiro, Zulema; Cantos-Villar, Emma; Palma, Miguel; Puertas, Belen

2011-11-09

A validated HPLC method with fluorescence detection for the simultaneous quantification of hydroxytyrosol and tyrosol in red wines is described. Detection conditions for both compounds were optimized (excitation at 279 and 278 and emission at 631 and 598 nm for hydroxytyrosol and tyrosol, respectively). The validation of the analytical method was based on selectivity, linearity, robustness, detection and quantification limits, repeatability, and recovery. The detection and quantification limits in red wines were set at 0.023 and 0.076 mg L(-1) for hydroxytyrosol and at 0.007 and 0.024 mg L(-1) for tyrosol determination, respectively. Precision values, both within-day and between-day (n = 5), remained below 3% for both compounds. In addition, a fractional factorial experimental design was developed to analyze the influence of six different conditions on analysis. The final optimized HPLC-fluorescence method allowed the analysis of 30 nonpretreated Spanish red wines to evaluate their hydroxytyrosol and tyrosol contents.

Trace detection of oxygen--ionic liquids in gas sensor design.

PubMed

Baltes, N; Beyle, F; Freiner, S; Geier, F; Joos, M; Pinkwart, K; Rabenecker, P

2013-11-15

This paper presents a novel electrochemical membrane sensor on basis of ionic liquids for trace analysis of oxygen in gaseous atmospheres. The faradaic response currents for the reduction of oxygen which were obtained by multiple-potential-step-chronoamperometry could be used for real time detection of oxygen down to concentrations of 30 ppm. The theoretical limit of detection was 5 ppm. The simple, non-expensive sensors varied in electrolyte composition and demonstrated a high sensitivity, a rapid response time and an excellent reproducibility at room temperature. Some of them were continuously used for at least one week and first results promise good long term stability. Voltammetric, impedance and oxygen detection studies at temperatures up to 200 °C (in the presence and absence of humidity and CO2) revealed also the limitations of certain ionic liquids for some electrochemical high temperature applications. Application areas of the developed sensors are control and analysis processes of non oxidative and oxygen free atmospheres. Copyright © 2013 Elsevier B.V. All rights reserved.

Improved detection limits for electrospray ionization on a magnetic sector mass spectrometer by using an array detector.

PubMed

Cody, R B; Tamura, J; Finch, J W; Musselman, B D

1994-03-01

Array detection was compared with point detection for solutions of hen egg-white lysozyme, equine myoglobin, and ubiquitin analyzed by electrospray ionization with a magnetic sector mass spectrometer. The detection limits for samples analyzed by using the array detector system were at least 10 times lower than could be achieved by using a point detector on the same mass spectrometer. The minimum detectable quantity of protein corresponded to a signal-to-background ratio of approximately 2∶1 for a 500 amol/μL solution of hen egg-white lysozyme. However, the ultimate practical sample concentrations appeared to be in the 10-100 fmol/μL range for the analysis of dilute solutions of relatively pure proteins or simple mixtures.

Deletion detection for diagnosis of Duchenne muscular dystrophy in the Japanese population--comparison between the polymerase chain reaction and the Southern blot analysis.

PubMed

Katayama, S; Takeshita, N; Yano, T; Ubagai, T; Qiu, X J; Katagiri, Y; Kubo, H; Hirakawa, S

1993-06-01

We compared the efficacy of the multiplex PCR with that of the cDNA analysis for detection of deletions of the DMD gene in the Japanese patients. Thirty males with DMD from 27 Japanese families were studied by the multiplex PCR, and 24 of them were also investigated by Southern blot analysis. We used five dystrophin cDNA probes for deletion analysis. A total of 19 regions were amplified by the PCR to detect deletions, 9 regions by the method of Chamberlain et al. and another 10 regions by the method of Beggs et al. Deletions were detected in 14 (52%) out of 27 DMD families by the PCR. Southern blot analysis detected deletions in 14 (64%) out of 22 families. Thirteen (93%) of the 14 DMD families with deletions detected by Southern blotting were also confirmed by the multiplex PCR. Provided care is taken in cases where the deletion is limited to a single exon, the multiplex PCR appears to be an efficient and useful alternative to conventional Southern blot analysis for detecting deletions during the prenatal and postnatal diagnosis of DMD.

Fast Detection of Copper Content in Rice by Laser-Induced Breakdown Spectroscopy with Uni- and Multivariate Analysis.

PubMed

Liu, Fei; Ye, Lanhan; Peng, Jiyu; Song, Kunlin; Shen, Tingting; Zhang, Chu; He, Yong

2018-02-27

Fast detection of heavy metals is very important for ensuring the quality and safety of crops. Laser-induced breakdown spectroscopy (LIBS), coupled with uni- and multivariate analysis, was applied for quantitative analysis of copper in three kinds of rice (Jiangsu rice, regular rice, and Simiao rice). For univariate analysis, three pre-processing methods were applied to reduce fluctuations, including background normalization, the internal standard method, and the standard normal variate (SNV). Linear regression models showed a strong correlation between spectral intensity and Cu content, with an R 2 more than 0.97. The limit of detection (LOD) was around 5 ppm, lower than the tolerance limit of copper in foods. For multivariate analysis, partial least squares regression (PLSR) showed its advantage in extracting effective information for prediction, and its sensitivity reached 1.95 ppm, while support vector machine regression (SVMR) performed better in both calibration and prediction sets, where R c 2 and R p 2 reached 0.9979 and 0.9879, respectively. This study showed that LIBS could be considered as a constructive tool for the quantification of copper contamination in rice.

Fast Detection of Copper Content in Rice by Laser-Induced Breakdown Spectroscopy with Uni- and Multivariate Analysis

PubMed Central

Ye, Lanhan; Song, Kunlin; Shen, Tingting

2018-01-01

Fast detection of heavy metals is very important for ensuring the quality and safety of crops. Laser-induced breakdown spectroscopy (LIBS), coupled with uni- and multivariate analysis, was applied for quantitative analysis of copper in three kinds of rice (Jiangsu rice, regular rice, and Simiao rice). For univariate analysis, three pre-processing methods were applied to reduce fluctuations, including background normalization, the internal standard method, and the standard normal variate (SNV). Linear regression models showed a strong correlation between spectral intensity and Cu content, with an R2 more than 0.97. The limit of detection (LOD) was around 5 ppm, lower than the tolerance limit of copper in foods. For multivariate analysis, partial least squares regression (PLSR) showed its advantage in extracting effective information for prediction, and its sensitivity reached 1.95 ppm, while support vector machine regression (SVMR) performed better in both calibration and prediction sets, where Rc2 and Rp2 reached 0.9979 and 0.9879, respectively. This study showed that LIBS could be considered as a constructive tool for the quantification of copper contamination in rice. PMID:29495445

Validation of a near infrared microscopy method for the detection of animal products in feedingstuffs: results of a collaborative study.

PubMed

Boix, A; Fernández Pierna, J A; von Holst, C; Baeten, V

2012-01-01

The performance characteristics of a near infrared microscopy (NIRM) method, when applied to the detection of animal products in feedingstuffs, were determined via a collaborative study. The method delivers qualitative results in terms of the presence or absence of animal particles in feed and differentiates animal from vegetable feed ingredients on the basis of the evaluation of near infrared spectra obtained from individual particles present in the sample. The specificity ranged from 86% to 100%. The limit of detection obtained on the analysis of the sediment fraction, prepared as for the European official method, was 0.1% processed animal proteins (PAPs) in feed, since all laboratories correctly identified the positive samples. This limit has to be increased up to 2% for the analysis of samples which are not sedimented. The required sensitivity for the official control is therefore achieved in the analysis of the sediment fraction of the samples where the method can be applied for the detection of the presence of animal meal. Criteria for the classification of samples, when fewer than five spectra are found, as being of animal origin needs to be set up in order to harmonise the approach taken by the laboratories when applying NIRM for the detection of the presence of animal meal in feed.

Comparision of ICP-OES and MP-AES in determing soil nutrients by Mechlich3 method

NASA Astrophysics Data System (ADS)

Tonutare, Tonu; Penu, Priit; Krebstein, Kadri; Rodima, Ako; Kolli, Raimo; Shanskiy, Merrit

2014-05-01

Accurate, routine testing of nutrients in soil samples is critical to understanding soil potential fertility. There are different factors which must be taken into account selecting the best analytical technique for soil laboratory analysis. Several techniques can provide adequate detection range for same analytical subject. In similar cases the choise of technique will depend on factors such as sample throughput, required infrastructure, ease of use, used chemicals and need for gas supply and operating costs. Mehlich 3 extraction method is widely used for the determination of the plant available nutrient elements contents in agricultural soils. For determination of Ca, K, and Mg from soil extract depending of laboratory ICP and AAS techniques are used, also flame photometry for K in some laboratories. For the determination of extracted P is used ICP or Vis spectrometry. The excellent sensitivity and wide working range for all extracted elements make ICP a nearly ideal method, so long as the sample throughput is big enough to justify the initial capital outlay. Other advantage of ICP techniques is the multiplex character (simultaneous acquisition of all wavelengths). Depending on element the detection limits are in range 0.1 - 1000 μg/L. For smaller laboratories with low sample throughput requirements the use of AAS is more common. Flame AAS is a fast, relatively cheap and easy technique for analysis of elements. The disadvantages of the method is single element analysis and use of flammable gas, like C2H2 and oxidation gas N2O for some elements. Detection limits of elements for AAS lays from 1 to 1000 μg/L. MP-AES offers a unique alternative to both, AAS and ICP-OES techniques with its detection power, speed of analysis. MP-AES is quite new, simple and relatively inexpensive multielemental technique, which is use self-sustained atmospheric pressure microwave plasma (MP) using nitrogen gas generated by nitrogen generator. Therefore not needs for argon and flammable (C2H2) gases, cylinder handling and the running costs of equipment are low. Detection limits of elements for MP-AES lays between the AAS and ICP ones. The objective of this study was to compare the results of soil analysis using two multielemental analytical methods - ICP-OES and MP-AES. In the experiment, different soil types with various texture, content of organic matter and pH were used. For the study soil samples of Albeluvisols, Leptosols, Cambisols, Regosols and Histosols were used . The plant available nutrients were estimated by Mehlich 3 extraction. The ICP-OES analysis were provided in the Estonian Agricultural Research Centre and MP-AES analysis in department of Soil Science and Agrochemistry at Estonian University of Life Sciences. The detection limits and limits of quantification of Ca, K, Mg and P in extracts are calculated and reported.

Development of duplex SYBR Green I-based real-time quantitative reverse-transcription PCR for detection and discrimination of grapevine viruses

USDA-ARS?s Scientific Manuscript database

A SYBR® Green-based real-time quantitative reverse transcription PCR (qRT-PCR) assay in combination with melt curve analysis (MCA) was developed for the detection of nine grapevine viruses. The detection limits for singleplex qRT-PCR for all nine grapevine viruses were determined to be in the range ...

Determination of glucose and uric acid with bienzyme colorimetry on microfluidic paper-based analysis devices.

PubMed

Chen, Xi; Chen, Jin; Wang, Fubin; Xiang, Xia; Luo, Ming; Ji, Xinghu; He, Zhike

2012-05-15

In this work, we first employ a drying method combining with the bienzyme colorimetric detection of glucose and uric acid on microfluidic paper-based analysis devices (μPADs). The channels of 3D μPADs are also designed by us to get better results. The color results are recorded by both Gel Documentation systems and a common camera. By using Gel Documentation systems, the limits of detection (LOD) of glucose and uric acid are 3.81 × 10(-5)M and 4.31 × 10(-5)M, respectively one order of magnitude lower than that of the reported methods on μPADs. By using a common camera, the limits of detection (LOD) of glucose and uric acid are 2.13 × 10(-4)M and 2.87 × 10(-4)M, respectively. Furthermore, the effects of detection conditions have been investigated and discussed comprehensively. Human serum samples are detected with satisfactory results, which are comparable with the clinical testing results. A low-cost, simple and rapid colorimetric method for the simultaneous detection of glucose and uric acid on the μPADs has been developed with enhanced sensitivity. Copyright © 2012 Elsevier B.V. All rights reserved.

Electro-optical system for gunshot detection: analysis, concept, and performance

NASA Astrophysics Data System (ADS)

Kastek, M.; Dulski, R.; Madura, H.; Trzaskawka, P.; Bieszczad, G.; Sosnowski, T.

2011-08-01

The paper discusses technical possibilities to build an effective electro-optical sensor unit for sniper detection using infrared cameras. This unit, comprising of thermal and daylight cameras, can operate as a standalone device but its primary application is a multi-sensor sniper and shot detection system. At first, the analysis was presented of three distinguished phases of sniper activity: before, during and after the shot. On the basis of experimental data the parameters defining the relevant sniper signatures were determined which are essential in assessing the capability of infrared camera to detect sniper activity. A sniper body and muzzle flash were analyzed as targets and the descriptions of phenomena which make it possible to detect sniper activities in infrared spectra as well as analysis of physical limitations were performed. The analyzed infrared systems were simulated using NVTherm software. The calculations for several cameras, equipped with different lenses and detector types were performed. The simulation of detection ranges was performed for the selected scenarios of sniper detection tasks. After the analysis of simulation results, the technical specifications of infrared sniper detection system were discussed, required to provide assumed detection range. Finally the infrared camera setup was proposed which can detected sniper from 1000 meters range.

Multispecies breath analysis faster than a single respiratory cycle by optical-feedback cavity-enhanced absorption spectroscopy

NASA Astrophysics Data System (ADS)

Ventrillard-Courtillot, Irene; Gonthiez, Thierry; Clerici, Christine; Romanini, Daniel

2009-11-01

We demonstrate a first application, of optical-feedback cavity-enhanced absorption spectroscopy (OF-CEAS) to breath analysis in a medical environment. Noninvasive monitoring of trace species in exhaled air was performed simultaneous to spirometric measurements on patients at Bichat Hospital (Paris). The high selectivity of the OF-CEAS spectrometer and a time response of 0.3 s (limited by sample flow rate) allowed following the evolution of carbon monoxide and methane concentrations during individual respiratory cycles, and resolving variations among different ventilatory patterns. The minimum detectable absorption on this time scale is about 3×10-10 cm-1. At the working wavelength of the instrument (2.326 μm), this translates to concentration detection limits of ~1 ppbv (45 picomolar, or ~1.25 μg/m3) for CO and 25 ppbv for CH4, well below concentration values found in exhaled air. This same instrument is also able to provide measurement of NH3 concentrations with a detection limit of ~10 ppbv however, at present, memory effects do not allow its measurement on fast time scales.

Indirect Detection Analysis: Wino Dark Matter Case Study

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

Hryczuk, Andrzej; Cholis, Ilias; Iengo, Roberto

2014-07-15

We perform a multichannel analysis of the indirect signals for the Wino Dark Matter, including one-loop electroweak and Sommerfeld enhancement corrections. We derive limits from cosmic ray antiprotons and positrons, from continuum galactic and extragalactic diffuse γ-ray spectra, from the absence of γ-ray line features at the galactic center above 500 GeV in energy, from γ-rays toward nearby dwarf spheroidal galaxies and galaxy clusters, and from CMB power-spectra. Additionally, we show the future prospects for neutrino observations toward the inner Galaxy and from antideuteron searches. For each of these indirect detection probes we include and discuss the relevance of themore » most important astrophysical uncertainties that can impact the strength of the derived limits. We find that the Wino as a dark matter candidate is excluded in the mass range bellow simeq 800 GeV from antiprotons and between 1.8 and 3.5 TeV from the absence of a γ-ray line feature toward the galactic center. Limits from other indirect detection probes confirm the main bulk of the excluded mass ranges.« less

Investigation of detection limits for solutes in water measured by laser raman spectrometry

USGS Publications Warehouse

Goldberg, M.C.

1977-01-01

The influence of experimental parameters on detection sensitivity was determined for laser Raman analysis of dissolved solutes in water. Individual solutions of nitrate, sulfate, carbonate, bicarbonate, monohydrogen phosphate, dihydrogen phosphate, acetate ion, and acetic acid were measured. An equation is derived which expresses the signal-to-noise ratio in terms of solute concentration, measurement time, spectral slit width, laser power fluctuations, and solvent background intensity. Laser beam intensity fluctuations at the sample and solvent background intensity are the most important limiting factors.

Integrated on-chip derivatization and electrophoresis for the rapid analysis of biogenic amines.

PubMed

Beard, Nigel P; Edel, Joshua B; deMello, Andrew J

2004-07-01

We demonstrate the monolithic integration of a chemical reactor with a capillary electrophoresis device for the rapid and sensitive analysis of biogenic amines. Fluorescein isothiocyanate (FITC) is widely employed for the analysis of amino-group containing analytes. However, the slow reaction kinetics hinders the use of this dye for on-chip labeling applications. Other alternatives are available such as o-phthaldehyde (OPA), however, the inferior photophysical properties and the UV lambdamax present difficulties when using common excitation sources leading to a disparity in sensitivity. Consequently, we present for the first time the use of dichlorotriazine fluorescein (DTAF) as a superior in situ derivatizing agent for biogenic amines in microfluidic devices. The developed microdevice employs both hydrodynamic and electroosmotic flow, facilitating the creation of a polymeric microchip to perform both precolumn derivatization and electrophoretic analysis. The favorable photophysical properties of the DTAF and its fast reaction kinetics provide detection limits down to 1 nM and total analysis times (including on-chip mixing and reaction) of <60 s. The detection limits are two orders of magnitude lower than current limits obtained with both FITC and OPA. The optimized microdevice is also employed to probe biogenic amines in real samples.

Approaching the Limit in Atomic Spectrochemical Analysis.

ERIC Educational Resources Information Center

Hieftje, Gary M.

1982-01-01

To assess the ability of current analytical methods to approach the single-atom detection level, theoretical and experimentally determined detection levels are presented for several chemical elements. A comparison of these methods shows that the most sensitive atomic spectrochemical technique currently available is based on emission from…

Analysis of Endocrine Disrupting Pesticides by Capillary GC with Mass Spectrometric Detection

PubMed Central

Matisová, Eva; Hrouzková, Svetlana

2012-01-01

Endocrine disrupting chemicals, among them many pesticides, alter the normal functioning of the endocrine system of both wildlife and humans at very low concentration levels. Therefore, the importance of method development for their analysis in food and the environment is increasing. This also covers contributions in the field of ultra-trace analysis of multicomponent mixtures of organic pollutants in complex matrices. With this fact conventional capillary gas chromatography (CGC) and fast CGC with mass spectrometric detection (MS) has acquired a real importance in the analysis of endocrine disrupting pesticide (EDP) residues. This paper provides an overview of GC methods, including sample preparation steps, for analysis of EDPs in a variety of matrices at ultra-trace concentration levels. Emphasis is put on separation method, mode of MS detection and ionization and obtained limits of detection and quantification. Analysis time is one of the most important aspects that should be considered in the choice of analytical methods for routine analysis. Therefore, the benefits of developed fast GC methods are important. PMID:23202677

Comparison of Analysis and Quantification of Cell Death in vivo and in vitro

DTIC Science & Technology

1985-05-01

mammalian somatic cells appear to have a finite life span that is genetically programmed ( Hayflick , 1977). Following the consummation of this program... limited situations it is possible to evaluate the proliferation kinetics of cell populations in tis- sues by autoradiographically detecting radiolabeled...are, therefore, virtually limited to the analysis of toxicity of directly active chemicals. Primary cultures of target cells retain the ability to

Analysis of Eddy Current Capabilities for the Detection of Outer Diameter Stress Corrosion Cracking in Small Bore Metallic Structures

NASA Technical Reports Server (NTRS)

Wincheski, Buzz; Williams, Phillip; Simpson, John

2007-01-01

The use of eddy current techniques for the detection of outer diameter damage in tubing and many complex aerospace structures often requires the use of an inner diameter probe due to a lack of access to the outside of the part. In small bore structures the probe size and orientation are constrained by the inner diameter of the part, complicating the optimization of the inspection technique. Detection of flaws through a significant remaining wall thickness becomes limited not only by the standard depth of penetration, but also geometrical aspects of the probe. Recently, an orthogonal eddy current probe was developed for detection of such flaws in Space Shuttle Primary Reaction Control System (PRCS) Thrusters. In this case, the detection of deeply buried stress corrosion cracking by an inner diameter eddy current probe was sought. Probe optimization was performed based upon the limiting spatial dimensions, flaw orientation, and required detection sensitivity. Analysis of the probe/flaw interaction was performed through the use of finite and boundary element modeling techniques. Experimental data for the flaw detection capabilities, including a probability of detection study, will be presented along with the simulation data. The results of this work have led to the successful deployment of an inspection system for the detection of stress corrosion cracking in Space Shuttle Primary Reaction Control System (PRCS) Thrusters.

Detection limits of organic compounds achievable with intense, short-pulse lasers.

PubMed

Miles, Jordan; De Camillis, Simone; Alexander, Grace; Hamilton, Kathryn; Kelly, Thomas J; Costello, John T; Zepf, Matthew; Williams, Ian D; Greenwood, Jason B

2015-06-21

Many organic molecules have strong absorption bands which can be accessed by ultraviolet short pulse lasers to produce efficient ionization. This resonant multiphoton ionization scheme has already been exploited as an ionization source in time-of-flight mass spectrometers used for environmental trace analysis. In the present work we quantify the ultimate potential of this technique by measuring absolute ion yields produced from the interaction of 267 nm femtosecond laser pulses with the organic molecules indole and toluene, and gases Xe, N2 and O2. Using multiphoton ionization cross sections extracted from these results, we show that the laser pulse parameters required for real-time detection of aromatic molecules at concentrations of one part per trillion in air and a limit of detection of a few attomoles are achievable with presently available commercial laser systems. The potential applications for the analysis of human breath, blood and tissue samples are discussed.

Global limits and interference patterns in dark matter direct detection

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

Catena, Riccardo; Gondolo, Paolo

2015-08-13

We compare the general effective theory of one-body dark matter nucleon interactions to current direct detection experiments in a global multidimensional statistical analysis. We derive exclusion limits on the 28 isoscalar and isovector coupling constants of the theory, and show that current data place interesting constraints on dark matter-nucleon interaction operators usually neglected in this context. We characterize the interference patterns that can arise in dark matter direct detection from pairs of dark matter-nucleon interaction operators, or from isoscalar and isovector components of the same operator. We find that commonly neglected destructive interference effects weaken standard direct detection exclusion limitsmore » by up to one order of magnitude in the coupling constants.« less

Global limits and interference patterns in dark matter direct detection

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

Catena, Riccardo; Gondolo, Paolo, E-mail: riccardo.catena@theorie.physik.uni-goettingen.de, E-mail: paolo.gondolo@utah.edu

2015-08-01

We compare the general effective theory of one-body dark matter nucleon interactions to current direct detection experiments in a global multidimensional statistical analysis. We derive exclusion limits on the 28 isoscalar and isovector coupling constants of the theory, and show that current data place interesting constraints on dark matter-nucleon interaction operators usually neglected in this context. We characterize the interference patterns that can arise in dark matter direct detection from pairs of dark matter-nucleon interaction operators, or from isoscalar and isovector components of the same operator. We find that commonly neglected destructive interference effects weaken standard direct detection exclusion limitsmore » by up to one order of magnitude in the coupling constants.« less

Laser fluorometric analysis of plants for uranium exploration

USGS Publications Warehouse

Harms, T.F.; Ward, F.N.; Erdman, J.A.

1981-01-01

A preliminary test of biogeochemical exploration for locating uranium occurrences in the Marfa Basin, Texas, was conducted in 1978. Only 6 of 74 plant samples (mostly catclaw mimosa, Mimosa biuncifera) contained uranium in amounts above the detection limit (0.4 ppm in the ash) of the conventional fluorometric method. The samples were then analyzed using a Scintrex UA-3 uranium analyzer* * Use of trade names in this paper is for descriptive purposes only and does not constitute endorsement by the U.S. Geological Survey. - an instrument designed for direct analysis of uranium in water, and which can be conveniently used in a mobile field laboratory. The detection limit for uranium in plant ash (0.05 ppm) by this method is almost an order of magnitude lower than with the fluorometric conventional method. Only 1 of the 74 samples contained uranium below the detection limit of the new method. Accuracy and precision were determined to be satisfactory. Samples of plants growing on mineralized soils and nonmineralized soils show a 15-fold difference in uranium content; whereas the soils themselves (analyzed by delayed neutron activation analysis) show only a 4-fold difference. The method involves acid digestion of ashed tissue, extraction of uranium into ethyl acetate, destruction of the ethyl acetate, dissolution of the residue in 0.005% nitric acid, and measurement. ?? 1981.

Exploring laser-induced breakdown spectroscopy for nuclear materials analysis and in-situ applications

NASA Astrophysics Data System (ADS)

Martin, Madhavi Z.; Allman, Steve; Brice, Deanne J.; Martin, Rodger C.; Andre, Nicolas O.

2012-08-01

Laser-induced breakdown spectroscopy (LIBS) has been used to determine the limits of detection of strontium (Sr) and cesium (Cs), common nuclear fission products. Additionally, detection limits were determined for cerium (Ce), often used as a surrogate for radioactive plutonium in laboratory studies. Results were obtained using a laboratory instrument with a Nd:YAG laser at fundamental wavelength of 1064 nm, frequency doubled to 532 nm with energy of 50 mJ/pulse. The data was compared for different concentrations of Sr and Ce dispersed in a CaCO3 (white) and carbon (black) matrix. We have addressed the sampling errors, limits of detection, reproducibility, and accuracy of measurements as they relate to multivariate analysis in pellets that were doped with the different elements at various concentrations. These results demonstrate that LIBS technique is inherently well suited for in situ analysis of nuclear materials in hot cells. Three key advantages are evident: (1) small samples (mg) can be evaluated; (2) nuclear materials can be analyzed with minimal sample preparation; and (3) samples can be remotely analyzed very rapidly (ms-seconds). Our studies also show that the methods can be made quantitative. Very robust multivariate models have been used to provide quantitative measurement and statistical evaluation of complex materials derived from our previous research on wood and soil samples.

LC/ESI-MS/MS method for quantification of 28 synthetic cannabinoids in neat oral fluid and its application to preliminary studies on their detection windows.

PubMed

Kneisel, Stefan; Speck, Michael; Moosmann, Bjoern; Corneillie, Todd M; Butlin, Nathaniel G; Auwärter, Volker

2013-05-01

Serum and urine samples are commonly used for the analysis of synthetic cannabinoids in biofluids; however, their utilization as analytical matrices for drug abstinence control features some substantial drawbacks. While for blood collection invasive sampling is inevitable, the urinary analysis of synthetic cannabinoids is limited by the lack of available reference standards of the respective major metabolites. Moreover, the long detectability of synthetic cannabinoids in both matrices hampers the identification of a recent synthetic cannabinoid use. This article describes the development, validation and application of an LC/ESI-MS/MS method for the quantification of 28 synthetic cannabinoids in neat oral fluid (OF) samples. OF samples were prepared by protein precipitation using ice-cold acetonitrile. Chromatographic separation was achieved by gradient elution on a Luna Phenyl Hexyl column (50 × 2 mm, 5 μm), while detection was carried out on a QTrap 4000 instrument in positive ionization mode. The limits of detection ranged from 0.02 to 0.40 ng/mL, whereas the lower limits of quantification ranged from 0.2 to 4.0 ng/mL. The method was applied to authentic samples collected during two preliminary studies in order to obtain insights into the general detectability and detection windows of synthetic cannabinoids in this matrix. The results indicate that synthetic cannabinoids are transferred from the blood stream into OF and vice versa only at a very low rate. Therefore, positive OF samples are due to contamination of the oral cavity during smoking. As these drug-contaminations could be detected up to approximately 2 days, neat oral fluid appears to be well suited for detection of a recent synthetic cannabinoid use.

Novel approaches in diagnosing tuberculosis

NASA Astrophysics Data System (ADS)

Kolk, Arend H. J.; Dang, Ngoc A.; Kuijper, Sjoukje; Gibson, Tim; Anthony, Richard; Claassens, Mareli M.; Kaal, Erwin; Janssen, Hans-Gerd

2011-06-01

The WHO declared tuberculosis (TB) a global emergency. An estimated 8-9 million new cases occur each year with 2-3 million deaths. Currently, TB is diagnosed mostly by chest-X ray and staining of the mycobacteria in sputum with a detection limit of 1x104 bacteria /ml. There is an urgent need for better diagnostic tools for TB especially for developing countries. We have validated the electronic nose from TD Technology for the detection of Mycobacterium tuberculosis by headspace analysis of 284 sputum samples from TB patients. We used linear discriminant function analysis resulting in a sensitivity of 75% a specificity of 67% and an accuracy of 69%. Further research is still required to improve the results by choosing more selective sensors and sampling techniques. We used a fast gas chromatography- mass spectrometry method (GC-MS). The automated procedure is based on the injection of sputum samples which are methylated inside the GC injector using thermally assisted hydrolysis and methylation (THM-GC-MS). Hexacosanoic acid in combination with tuberculostearic acid was found to be specific for the presence of M. tuberculosis. The detection limit was similar to microscopy. We found no false positives, all microscopy and culture positive samples were also found positive with the THM-GC-MS method. The detection of ribosomal RNA from the infecting organism offers great potential since rRNA molecules outnumber chromosomal DNA by a factor 1000. It thus may possible to detect the organism without amplification of the nucleic acids (NA). We used a capture and a tagged detector probe for the direct detection of M. tuberculosis in sputum. So far the detection limit is 1x106 bacteria / ml. Currently we are testing a Lab-On-A-Chip Interferometer detection system.

Drug detection in breath: non-invasive assessment of illicit or pharmaceutical drugs.

PubMed

Trefz, Phillip; Kamysek, Svend; Fuchs, Patricia; Sukul, Pritam; Schubert, Jochen K; Miekisch, Wolfram

2017-03-20

Breath analysis not only holds great potential for the development of new non-invasive diagnostic methods, but also for the identification and follow up of drug levels in breath. This is of interest for both, forensic and medical science. On the one hand, the detection of drugs of abuse in exhaled breath-similar to the well-known breath alcohol tests-would be highly desirable as an alternative to blood or urine analysis in situations such as police controls for drugged driving. The non-invasive detection of drugs and their metabolites is thus of great interest in forensic science, especially since marijuana is becoming legalized in certain parts of the US and the EU. The detection and monitoring of medical drugs in exhaled breath without the need of drawing blood samples on the other hand, is of high relevance in the clinical environment. This could facilitate a more precise medication and enable therapy control without any burden to the patient. Furthermore, it could be a step towards personalized medicine. This review gives an overview of the current state of drug detection in breath, including both volatile and non-volatile substances. The review is divided into two sections. The first section deals with qualitative detection of drugs (drugs of abuse), while the second is related to quantitative drug detection (medical drugs). Chances and limitations are discussed for both aspects. The detection of the intravenous anesthetic propofol is presented as a detailed example that demonstrates the potential, requirements, pitfalls and limitations of therapeutic drug monitoring by means of breath analysis.

Polymer microchip CE of proteins either off- or on-chip labeled with chameleon dye for simplified analysis.

PubMed

Yu, Ming; Wang, Hsiang-Yu; Woolley, Adam T

2009-12-01

Microchip CE of proteins labeled either off- or on-chip with the "chameleon" CE dye 503 using poly(methyl methacrylate) microchips is presented. A simple dynamic coating using the cationic surfactant CTAB prevented nonspecific adsorption of protein and dye to the channel walls. The labeling reactions for both off- and on-chip labeling proceeded at room temperature without requiring heating steps. In off-chip labeling, a 9 ng/mL concentration detection limit for BSA, corresponding to a approximately 7 fg (100 zmol) mass detection limit, was obtained. In on-chip tagging, the free dye and protein were placed in different reservoirs of the microchip, and an extra incubation step was not needed. A 1 microg/mL concentration detection limit for BSA, corresponding to a approximately 700 fg (10 amol) mass detection limit, was obtained from this protocol. The earlier elution time of the BSA peak in on-chip labeling resulted from fewer total labels on each protein molecule. Our on-chip labeling method is an important part of automation in miniaturized devices.

An adaptive confidence limit for periodic non-steady conditions fault detection

NASA Astrophysics Data System (ADS)

Wang, Tianzhen; Wu, Hao; Ni, Mengqi; Zhang, Milu; Dong, Jingjing; Benbouzid, Mohamed El Hachemi; Hu, Xiong

2016-05-01

System monitoring has become a major concern in batch process due to the fact that failure rate in non-steady conditions is much higher than in steady ones. A series of approaches based on PCA have already solved problems such as data dimensionality reduction, multivariable decorrelation, and processing non-changing signal. However, if the data follows non-Gaussian distribution or the variables contain some signal changes, the above approaches are not applicable. To deal with these concerns and to enhance performance in multiperiod data processing, this paper proposes a fault detection method using adaptive confidence limit (ACL) in periodic non-steady conditions. The proposed ACL method achieves four main enhancements: Longitudinal-Standardization could convert non-Gaussian sampling data to Gaussian ones; the multiperiod PCA algorithm could reduce dimensionality, remove correlation, and improve the monitoring accuracy; the adaptive confidence limit could detect faults under non-steady conditions; the fault sections determination procedure could select the appropriate parameter of the adaptive confidence limit. The achieved result analysis clearly shows that the proposed ACL method is superior to other fault detection approaches under periodic non-steady conditions.

Statistical analysis of water-quality data containing multiple detection limits: S-language software for regression on order statistics

USGS Publications Warehouse

Lee, L.; Helsel, D.

2005-01-01

Trace contaminants in water, including metals and organics, often are measured at sufficiently low concentrations to be reported only as values below the instrument detection limit. Interpretation of these "less thans" is complicated when multiple detection limits occur. Statistical methods for multiply censored, or multiple-detection limit, datasets have been developed for medical and industrial statistics, and can be employed to estimate summary statistics or model the distributions of trace-level environmental data. We describe S-language-based software tools that perform robust linear regression on order statistics (ROS). The ROS method has been evaluated as one of the most reliable procedures for developing summary statistics of multiply censored data. It is applicable to any dataset that has 0 to 80% of its values censored. These tools are a part of a software library, or add-on package, for the R environment for statistical computing. This library can be used to generate ROS models and associated summary statistics, plot modeled distributions, and predict exceedance probabilities of water-quality standards. ?? 2005 Elsevier Ltd. All rights reserved.

Detectability Thresholds and Optimal Algorithms for Community Structure in Dynamic Networks

NASA Astrophysics Data System (ADS)

Ghasemian, Amir; Zhang, Pan; Clauset, Aaron; Moore, Cristopher; Peel, Leto

2016-07-01

The detection of communities within a dynamic network is a common means for obtaining a coarse-grained view of a complex system and for investigating its underlying processes. While a number of methods have been proposed in the machine learning and physics literature, we lack a theoretical analysis of their strengths and weaknesses, or of the ultimate limits on when communities can be detected. Here, we study the fundamental limits of detecting community structure in dynamic networks. Specifically, we analyze the limits of detectability for a dynamic stochastic block model where nodes change their community memberships over time, but where edges are generated independently at each time step. Using the cavity method, we derive a precise detectability threshold as a function of the rate of change and the strength of the communities. Below this sharp threshold, we claim that no efficient algorithm can identify the communities better than chance. We then give two algorithms that are optimal in the sense that they succeed all the way down to this threshold. The first uses belief propagation, which gives asymptotically optimal accuracy, and the second is a fast spectral clustering algorithm, based on linearizing the belief propagation equations. These results extend our understanding of the limits of community detection in an important direction, and introduce new mathematical tools for similar extensions to networks with other types of auxiliary information.

Direct detection of light ''Ge-phobic'' exothermic dark matter

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

Gelmini, Graciela B.; Georgescu, Andreea; Huh, Ji-Haeng, E-mail: gelmini@physics.ucla.edu, E-mail: a.georgescu@physics.ucla.edu, E-mail: jhhuh@physics.ucla.edu

2014-07-01

We present comparisons of direct dark matter (DM) detection data for light WIMPs with exothermic scattering with nuclei (exoDM), both assuming the Standard Halo Model (SHM) and in a halo model–independent manner. Exothermic interactions favor light targets, thus reducing the importance of upper limits derived from xenon targets, the most restrictive of which is at present the LUX limit. In our SHM analysis the CDMS-II-Si and CoGeNT regions become allowed by these bounds, however the recent SuperCDMS limit rejects both regions for exoDM with isospin-conserving couplings. An isospin-violating coupling of the exoDM, in particular one with a neutron to protonmore » coupling ratio of -0.8 (which we call ''Ge-phobic''), maximally reduces the DM coupling to germanium and allows the CDMS-II-Si region to become compatible with all bounds. This is also clearly shown in our halo-independent analysis.« less

Analysis of eight glycols in serum using LC-ESI-MS-MS.

PubMed

Imbert, Laurent; Saussereau, Elodie; Lacroix, Christian

2014-01-01

A liquid chromatography coupled with electrospray tandem mass spectrometry method was developed for the analysis of ethylene glycol, diethylene glycol, triethylene glycol, 1,4-butanediol, 1,2-butanediol, 2,3-butanediol, 1,2-propanediol and 1,3-propanediol, in serum after a Schotten-Baumann derivatization by benzoyl chloride. Usual validation parameters were tested: linearity, repeatability and intermediate precision, limits of detection and quantification, carry over and ion suppression. Limits of detection were between 0.18 and 1.1 mg/L, and limits of quantification were between 0.4 and 2.3 mg/L. Separation of isomers was possible either chromatographically or by selecting specific multiple reaction monitoring transitions. This method could be a useful tool in case of suspected intoxication with antifreeze agents, solvents, dietary supplements or some medical drug compounds. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

A sensitive and innovative detection method for rapid C-reactive proteins analysis based on a micro-fluxgate sensor system

PubMed Central

Yang, Zhen; Zhi, Shaotao; Feng, Zhu; Lei, Chong; Zhou, Yong

2018-01-01

A sensitive and innovative assay system based on a micro-MEMS-fluxgate sensor and immunomagnetic beads-labels was developed for the rapid analysis of C-reactive proteins (CRP). The fluxgate sensor presented in this study was fabricated through standard micro-electro-mechanical system technology. A multi-loop magnetic core made of Fe-based amorphous ribbon was employed as the sensing element, and 3-D solenoid copper coils were used to control the sensing core. Antibody-conjugated immunomagnetic microbeads were strategically utilized as signal tags to label the CRP via the specific conjugation of CRP to polyclonal CRP antibodies. Separate Au film substrates were applied as immunoplatforms to immobilize CRP-beads labels through classical sandwich assays. Detection and quantification of the CRP at different concentrations were implemented by detecting the stray field of CRP labeled magnetic beads using the newly-developed micro-fluxgate sensor. The resulting system exhibited the required sensitivity, stability, reproducibility, and selectivity. A detection limit as low as 0.002 μg/mL CRP with a linearity range from 0.002 μg/mL to 10 μg/mL was achieved, and this suggested that the proposed biosystem possesses high sensitivity. In addition to the extremely low detection limit, the proposed method can be easily manipulated and possesses a quick response time. The response time of our sensor was less than 5 s, and the entire detection period for CRP analysis can be completed in less than 30 min using the current method. Given the detection performance and other advantages such as miniaturization, excellent stability and specificity, the proposed biosensor can be considered as a potential candidate for the rapid analysis of CRP, especially for point-of-care platforms. PMID:29601593

Analysis of synthetic and biological microparticles on several flow cytometric platforms

EPA Science Inventory

Microparticles (MPs) are membrane vesicles (0.1 to 1 urn) released from cells upon activation. The limit of detection ofmost standard flow cytometers is just below 1 urn. Recent advances enable detection of particles lower than 0.5 urn, Synthetic. beads are used to define size ra...

Immuno-analysis of microparticles: probing at the limits of detection

PubMed Central

Latham, Sharissa L.; Tiberti, Natalia; Gokoolparsadh, Naveena; Holdaway, Karen; Olivier Couraud, Pierre; Grau, Georges E. R.; Combes, Valery

2015-01-01

Microparticle (MP) research is clouded by debate regarding the accuracy and validity of flow cytometry (FCM) as an analytical methodology, as it is influenced by many variables including the pre-analytical conditions, instruments physical capabilities and detection parameters. This study utilises a simplistic in vitro system for generating MP, and through comparative analysis with immuno-electron microscopy (Immuno-EM) assesses the strengths and limitations of probe selection and high-sensitivity FCM. Of the markers examined, MP were most specifically labelled with phosphatidylserine ligands, annexin V and lactadherin, although only ~60% MP are PS positive. Whilst these two ligands detect comparable absolute MP numbers, they interact with the same population in distinct manners; annexin V binding is enhanced on TNF induced MP. CD105 and CD54 expression were, as expected, consistent and enhanced following TNF activation respectively. Their labelling however accounted for as few as 30–40% of MP. The greatest discrepancies between FCM and I-EM were observed in the population solely labelled for the surface antigen. These findings demonstrate that despite significant improvements in resolution, high-sensitivity FCM remains limited in detecting small-size MP expressing low antigen levels. This study highlights factors to consider when selecting endothelial MP probes, as well as interpreting and representing data. PMID:26553743

State of the art in hair analysis for detection of drug and alcohol abuse.

PubMed

Pragst, Fritz; Balikova, Marie A

2006-08-01

Hair differs from other materials used for toxicological analysis because of its unique ability to serve as a long-term storage of foreign substances with respect to the temporal appearance in blood. Over the last 20 years, hair testing has gained increasing attention and recognition for the retrospective investigation of chronic drug abuse as well as intentional or unintentional poisoning. In this paper, we review the physiological basics of hair growth, mechanisms of substance incorporation, analytical methods, result interpretation and practical applications of hair analysis for drugs and other organic substances. Improved chromatographic-mass spectrometric techniques with increased selectivity and sensitivity and new methods of sample preparation have improved detection limits from the ng/mg range to below pg/mg. These technical advances have substantially enhanced the ability to detect numerous drugs and other poisons in hair. For example, it was possible to detect previous administration of a single very low dose in drug-facilitated crimes. In addition to its potential application in large scale workplace drug testing and driving ability examination, hair analysis is also used for detection of gestational drug exposure, cases of criminal liability of drug addicts, diagnosis of chronic intoxication and in postmortem toxicology. Hair has only limited relevance in therapy compliance control. Fatty acid ethyl esters and ethyl glucuronide in hair have proven to be suitable markers for alcohol abuse. Hair analysis for drugs is, however, not a simple routine procedure and needs substantial guidelines throughout the testing process, i.e., from sample collection to results interpretation.

Analysis of Glutamate, GABA, Noradrenaline, Dopamine, Serotonin, and Metabolites Using Microbore UHPLC with Electrochemical Detection

PubMed Central

2013-01-01

The applicability of microbore ultrahigh performance liquid chromatography (UHPLC) with electrochemical detection for offline analysis of a number of well-known neurotransmitters in less than 10 μL microdialysis fractions is described. Two methods are presented for the analysis of monoamine or amino acid neurotransmitters, using the same UHPLC instrument. Speed of analysis of noradrenaline (NA), dopamine (DA), serotonin (5-HT), and the metabolites homovanillic acid (HVA), 5-hydroxyindole aceticacid (5-HIAA), and 3,4-dihydroxyphenylacetic acid (DOPAC) was predominated by the retention behavior of NA, the nonideal behavior of matrix components, and the loss in signal of 5-HT. This method was optimized to meet the requirements for detection sensitivity and minimizing the size of collected fractions, which determines temporal resolution in microdialysis. The amino acid neurotransmitters glutamate (Glu) and γ-aminobutyric acid (GABA) were analyzed after an automated derivatization procedure. Under optimized conditions, Glu was resolved from a number of early eluting system peaks, while the total runtime was decreased to 15 min by a 4-fold increase of the flow rate under UHPLC conditions. The detection limit for Glu and GABA was 10 nmol/L (15 fmol in 1.5 μL); the monoamine neurotransmitters had a detection limit between 32 and 83 pmol/L (0.16–0.42 fmol in 5 μL) in standard solutions. Using UHPLC, the analysis times varied from 15 min to less than 2 min depending on the complexity of the samples and the substances to be analyzed. PMID:23642417

Direct Detection Electron Energy-Loss Spectroscopy: A Method to Push the Limits of Resolution and Sensitivity.

PubMed

Hart, James L; Lang, Andrew C; Leff, Asher C; Longo, Paolo; Trevor, Colin; Twesten, Ray D; Taheri, Mitra L

2017-08-15

In many cases, electron counting with direct detection sensors offers improved resolution, lower noise, and higher pixel density compared to conventional, indirect detection sensors for electron microscopy applications. Direct detection technology has previously been utilized, with great success, for imaging and diffraction, but potential advantages for spectroscopy remain unexplored. Here we compare the performance of a direct detection sensor operated in counting mode and an indirect detection sensor (scintillator/fiber-optic/CCD) for electron energy-loss spectroscopy. Clear improvements in measured detective quantum efficiency and combined energy resolution/energy field-of-view are offered by counting mode direct detection, showing promise for efficient spectrum imaging, low-dose mapping of beam-sensitive specimens, trace element analysis, and time-resolved spectroscopy. Despite the limited counting rate imposed by the readout electronics, we show that both core-loss and low-loss spectral acquisition are practical. These developments will benefit biologists, chemists, physicists, and materials scientists alike.

Analysis of copy number variants by three detection algorithms and their association with body size in horses.

PubMed

Metzger, Julia; Philipp, Ute; Lopes, Maria Susana; da Camara Machado, Artur; Felicetti, Michela; Silvestrelli, Maurizio; Distl, Ottmar

2013-07-18

Copy number variants (CNVs) have been shown to play an important role in genetic diversity of mammals and in the development of many complex phenotypic traits. The aim of this study was to perform a standard comparative evaluation of CNVs in horses using three different CNV detection programs and to identify genomic regions associated with body size in horses. Analysis was performed using the Illumina Equine SNP50 genotyping beadchip for 854 horses. CNVs were detected by three different algorithms, CNVPartition, PennCNV and QuantiSNP. Comparative analysis revealed 50 CNVs that affected 153 different genes mainly involved in sensory perception, signal transduction and cellular components. Genome-wide association analysis for body size showed highly significant deleted regions on ECA1, ECA8 and ECA9. Homologous regions to the detected CNVs on ECA1 and ECA9 have also been shown to be correlated with human height. Comparative analysis of CNV detection algorithms was useful to increase the specificity of CNV detection but had certain limitations dependent on the detection tool. GWAS revealed genome-wide associated CNVs for body size in horses.

Fast and objective detection and analysis of structures in downhole images

NASA Astrophysics Data System (ADS)

Wedge, Daniel; Holden, Eun-Jung; Dentith, Mike; Spadaccini, Nick

2017-09-01

Downhole acoustic and optical televiewer images, and formation microimager (FMI) logs are important datasets for structural and geotechnical analyses for the mineral and petroleum industries. Within these data, dipping planar structures appear as sinusoids, often in incomplete form and in abundance. Their detection is a labour intensive and hence expensive task and as such is a significant bottleneck in data processing as companies may have hundreds of kilometres of logs to process each year. We present an image analysis system that harnesses the power of automated image analysis and provides an interactive user interface to support the analysis of televiewer images by users with different objectives. Our algorithm rapidly produces repeatable, objective results. We have embedded it in an interactive workflow to complement geologists' intuition and experience in interpreting data to improve efficiency and assist, rather than replace the geologist. The main contributions include a new image quality assessment technique for highlighting image areas most suited to automated structure detection and for detecting boundaries of geological zones, and a novel sinusoid detection algorithm for detecting and selecting sinusoids with given confidence levels. Further tools are provided to perform rapid analysis of and further detection of structures e.g. as limited to specific orientations.

Supporting secure programming in web applications through interactive static analysis.

PubMed

Zhu, Jun; Xie, Jing; Lipford, Heather Richter; Chu, Bill

2014-07-01

Many security incidents are caused by software developers' failure to adhere to secure programming practices. Static analysis tools have been used to detect software vulnerabilities. However, their wide usage by developers is limited by the special training required to write rules customized to application-specific logic. Our approach is interactive static analysis, to integrate static analysis into Integrated Development Environment (IDE) and provide in-situ secure programming support to help developers prevent vulnerabilities during code construction. No additional training is required nor are there any assumptions on ways programs are built. Our work is motivated in part by the observation that many vulnerabilities are introduced due to failure to practice secure programming by knowledgeable developers. We implemented a prototype interactive static analysis tool as a plug-in for Java in Eclipse. Our technical evaluation of our prototype detected multiple zero-day vulnerabilities in a large open source project. Our evaluations also suggest that false positives may be limited to a very small class of use cases.

Supporting secure programming in web applications through interactive static analysis

PubMed Central

Zhu, Jun; Xie, Jing; Lipford, Heather Richter; Chu, Bill

2013-01-01

Many security incidents are caused by software developers’ failure to adhere to secure programming practices. Static analysis tools have been used to detect software vulnerabilities. However, their wide usage by developers is limited by the special training required to write rules customized to application-specific logic. Our approach is interactive static analysis, to integrate static analysis into Integrated Development Environment (IDE) and provide in-situ secure programming support to help developers prevent vulnerabilities during code construction. No additional training is required nor are there any assumptions on ways programs are built. Our work is motivated in part by the observation that many vulnerabilities are introduced due to failure to practice secure programming by knowledgeable developers. We implemented a prototype interactive static analysis tool as a plug-in for Java in Eclipse. Our technical evaluation of our prototype detected multiple zero-day vulnerabilities in a large open source project. Our evaluations also suggest that false positives may be limited to a very small class of use cases. PMID:25685513

A fully battery-powered inexpensive spectrophotometric system for high-sensitivity point-of-care analysis on a microfluidic chip

PubMed Central

Dou, Maowei; Lopez, Juan; Rios, Misael; Garcia, Oscar; Xiao, Chuan; Eastman, Michael

2016-01-01

A cost-effective battery-powered spectrophotometric system (BASS) was developed for quantitative point-of-care (POC) analysis on a microfluidic chip. By using methylene blue as a model analyte, we first compared the performance of the BASS with a commercial spectrophotometric system, and further applied the BASS for loop-mediated isothermal amplification (LAMP) detection and subsequent quantitative nucleic acid analysis which exhibited a comparable limit of detection to that of Nanodrop. Compared to the commercial spectrophotometric system, our spectrophotometric system is lower-cost, consumes less reagents, and has a higher detection sensitivity. Most importantly, it does not rely on external power supplies. All these features make our spectrophotometric system highly suitable for a variety of POC analyses, such as field detection. PMID:27143408

ELISA for sulfonamides and its application for screening in water contamination.

PubMed

Shelver, Weilin L; Shappell, Nancy W; Franek, Milan; Rubio, Fernando R

2008-08-13

Two enzyme-linked immunosorbent assays (ELISAs) were tested for their suitability for detecting sulfonamides in wastewater from various stages in wastewater treatment plants (WWTPs), the river into which the wastewater is discharged, and two swine-rearing facilities. The sulfamethoxazole ELISA cross-reacts with several compounds, achieving detection limits of <0.04 microg/L for sulfamethoxazole (SMX), sulfamethoxypyridine, sulfachloropyridine, and sulfamethoxine, whereas the sulfamethazine (SMZ) ELISA is more compound specific, with a detection limit of <0.03 microg/L. Samples from various stages of wastewater purifications gave 0.6-3.1 microg/L by SMX-ELISA, whereas river samples were approximately 10-fold lower, ranging from below detection to 0.09 microg/L. Swine wastewater samples analyzed by the SMX-ELISA were either at or near detectable limits from one facility, whereas the other facility had concentrations of approximately 0.5 microg/L, although LC-MS/MS did not confirm the presence of SMX. Sulfamethazine ELISA detected no SMZ in either WWTP or river samples. In contrast, wastewater samples from swine facilities analyzed by SMZ-ELISA were found to contain approximately 30 microg/L [piglet (50-100 lb) wastewater] and approximately 7 microg/L (market-weight hog wastewater). Sulfamethazine ELISA analyses of wastewater from another swine facility found concentrations to be near or below detection limits. A solid phase extraction method was used to isolate and concentrate sulfonamides from water samples prior to LC-MS/MS multiresidue confirmatory analysis. The recoveries at 1 microg/L fortification ranged from 42 +/- 4% for SMZ to 88 +/- 4% for SMX ( n = 6). The ELISA results in the WWTPs were confirmed by LC-MS/MS, as sulfonamide multiresidue confirmatory analysis identified SMX, sulfapyridine, and sulfasalazine to be present in the wastewater. Sulfamethazine presence at one swine-rearing facility was also confirmed by LC-MS/MS, demonstrating the usefulness of the ELISA technique as a rapid and high-throughput screening method.

Covariance of lucky images: performance analysis

NASA Astrophysics Data System (ADS)

Cagigal, Manuel P.; Valle, Pedro J.; Cagigas, Miguel A.; Villó-Pérez, Isidro; Colodro-Conde, Carlos; Ginski, C.; Mugrauer, M.; Seeliger, M.

2017-01-01

The covariance of ground-based lucky images is a robust and easy-to-use algorithm that allows us to detect faint companions surrounding a host star. In this paper, we analyse the relevance of the number of processed frames, the frames' quality, the atmosphere conditions and the detection noise on the companion detectability. This analysis has been carried out using both experimental and computer-simulated imaging data. Although the technique allows us the detection of faint companions, the camera detection noise and the use of a limited number of frames reduce the minimum detectable companion intensity to around 1000 times fainter than that of the host star when placed at an angular distance corresponding to the few first Airy rings. The reachable contrast could be even larger when detecting companions with the assistance of an adaptive optics system.

Extractive electrospray ionization mass spectrometry toward in situ analysis without sample pretreatment.

PubMed

Li, Ming; Hu, Bin; Li, Jianqiang; Chen, Rong; Zhang, Xie; Chen, Huanwen

2009-09-15

A homemade novel nanoextractive electrospray ionization (nanoEESI) source has been characterized for in situ mass spectrometric analysis of ambient samples without sample pretreatment. The primary ions generated using a nanospray emitter interact with the neutral sample plume created by manually nebulizing liquid samples, allowing production of the analyte ions in the spatial cross section of the nanoEESI source. The performance of nanoEESI is experimentally investigated by coupling the nanoEESI source to a commercial LTQ mass spectrometer for rapid analysis of various ambient samples using positive/negative ion detection modes. Compounds of interest in actual samples such as aerosol drug preparations, beverages, milk suspensions, farmland water, and groundwater were unambiguously detected using tandem nanoEESI ion trap mass spectrometry. The limit of detection was low picogram per milliliter levels for the compounds tested. Acceptable relative standard deviation (RSD) values (5-10%) were obtained for direct measurement of analytes in complex matrixes, providing linear dynamic signal responses using manual sample introduction. A single sample analysis was completed within 1.2 s. Requiring no sheath gas for either primary ion production or neutral sample introduction, the nanoEESI has advantages including readiness for miniaturization and integration, simple maintenance, easy operation, and low cost. The experimental data demonstrate that the nanoEESI is a promising tool for high-throughput, sensitive, quantitative, in situ analysis of ambient complex samples, showing potential applications for in situ analysis in multiple disciplines including but not limited to pharmaceutical analysis, food quality control, pesticides residue detection, and homeland security.

A novel vacuum spectrometer for total reflection x-ray fluorescence analysis with two exchangeable low power x-ray sources for the analysis of low, medium, and high Z elements in sequence

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

Wobrauschek, P., E-mail: wobi@ati.ac.at; Prost, J.; Ingerle, D.

2015-08-15

The extension of the detectable elemental range with Total Reflection X-ray Fluorescence (TXRF) analysis is a challenging task. In this paper, it is demonstrated how a TXRF spectrometer is modified to analyze elements from carbon to uranium. Based on the existing design of a vacuum TXRF spectrometer with a 12 specimen sample changer, the following components were renewed: the silicon drift detector with 20 mm{sup 2} active area and having a special ultra-thin polymer window allowing the detection of elements from carbon upwards. Two exchangeable X-ray sources guarantee the efficient excitation of both low and high Z elements. These X-raymore » sources were two light-weighted easily mountable 35 W air-cooled low-power tubes with Cr and Rh anodes, respectively. The air cooled tubes and the Peltier-cooled detector allowed to construct a transportable tabletop spectrometer with compact dimensions, as neither liquid nitrogen cooling for the detector nor a water cooling circuit and a bulky high voltage generator for the X-ray tubes are required. Due to the excellent background conditions as a result of the TXRF geometry, detection limits of 150 ng for C, 12 ng for F, and 3.3 ng for Na have been obtained using Cr excitation in vacuum. For Rh excitation, the detection limits of 90 pg could be achieved for Sr. Taking 10 to 20 μl of sample volume, extrapolated detection limits in the ng/g (ppb) range are resulting in terms of concentration.« less

Optical detection of glyphosate in water

NASA Astrophysics Data System (ADS)

de Góes, R. E.; Possetti, G. R. C.; Muller, M.; Fabris, J. L.

2017-04-01

This work shows preliminary results of the detection of Glyphosate in water by using optical fiber spectroscopy. A colloid with citrate-caped silver nanoparticles was employed as substrate for the measurements. A cross analysis between optical absorption and inelastic scattering evidenced a controlled aggregation of the sample constituents, leading to the possibility of quantitative detection of the analyte. The estimate limit of detection for Glyphosate in water for the proposed sensing scheme was about 1.7 mg/L.

Development of binding assays in microfabricated picoliter vials: an assay for biotin.

PubMed

Grosvenor, A L; Feltus, A; Conover, R C; Daunert, S; Anderson, K W

2000-06-01

A homogeneous binding assay for the detection of biotin in picoliter vials was developed using the photoprotein aequorin as the label. The binding assay was based on the competition of free biotin with biotinylated aequorin (AEQ-biotin) for avidin. A sequential protocol was used, and modification of the assay to reduce the number of steps was examined. Results showed that detection limits on the order of 10(-14) mol of biotin were possible. Reducing the number of steps provided similar detection limits but only if the amount of avidin used was decreased. These binding assays based on picoliter volumes have potential applications in a variety of fields, including microanalysis and single-cell analysis, where the amount of sample is limited. In addition, these assays are suitable for the high-throughput screening of biopharmaceuticals.

Analysis of nuclear resonance fluorescence excitation measured with LaBr3(Ce) detectors near 2 MeV

NASA Astrophysics Data System (ADS)

Omer, Mohamed; Negm, Hani; Ohgaki, Hideaki; Daito, Izuru; Hayakawa, Takehito; Bakr, Mahmoud; Zen, Heishun; Hori, Toshitada; Kii, Toshiteru; Masuda, Kai; Hajima, Ryoichi; Shizuma, Toshiyuki; Toyokawa, Hiroyuki; Kikuzawa, Nobuhiro

2013-11-01

The performance of LaBr3(Ce) to measure nuclear resonance fluorescence (NRF) excitations is discussed in terms of limits of detection and in comparison with high-purity germanium (HPGe) detectors near the 2 MeV region where many NRF excitation levels from special nuclear materials are located. The NRF experiment was performed at the High Intensity γ-ray Source (HIγS) facility. The incident γ-rays, of 2.12 MeV energy, hit a B4C target to excite the 11B nuclei to the first excitation level. The statistical-sensitive non-linear peak clipping (SNIP) algorithm was implemented to eliminate the background and enhance the limits of detection for the spectra measured with LaBr3(Ce). Both detection and determination limits were deduced from the experimental data.

An integrated microfluidic analysis microsystems with bacterial capture enrichment and in-situ impedance detection

NASA Astrophysics Data System (ADS)

Liu, Hai-Tao; Wen, Zhi-Yu; Xu, Yi; Shang, Zheng-Guo; Peng, Jin-Lan; Tian, Peng

2017-09-01

In this paper, an integrated microfluidic analysis microsystems with bacterial capture enrichment and in-situ impedance detection was purposed based on microfluidic chips dielectrophoresis technique and electrochemical impedance detection principle. The microsystems include microfluidic chip, main control module, and drive and control module, and signal detection and processing modulet and result display unit. The main control module produce the work sequence of impedance detection system parts and achieve data communication functions, the drive and control circuit generate AC signal which amplitude and frequency adjustable, and it was applied on the foodborne pathogens impedance analysis microsystems to realize the capture enrichment and impedance detection. The signal detection and processing circuit translate the current signal into impendence of bacteria, and transfer to computer, the last detection result is displayed on the computer. The experiment sample was prepared by adding Escherichia coli standard sample into chicken sample solution, and the samples were tested on the dielectrophoresis chip capture enrichment and in-situ impedance detection microsystems with micro-array electrode microfluidic chips. The experiments show that the Escherichia coli detection limit of microsystems is 5 × 104 CFU/mL and the detection time is within 6 min in the optimization of voltage detection 10 V and detection frequency 500 KHz operating conditions. The integrated microfluidic analysis microsystems laid the solid foundation for rapid real-time in-situ detection of bacteria.

Organic chemical analysis on a microscopic scale using two-step laser desorption/laser ionization mass spectrometry

NASA Technical Reports Server (NTRS)

Kovalenko, L. J.; Philippoz, J.-M.; Bucenell, J. R.; Zenobi, R.; Zare, R. N.

1991-01-01

The distribution of PAHs in the Allende meteorite has been measured using two-step laser desorption and laser multiphoton-ionization mass spectrometry. This method enables in situ analysis (with a spatial resolution of 1 mm or better) of selected organic molecules. Results show that PAH concentrations are locally high compared to the average concentration found by analysis of pulverized samples, and are found primarily in the fine-grained matrix; no PAHs were detected in the interiors of individual chondrules at the detection limit (about 0.05 ppm).

Accuracy of urinary human papillomavirus testing for presence of cervical HPV: systematic review and meta-analysis

PubMed Central

Pathak, Neha; Dodds, Julie; Khan, Khalid

2014-01-01

Objective To determine the accuracy of testing for human papillomavirus (HPV) DNA in urine in detecting cervical HPV in sexually active women. Design Systematic review and meta-analysis. Data sources Searches of electronic databases from inception until December 2013, checks of reference lists, manual searches of recent issues of relevant journals, and contact with experts. Eligibility criteria Test accuracy studies in sexually active women that compared detection of urine HPV DNA with detection of cervical HPV DNA. Data extraction and synthesis Data relating to patient characteristics, study context, risk of bias, and test accuracy. 2×2 tables were constructed and synthesised by bivariate mixed effects meta-analysis. Results 16 articles reporting on 14 studies (1443 women) were eligible for meta-analysis. Most used commercial polymerase chain reaction methods on first void urine samples. Urine detection of any HPV had a pooled sensitivity of 87% (95% confidence interval 78% to 92%) and specificity of 94% (95% confidence interval 82% to 98%). Urine detection of high risk HPV had a pooled sensitivity of 77% (68% to 84%) and specificity of 88% (58% to 97%). Urine detection of HPV 16 and 18 had a pooled sensitivity of 73% (56% to 86%) and specificity of 98% (91% to 100%). Metaregression revealed an increase in sensitivity when urine samples were collected as first void compared with random or midstream (P=0.004). Limitations The major limitations of this review are the lack of a strictly uniform method for the detection of HPV in urine and the variation in accuracy between individual studies. Conclusions Testing urine for HPV seems to have good accuracy for the detection of cervical HPV, and testing first void urine samples is more accurate than random or midstream sampling. When cervical HPV detection is considered difficult in particular subgroups, urine testing should be regarded as an acceptable alternative. PMID:25232064

Optimization of data analysis for the in vivo neutron activation analysis of aluminum in bone.

PubMed

Mohseni, H K; Matysiak, W; Chettle, D R; Byun, S H; Priest, N; Atanackovic, J; Prestwich, W V

2016-10-01

An existing system at McMaster University has been used for the in vivo measurement of aluminum in human bone. Precise and detailed analysis approaches are necessary to determine the aluminum concentration because of the low levels of aluminum found in the bone and the challenges associated with its detection. Phantoms resembling the composition of the human hand with varying concentrations of aluminum were made for testing the system prior to the application to human studies. A spectral decomposition model and a photopeak fitting model involving the inverse-variance weighted mean and a time-dependent analysis were explored to analyze the results and determine the model with the best performance and lowest minimum detection limit. The results showed that the spectral decomposition and the photopeak fitting model with the inverse-variance weighted mean both provided better results compared to the other methods tested. The spectral decomposition method resulted in a marginally lower detection limit (5μg Al/g Ca) compared to the inverse-variance weighted mean (5.2μg Al/g Ca), rendering both equally applicable to human measurements. Copyright © 2016 Elsevier Ltd. All rights reserved.

Gas chromatography--inductively coupled plasma--time-of-flight mass spectrometry for the speciation analysis of organolead compounds in environmental water samples.

PubMed

Heisterkamp, M; Adams, F C

2001-07-01

The application of inductively coupled plasma--time-of-flight mass spectrometry for the speciation analysis of organolead compounds in environmental waters is described. Construction of the transfer line was achieved by means of a relatively simple and rapid coupling procedure. Derivatization of the ionic lead species was achieved by in-situ propylation with sodium tetrapropylborate; simultaneous extraction of the derivatized compounds in hexane was followed by separation and detection by capillary gas chromatography hyphenated to inductively coupled plasma-time-of-flight mass spectrometry. Detection limits for the different organolead species ranged from 10 to 15 fg (as Pb), corresponding to procedural detection limits between 50 and 75 ng L(-1), on the basis of a 50 mL snow sample, extraction with 200 microL hexane, and subsequent injection of 1 microL of the organic extract on to the column. The accuracy of the system was confirmed by additional analysis of the water samples by capillary gas chromatography coupled with microwave-induced plasma-atomic-emission spectrometry and the analysis of a standard reference material CRM 605 (road dust) with a certified content of trimethyllead.

Quantitative analysis of sitagliptin using the (19)F-NMR method: a universal technique for fluorinated compound detection.

PubMed

Zhang, Fen-Fen; Jiang, Meng-Hong; Sun, Lin-Lin; Zheng, Feng; Dong, Lei; Shah, Vishva; Shen, Wen-Bin; Ding, Ya

2015-01-07

To expand the application scope of nuclear magnetic resonance (NMR) technology in quantitative analysis of pharmaceutical ingredients, (19)F nuclear magnetic resonance ((19)F-NMR) spectroscopy has been employed as a simple, rapid, and reproducible approach for the detection of a fluorine-containing model drug, sitagliptin phosphate monohydrate (STG). ciprofloxacin (Cipro) has been used as the internal standard (IS). Influential factors, including the relaxation delay time (d1) and pulse angle, impacting the accuracy and precision of spectral data are systematically optimized. Method validation has been carried out in terms of precision and intermediate precision, linearity, limit of detection (LOD) and limit of quantification (LOQ), robustness, and stability. To validate the reliability and feasibility of the (19)F-NMR technology in quantitative analysis of pharmaceutical analytes, the assay result has been compared with that of (1)H-NMR. The statistical F-test and student t-test at 95% confidence level indicate that there is no significant difference between these two methods. Due to the advantages of (19)F-NMR, such as higher resolution and suitability for biological samples, it can be used as a universal technology for the quantitative analysis of other fluorine-containing pharmaceuticals and analytes.

SWAN - Detection of explosives by means of fast neutron activation analysis

NASA Astrophysics Data System (ADS)

Gierlik, M.; Borsuk, S.; Guzik, Z.; Iwanowska, J.; Kaźmierczak, Ł.; Korolczuk, S.; Kozłowski, T.; Krakowski, T.; Marcinkowski, R.; Swiderski, L.; Szeptycka, M.; Szewiński, J.; Urban, A.

2016-10-01

In this work we report on SWAN, the experimental, portable device for explosives detection. The device was created as part of the EU Structural Funds Project "Accelerators & Detectors" (POIG.01.01.02-14-012/08-00), with the goal to increase beneficiary's expertise and competencies in the field of neutron activation analysis. Previous experiences and budged limitations lead toward a less advanced design based on fast neutron interactions and unsophisticated data analysis with the emphasis on the latest gamma detection and spectrometry solutions. The final device has been designed as a portable, fast neutron activation analyzer, with the software optimized for detection of carbon, nitrogen and oxygen. SWAN's performance in the role of explosives detector is elaborated in this paper. We demonstrate that the unique features offered by neutron activation analysis might not be impressive enough when confronted with practical demands and expectations of a generic homeland security customer.

Liquid biopsy on chip: a paradigm shift towards the understanding of cancer metastasis.

PubMed

Tadimety, Amogha; Syed, Abeer; Nie, Yuan; Long, Christina R; Kready, Kasia M; Zhang, John X J

2017-01-23

This comprehensive review serves as a guide for developing scalable and robust liquid biopsies on chip for capture, detection, and analysis of circulating tumor cells (CTCs). Liquid biopsy, the detection of biomarkers from body fluids, has proven challenging because of CTC rarity and the heterogeneity of CTCs shed from tumors. The review starts with the underlying biological mechanisms that make liquid biopsy a challenge before moving into an evaluation of current technological progress. Then, a framework for evaluation of the technologies is presented with special attention to throughput, capture rate, and cell viability for analysis. Technologies for CTC capture, detection, and analysis will be evaluated based on these criteria, with a focus on current approaches, limitations and future directions. The paper provides a critical review for microchip developers as well as clinical investigators to build upon the existing progress towards the goal of designing CTC capture, detection, and analysis platforms.

European Pulsar Timing Array limits on continuous gravitational waves from individual supermassive black hole binaries

NASA Astrophysics Data System (ADS)

Babak, S.; Petiteau, A.; Sesana, A.; Brem, P.; Rosado, P. A.; Taylor, S. R.; Lassus, A.; Hessels, J. W. T.; Bassa, C. G.; Burgay, M.; Caballero, R. N.; Champion, D. J.; Cognard, I.; Desvignes, G.; Gair, J. R.; Guillemot, L.; Janssen, G. H.; Karuppusamy, R.; Kramer, M.; Lazarus, P.; Lee, K. J.; Lentati, L.; Liu, K.; Mingarelli, C. M. F.; Osłowski, S.; Perrodin, D.; Possenti, A.; Purver, M. B.; Sanidas, S.; Smits, R.; Stappers, B.; Theureau, G.; Tiburzi, C.; van Haasteren, R.; Vecchio, A.; Verbiest, J. P. W.

2016-01-01

We have searched for continuous gravitational wave (CGW) signals produced by individually resolvable, circular supermassive black hole binaries (SMBHBs) in the latest European Pulsar Timing Array (EPTA) data set, which consists of ultraprecise timing data on 41-ms pulsars. We develop frequentist and Bayesian detection algorithms to search both for monochromatic and frequency-evolving systems. None of the adopted algorithms show evidence for the presence of such a CGW signal, indicating that the data are best described by pulsar and radiometer noise only. Depending on the adopted detection algorithm, the 95 per cent upper limit on the sky-averaged strain amplitude lies in the range 6 × 10-15 < A < 1.5 × 10-14 at 5 nHz < f < 7 nHz. This limit varies by a factor of five, depending on the assumed source position and the most constraining limit is achieved towards the positions of the most sensitive pulsars in the timing array. The most robust upper limit - obtained via a full Bayesian analysis searching simultaneously over the signal and pulsar noise on the subset of ours six best pulsars - is A ≈ 10-14. These limits, the most stringent to date at f < 10 nHz, exclude the presence of sub-centiparsec binaries with chirp mass M_c>10^9 M_{⊙} out to a distance of about 25 Mpc, and with M_c>10^{10} M_{⊙} out to a distance of about 1Gpc (z ≈ 0.2). We show that state-of-the-art SMBHB population models predict <1 per cent probability of detecting a CGW with the current EPTA data set, consistent with the reported non-detection. We stress, however, that PTA limits on individual CGW have improved by almost an order of magnitude in the last five years. The continuing advances in pulsar timing data acquisition and analysis techniques will allow for strong astrophysical constraints on the population of nearby SMBHBs in the coming years.

Quantitative analysis of ginger components in commercial products using liquid chromatography with electrochemical array detection

PubMed Central

Shao, Xi; Lv, Lishuang; Parks, Tiffany; Wu, Hou; Ho, Chi-Tang; Sang, Shengmin

2010-01-01

For the first time, a sensitive reversed-phase HPLC electrochemical array method has been developed for the quantitative analysis of eight major ginger components ([6]-, [8]-, and [10]-gingerol, [6]-, [8]-, and [10]-shogaol, [6]-paradol, and [1]-dehydrogingerdione) in eleven ginger-containing commercial products. This method was valid with unrivaled sensitivity as low as 7.3 – 20.2 pg of limit of detection and a range of 14.5 to 40.4 pg of limit of quantification. Using this method, we quantified the levels of eight ginger components in eleven different commercial products. Our results found that both levels and ratios among the eight compounds vary greatly in commercial products. PMID:21090746

Extraction and determination of biogenic amines in fermented sausages and other meat products using reversed-phase-HPLC.

PubMed

Straub, B; Schollenberger, M; Kicherer, M; Luckas, B; Hammes, W P

1993-09-01

A convenient method is described for the analysis of biogenic amines (BA) by means of reversed-phase-HPLC. The method is characterized by multi-channel UV detection (diodearray), subsequent post-column derivatization with o-phthaldialdehyde and 3-mercaptopropionic acid, and fluorescence detection. For the analysis of meat products and especially fermented sausages an optimized perchloric acid extraction process was introduced to determine putrescine, cadaverine, histamine, tyramine and 2-phenylethylamine. BA recoveries from meat ranged between 96 and 113% with a detection limit for amines of 0.5 mg/kg.

Solid-phase extraction with the metal-organic framework MIL-101(Cr) combined with direct analysis in real time mass spectrometry for the fast analysis of triazine herbicides.

PubMed

Li, Xianjiang; Xing, Jiawei; Chang, Cuilan; Wang, Xin; Bai, Yu; Yan, Xiuping; Liu, Huwei

2014-06-01

MIL-101(Cr) is an excellent metal-organic framework with high surface area and nanoscale cavities, making it promising in solid-phase extraction. Herein, we used MIL-101(Cr) as a solid-phase extraction packing material combined with fast detection of direct analysis in real time mass spectrometry (DART-MS) for the analysis of triazine herbicides. After systematic optimization of the operation parameters, including the gas temperature of DART, the moving speed of the 1D platform, solvent for desorption, amount of MIL-101(Cr) extraction time, eluent volume and salt concentration, this method can realize the simultaneous detection of five kinds of triazine herbicides. The limits of detection were 0.1∼0.2 ng/mL and the linear ranges covered more than two orders of magnitude with the quantitation limits of 0.5∼1 ng/mL. Moreover, the developed method has been applied for the analysis of lake water samples and the recoveries for spiked analytes were in the range of 85∼110%. These results showed that solid-phase extraction with metal-organic frameworks is an efficient sample preparation approach for DART-MS analysis and could find more applications in environmental analysis. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Multiplexed Paper Analytical Device for Quantification of Metals using Distance-Based Detection

PubMed Central

Cate, David M.; Noblitt, Scott D.; Volckens, John; Henry, Charles S.

2015-01-01

Exposure to metal-containing aerosols has been linked with adverse health outcomes for almost every organ in the human body. Commercially available techniques for quantifying particulate metals are time-intensive, laborious, and expensive; often sample analysis exceeds $100. We report a simple technique, based upon a distance-based detection motif, for quantifying metal concentrations of Ni, Cu, and Fe in airborne particulate matter using microfluidic paper-based analytical devices. Paper substrates are used to create sensors that are self-contained, self-timing, and require only a drop of sample for operation. Unlike other colorimetric approaches in paper microfluidics that rely on optical instrumentation for analysis, with distance-based detection, analyte is quantified visually based on the distance of a colorimetric reaction, similar to reading temperature on a thermometer. To demonstrate the effectiveness of this approach, Ni, Cu, and Fe were measured individually in single-channel devices; detection limits as low as 0.1, 0.1, and 0.05 µg were reported for Ni, Cu, and Fe. Multiplexed analysis of all three metals was achieved with detection limits of 1, 5, and 1 µg for Ni, Cu, and Fe. We also extended the dynamic range for multi-analyte detection by printing concentration gradients of colorimetric reagents using an off the shelf inkjet printer. Analyte selectivity was demonstrated for common interferences. To demonstrate utility of the method, Ni, Cu, and Fe were measured from samples of certified welding fume; levels measured with paper sensors matched known values determined gravimetrically. PMID:26009988

Detection, Size, Measurement, and Structural Analysis Limits for the 2MASS, UKIDSS-LAS, and VISTA VIKING Surveys

NASA Astrophysics Data System (ADS)

Andrews, Stephen K.; Kelvin, Lee S.; Driver, Simon P.; Robotham, Aaron S. G.

2014-01-01

The 2MASS, UKIDSS-LAS, and VISTA VIKING surveys have all now observed the GAMA 9hr region in the Ks band. Here we compare the detection rates, photometry, basic size measurements, and single-component GALFIT structural measurements for a sample of 37 591 galaxies. We explore the sensitivity limits where the data agree for a variety of issues including: detection, star-galaxy separation, photometric measurements, size and ellipticity measurements, and Sérsic measurements. We find that 2MASS fails to detect at least 20% of the galaxy population within all magnitude bins, however for those that are detected we find photometry is robust (± 0.2 mag) to 14.7 AB mag and star-galaxy separation to 14.8 AB mag. For UKIDSS-LAS we find incompleteness starts to enter at a flux limit of 18.9 AB mag, star-galaxy separation is robust to 16.3 AB mag, and structural measurements are robust to 17.7 AB mag. VISTA VIKING data are complete to approximately 20.0 AB mag and structural measurements appear robust to 18.8 AB mag.

Integrating Oil Debris and Vibration Measurements for Intelligent Machine Health Monitoring. Degree awarded by Toledo Univ., May 2002

NASA Technical Reports Server (NTRS)

Dempsey, Paula J.

2003-01-01

A diagnostic tool for detecting damage to gears was developed. Two different measurement technologies, oil debris analysis and vibration were integrated into a health monitoring system for detecting surface fatigue pitting damage on gears. This integrated system showed improved detection and decision-making capabilities as compared to using individual measurement technologies. This diagnostic tool was developed and evaluated experimentally by collecting vibration and oil debris data from fatigue tests performed in the NASA Glenn Spur Gear Fatigue Rig. An oil debris sensor and the two vibration algorithms were adapted as the diagnostic tools. An inductance type oil debris sensor was selected for the oil analysis measurement technology. Gear damage data for this type of sensor was limited to data collected in the NASA Glenn test rigs. For this reason, this analysis included development of a parameter for detecting gear pitting damage using this type of sensor. The vibration data was used to calculate two previously available gear vibration diagnostic algorithms. The two vibration algorithms were selected based on their maturity and published success in detecting damage to gears. Oil debris and vibration features were then developed using fuzzy logic analysis techniques, then input into a multi sensor data fusion process. Results show combining the vibration and oil debris measurement technologies improves the detection of pitting damage on spur gears. As a result of this research, this new diagnostic tool has significantly improved detection of gear damage in the NASA Glenn Spur Gear Fatigue Rigs. This research also resulted in several other findings that will improve the development of future health monitoring systems. Oil debris analysis was found to be more reliable than vibration analysis for detecting pitting fatigue failure of gears and is capable of indicating damage progression. Also, some vibration algorithms are as sensitive to operational effects as they are to damage. Another finding was that clear threshold limits must be established for diagnostic tools. Based on additional experimental data obtained from the NASA Glenn Spiral Bevel Gear Fatigue Rig, the methodology developed in this study can be successfully implemented on other geared systems.

Step-scan T cell-based differential Fourier transform infrared photoacoustic spectroscopy (DFTIR-PAS) for detection of ambient air contaminants

NASA Astrophysics Data System (ADS)

Liu, Lixian; Mandelis, Andreas; Huan, Huiting; Melnikov, Alexander

2016-10-01

A step-scan differential Fourier transform infrared photoacoustic spectroscopy (DFTIR-PAS) using a commercial FTIR spectrometer was developed theoretically and experimentally for air contaminant monitoring. The configuration comprises two identical, small-size and low-resonance-frequency T cells satisfying the conflicting requirements of low chopping frequency and limited space in the sample compartment. Carbon dioxide (CO2) IR absorption spectra were used to demonstrate the capability of the DFTIR-PAS method to detect ambient pollutants. A linear amplitude response to CO2 concentrations from 100 to 10,000 ppmv was observed, leading to a theoretical detection limit of 2 ppmv. The differential mode was able to suppress the coherent noise, thereby imparting the DFTIR-PAS method with a better signal-to-noise ratio and lower theoretical detection limit than the single mode. The results indicate that it is possible to use step-scan DFTIR-PAS with T cells as a quantitative method for high sensitivity analysis of ambient contaminants.

Determination of acrylamide and methacrylamide by normal phase high performance liquid chromatography and UV detection.

PubMed

Paleologos, E K; Kontominas, M G

2005-06-10

A method using normal phase high performance liquid chromatography (NP-HPLC) with UV detection was developed for the analysis of acrylamide and methacrylamide. The method relies on the chromatographic separation of these analytes on a polar HPLC column designed for the separation of organic acids. Identification of acrylamide and methacrylamide is approached dually, that is directly in their protonated forms and as their hydrolysis products acrylic and methacrylic acid respectively, for confirmation. Detection and quantification is performed at 200 nm. The method is simple allowing for clear resolution of the target peaks from any interfering substances. Detection limits of 10 microg L(-1) were obtained for both analytes with the inter- and intra-day RSD for standard analysis lying below 1.0%. Use of acetonitrile in the elution solvent lowers detection limits and retention times, without impairing resolution of peaks. The method was applied for the determination of acrylamide and methacrylamide in spiked food samples without native acrylamide yielding recoveries between 95 and 103%. Finally, commercial samples of french and roasted fries, cookies, cocoa and coffee were analyzed to assess applicability of the method towards acrylamide, giving results similar with those reported in the literature.

Detection limits of quantitative and digital PCR assays and their influence in presence-absence surveys of environmental DNA

USGS Publications Warehouse

Hunter, Margaret; Dorazio, Robert M.; Butterfield, John S.; Meigs-Friend, Gaia; Nico, Leo; Ferrante, Jason A.

2017-01-01

A set of universal guidelines is needed to determine the limit of detection (LOD) in PCR-based analyses of low concentration DNA. In particular, environmental DNA (eDNA) studies require sensitive and reliable methods to detect rare and cryptic species through shed genetic material in environmental samples. Current strategies for assessing detection limits of eDNA are either too stringent or subjective, possibly resulting in biased estimates of species’ presence. Here, a conservative LOD analysis grounded in analytical chemistry is proposed to correct for overestimated DNA concentrations predominantly caused by the concentration plateau, a nonlinear relationship between expected and measured DNA concentrations. We have used statistical criteria to establish formal mathematical models for both quantitative and droplet digital PCR. To assess the method, a new Grass Carp (Ctenopharyngodon idella) TaqMan assay was developed and tested on both PCR platforms using eDNA in water samples. The LOD adjustment reduced Grass Carp occupancy and detection estimates while increasing uncertainty – indicating that caution needs to be applied to eDNA data without LOD correction. Compared to quantitative PCR, digital PCR had higher occurrence estimates due to increased sensitivity and dilution of inhibitors at low concentrations. Without accurate LOD correction, species occurrence and detection probabilities based on eDNA estimates are prone to a source of bias that cannot be reduced by an increase in sample size or PCR replicates. Other applications also could benefit from a standardized LOD such as GMO food analysis, and forensic and clinical diagnostics.

Applicability of direct total reflection X-ray fluorescence analysis for selenium determination in solutions related to environmental and geochemical studies

NASA Astrophysics Data System (ADS)

Marguí, E.; Floor, G. H.; Hidalgo, M.; Kregsamer, P.; Roman-Ross, G.; Streli, C.; Queralt, I.

2010-12-01

A significant amount of environmental studies related to selenium determination in different environmental compartments have been published in the last years due to the narrow range between the Se nutritious requirement as essential element and toxic effects upon exposure. However, the direct analysis of complex liquid samples like natural waters and extraction solutions presents significant problems related to the low Se concentrations and the complicated matrix of this type of samples. The goal of the present research was to study the applicability of direct TXRF analysis of different type of solutions commonly used in environmental and geochemical studies, confirm the absence or presence of matrix effects and evaluate the limits of detection and accuracy for Se determination in the different matrices. Good analytical results were obtained for the direct analysis of ground and rain water samples with limits of detection for Se two orders of magnitude lower than the permissible Se concentration in drinking waters ([Se] = 10 μg/L) according to the WHO. However, the Se detection limits for more complex liquid samples such as thermal waters and extraction solutions were in the μg/L range due to the presence of high contents of other elements present in the matrix (i.e., Br, Fe, Zn) or the high background of the TXRF spectrum that hamper the Se determination at trace levels. Our results give insight into the possibilities and drawbacks of direct TXRF analysis and to a certain extent the potential applications in the environmental and geochemical field.

Multiplex detection of pancreatic cancer biomarkers using a SERS-based immunoassay

NASA Astrophysics Data System (ADS)

Banaei, Nariman; Foley, Anne; Houghton, Jean Marie; Sun, Yubing; Kim, Byung

2017-11-01

Early diagnosis of pancreatic cancer (PC) is critical to reduce the mortality rate of this disease. Current biological analysis approaches cannot robustly detect several low abundance PC biomarkers in sera, limiting the clinical application of these biomarkers. Enzyme linked immunosorbent assay and radioimmunoassay are two common platforms for detection of biomarkers; however, they suffer from some limitation. This study demonstrates a novel system for multiplex detection of pancreatic biomarkers CA19-9, MMP7 and MUC4 in sera samples with high sensitivity using surface enhanced Raman spectroscopy. Measuring the levels of these biomarkers in PC patients, pancreatitis patients, and healthy individuals reveals the unique expression pattern of these markers in PC patients, suggesting the great potential of using this approach for early diagnostics of PCs.

Hyperspectral wide gap second derivative analysis for in vivo detection of cervical intraepithelial neoplasia

NASA Astrophysics Data System (ADS)

Zheng, Wenli; Wang, Chaojian; Chang, Shufang; Zhang, Shiwu; Xu, Ronald X.

2015-12-01

Hyperspectral reflectance imaging technique has been used for in vivo detection of cervical intraepithelial neoplasia. However, the clinical outcome of this technique is suboptimal owing to multiple limitations such as nonuniform illumination, high-cost and bulky setup, and time-consuming data acquisition and processing. To overcome these limitations, we acquired the hyperspectral data cube in a wavelength ranging from 600 to 800 nm and processed it by a wide gap second derivative analysis method. This method effectively reduced the image artifacts caused by nonuniform illumination and background absorption. Furthermore, with second derivative analysis, only three specific wavelengths (620, 696, and 772 nm) are needed for tissue classification with optimal separability. Clinical feasibility of the proposed image analysis and classification method was tested in a clinical trial where cervical hyperspectral images from three patients were used for classification analysis. Our proposed method successfully classified the cervix tissue into three categories of normal, inflammation and high-grade lesion. These classification results were coincident with those by an experienced gynecology oncologist after applying acetic acid. Our preliminary clinical study has demonstrated the technical feasibility for in vivo and noninvasive detection of cervical neoplasia without acetic acid. Further clinical research is needed in order to establish a large-scale diagnostic database and optimize the tissue classification technique.

Hyperspectral wide gap second derivative analysis for in vivo detection of cervical intraepithelial neoplasia.

PubMed

Zheng, Wenli; Wang, Chaojian; Chang, Shufang; Zhang, Shiwu; Xu, Ronald X

2015-12-01

Hyperspectral reflectance imaging technique has been used for in vivo detection of cervical intraepithelial neoplasia. However, the clinical outcome of this technique is suboptimal owing to multiple limitations such as nonuniform illumination, high-cost and bulky setup, and time-consuming data acquisition and processing. To overcome these limitations, we acquired the hyperspectral data cube in a wavelength ranging from 600 to 800 nm and processed it by a wide gap second derivative analysis method. This method effectively reduced the image artifacts caused by nonuniform illumination and background absorption. Furthermore, with second derivative analysis, only three specific wavelengths (620, 696, and 772 nm) are needed for tissue classification with optimal separability. Clinical feasibility of the proposed image analysis and classification method was tested in a clinical trial where cervical hyperspectral images from three patients were used for classification analysis. Our proposed method successfully classified the cervix tissue into three categories of normal, inflammation and high-grade lesion. These classification results were coincident with those by an experienced gynecology oncologist after applying acetic acid. Our preliminary clinical study has demonstrated the technical feasibility for in vivo and noninvasive detection of cervical neoplasia without acetic acid. Further clinical research is needed in order to establish a large-scale diagnostic database and optimize the tissue classification technique.

Comparative analysis of techniques for detection of quiescent Botrytis cinerea in grapes by quantitative PCR

USDA-ARS?s Scientific Manuscript database

Quantitative PCR (qPCR) can be used to detect and monitor pathogen colonization, but early attempts to apply the technology to quiescent Botrytis cinerea infections of grape berries identified some specific limitations. In this study, four DNA extraction methods, two tissue-grinding methods, two gra...

Detection of the Spermicide Nonoxynol-9 Via GC-MS

NASA Astrophysics Data System (ADS)

Musah, Rabi A.; Vuong, Angela L.; Henck, Colin; Shepard, Jason R. E.

2012-05-01

The spermicide nonoxynol-9 is actually a complex mixture of dozens of closely related amphiphilic compounds, and the chemical properties of this assortment significantly hamper its characterization by GC-MS. The inability to perform routine GC-MS testing on nonoxynol-9 has limited its evidentiary value in forensic casework, which relies heavily on this technique for analysis. A disturbing trend in sexual assault is the use of condoms by assailants, to avoid leaving behind DNA evidence that can connect a perpetrator to a victim. This observation necessitates the development of alternative methods for the analysis of trace evidence that can show causal links between a victim and a suspect. Detection of lubricants associated with sexual assault is one such way to establish this connection. The development of GC-MS methods that permit facile detection of both nonoxynol-9 alone and nonoxynol-9 extracted from other complex matrices that have potential as trace evidence in sexual assault is reported. A detection limit of 2.14 μg of nonoxynol-9 is demonstrated, and a detailed mass spectral profile that elaborates on what is known of its structure is provided.

Analysis and segmentation of images in case of solving problems of detecting and tracing objects on real-time video

NASA Astrophysics Data System (ADS)

Ezhova, Kseniia; Fedorenko, Dmitriy; Chuhlamov, Anton

2016-04-01

The article deals with the methods of image segmentation based on color space conversion, and allow the most efficient way to carry out the detection of a single color in a complex background and lighting, as well as detection of objects on a homogeneous background. The results of the analysis of segmentation algorithms of this type, the possibility of their implementation for creating software. The implemented algorithm is very time-consuming counting, making it a limited application for the analysis of the video, however, it allows us to solve the problem of analysis of objects in the image if there is no dictionary of images and knowledge bases, as well as the problem of choosing the optimal parameters of the frame quantization for video analysis.

Determination of the cyanobacterial toxin cylindrospermopsin in algal food supplements.

PubMed

Liu, H; Scott, P M

2011-06-01

For the analysis of blue-green algal food supplements for cylindrospermopsin (CYN), a C18 solid-phase extraction column and a polygraphitized carbon solid-phase extraction column in series was an effective procedure for the clean-up of extracts. Determination of CYN was by liquid chromatography with ultraviolet light detection. At extract spiking levels of CYN equivalent to 25-500 µg g(-1), blue-green algal supplement recoveries were in the range 70-90%. CYN was not detected in ten samples of food supplements and one chocolate product, all containing blue-green algae. The limit of detection for the method was 16 µg g(-1), and the limit of quantification was 52 µg g(-1).

Analyzing Responses of Chemical Sensor Arrays

NASA Technical Reports Server (NTRS)

Zhou, Hanying

2007-01-01

NASA is developing a third-generation electronic nose (ENose) capable of continuous monitoring of the International Space Station s cabin atmosphere for specific, harmful airborne contaminants. Previous generations of the ENose have been described in prior NASA Tech Briefs issues. Sensor selection is critical in both (prefabrication) sensor material selection and (post-fabrication) data analysis of the ENose, which detects several analytes that are difficult to detect, or that are at very low concentration ranges. Existing sensor selection approaches usually include limited statistical measures, where selectivity is more important but reliability and sensitivity are not of concern. When reliability and sensitivity can be major limiting factors in detecting target compounds reliably, the existing approach is not able to provide meaningful selection that will actually improve data analysis results. The approach and software reported here consider more statistical measures (factors) than existing approaches for a similar purpose. The result is a more balanced and robust sensor selection from a less than ideal sensor array. The software offers quick, flexible, optimal sensor selection and weighting for a variety of purposes without a time-consuming, iterative search by performing sensor calibrations to a known linear or nonlinear model, evaluating the individual sensor s statistics, scoring the individual sensor s overall performance, finding the best sensor array size to maximize class separation, finding optimal weights for the remaining sensor array, estimating limits of detection for the target compounds, evaluating fingerprint distance between group pairs, and finding the best event-detecting sensors.

Sensitive sub-Doppler nonlinear spectroscopy for hyperfine-structure analysis using simple atomizers

NASA Astrophysics Data System (ADS)

Mickadeit, Fritz K.; Kemp, Helen; Schafer, Julia; Tong, William M.

1998-05-01

Laser wave-mixing spectroscopy is presented as a sub-Doppler method that offers not only high spectral resolution, but also excellent detection sensitivity. It offers spectral resolution suitable for hyperfine structure analysis and isotope ratio measurements. In a non-planar backward- scattering four-wave mixing optical configuration, two of the three input beams counter propagate and the Doppler broadening is minimized, and hence, spectral resolution is enhanced. Since the signal is a coherent beam, optical collection is efficient and signal detection is convenient. This simple multi-photon nonlinear laser method offers un usually sensitive detection limits that are suitable for trace-concentration isotope analysis using a few different types of simple analytical atomizers. Reliable measurement of hyperfine structures allows effective determination of isotope ratios for chemical analysis.

Online detection and quantification of ergot bodies in cereals using near infrared hyperspectral imaging.

PubMed

Vermeulen, Ph; Pierna, J A Fernández; Egmond, H P van; Dardenne, P; Baeten, V

2012-01-01

The occurrence of ergot bodies (sclerotia of Claviceps purpurea) in cereals presents a high toxicity risk for animals and humans due to the alkaloid content. To reduce this risk, the European Commission fixed an ergot concentration limit of 0.1% in all feedstuffs containing unground cereals, and a limit of 0.05% in 'intervention' cereals destined for humans. This study sought to develop a procedure based on near infrared hyperspectral imaging and multivariate image analysis to detect and quantify ergot contamination in cereals. Hyperspectral images were collected using an NIR hyperspectral line scan combined with a conveyor belt. All images consisted of lines of 320 pixels that were acquired at 209 wavelength channels (1100-2400 nm). To test the procedure, several wheat samples with different levels of ergot contamination were prepared. The results showed a correlation higher than 0.99 between the predicted values obtained using chemometric tools such as partial least squares discriminant analysis or support vector machine and the reference values. For a wheat sample with a level of ergot contamination as low as 0.01 %, it was possible to identify groups of pixels detected as ergot to conclude that the sample was contaminated. In addition, no false positives were obtained with non-contaminated samples. The limit of detection was found to be 145 mg/kg and the limit of quantification 341 mg/kg. The reproducibility tests of the measurements performed over several weeks showed that the results were always within the limits allowed. Additional studies were done to optimise the parameters in terms of number of samples analysed per unit of time or conveyor belt speed. It was shown that ergot can be detected using a speed of 1-100 mm/s and that a sample of 250 g can be analysed in 1 min.

Development of high performance liquid chromatography method for miconazole analysis in powder sample

NASA Astrophysics Data System (ADS)

Hermawan, D.; Suwandri; Sulaeman, U.; Istiqomah, A.; Aboul-Enein, H. Y.

2017-02-01

A simple high performance liquid chromatography (HPLC) method has been developed in this study for the analysis of miconazole, an antifungal drug, in powder sample. The optimized HPLC system using C8 column was achieved using mobile phase composition containing methanol:water (85:15, v/v), a flow rate of 0.8 mL/min, and UV detection at 220 nm. The calibration graph was linear in the range from 10 to 50 mg/L with r 2 of 0.9983. The limit of detection (LOD) and limit of quantitation (LOQ) obtained were 2.24 mg/L and 7.47 mg/L, respectively. The present HPLC method is applicable for the determination of miconazole in the powder sample with a recovery of 101.28 % (RSD = 0.96%, n = 3). The developed HPLC method provides short analysis time, high reproducibility and high sensitivity.

Determination of trace quaternary ammonium surfactants in water by combining solid-phase extraction with surface-assisted laser desorption/ionization mass spectrometry.

PubMed

Chen, Y C; Sun, M C

2001-01-01

This study demonstrates the feasibility of combining solid-phase extraction (SPE) with surface-assisted laser desorption/ionization (SALDI) mass spectrometry to determine trace quaternary ammonium surfactants in water. The trace surfactants in water were directly concentrated on the surface of activated carbon sorbent in SPE. The activated carbon sorbent was then mixed with the SALDI liquid for SALDI analysis. No SPE elution procedure was necessary. Experimental results indicate that the surfactants with longer chain alkyl groups exhibit higher sensitivities than those with shorter chain alkyl groups in SPE-SALDI analysis. The detection limit for hexadecyltrimethylammonium bromide is around 10 ppt in SPE-SALDI analysis by sampling 100 mL of aqueous solution, while that of tetradecyltrimethylammonium bromide is about 100 ppt. The detection limit for decyltrimethylammonium bromide and dodecyltrimethylammonium bromide is in the low-ppb range. Copyright 2001 John Wiley & Sons, Ltd.

Heterogeneity, histological features and DNA ploidy in oral carcinoma by image-based analysis.

PubMed

Diwakar, N; Sperandio, M; Sherriff, M; Brown, A; Odell, E W

2005-04-01

Oral squamous carcinomas appear heterogeneous on DNA ploidy analysis. However, this may be partly a result of sample dilution or the detection limit of techniques. The aim of this study was to determine whether oral squamous carcinomas are heterogeneous for ploidy status using image-based ploidy analysis and to determine whether ploidy status correlates with histological parameters. Multiple samples from 42 oral squamous carcinomas were analysed for DNA ploidy using an image-based system and scored for histological parameters. 22 were uniformly aneuploid, 1 uniformly tetraploid and 3 uniformly diploid. 16 appeared heterogeneous but only 8 appeared to be genuinely heterogeneous when minor ploidy histogram peaks were taken into account. Ploidy was closely related to nuclear pleomorphism but not differentiation. Sample variation, detection limits and diagnostic criteria account for much of the ploidy heterogeneity observed. Confident diagnosis of diploid status in an oral squamous cell carcinoma requires a minimum of 5 samples.

Application of Lipschitz Regularity and Multiscale Techniques for the Automatic Detection of Oil Spills in Synthetic Aperture Radar Imagery

NASA Astrophysics Data System (ADS)

Ajadi, O. A.; Meyer, F. J.; Tello, M.

2015-12-01

This research presents a promising new method for the detection and tracking of oil spills from Synthetic Aperture Radar (SAR) data. The method presented here combines a number of advanced image processing techniques in order to overcome some common performance limitations of SAR-based oil spill detection. Principal among these limitations are: (1) the radar cross section of the ocean surface strongly depends on wind and wave activities and is therefore highly variable; (2) the radar cross section of oil covered waters is often indistinguishable from other dark ocean features such as low wind areas or oil lookalikes, leading to ambiguities in oil spill detection. In this paper, we introduce two novel image analysis techniques to largely mitigate the aforementioned performance limitations, namely Lipschitz regularity (LR) and Wavelet transforms. We used LR, an image texture parameter akin to the slope of the local power spectrum, in our approach to mitigate these limitations. We show that the LR parameter is much less sensitive to variations of wind and waves than the original image amplitude, lending itself well for normalizing image content. Beyond its benefit for image normalization, we also show that the LR transform enhances the contrast between oil-covered and oil-free ocean surfaces and therefore improves overall spill detection performance. To calculate LR, the SAR images are decomposed using two-dimensional continuous wavelet transform (2D-CWT), which are furthermore transformed into Holder space to measure LR. Finally, we demonstrate that the implementation of wavelet transforms provide additional benefits related to the adaptive reduction of speckle noise. We show how LR and CWT are integrated into our image analysis workflow for application to oil spill detection. To describe the performance of this approach under controlled conditions, we applied our method to simulated SAR data of wind driven oceans containing oil spills of various properties. We also show applications to several real life oil spill scenarios using a series of L-band ALOS PALSAR images and X-band TerraSAR-X images acquired during the Deep Water Horizon spill in the Gulf of Mexico in 2010. From our analysis, we concluded that the LR and CWT have distinct advantages in oil spill detection and lead to high performance spill mapping results.

A novel COLD-PCR/FMCA assay enhances the detection of low-abundance IDH1 mutations in gliomas.

PubMed

Pang, Brendan; Durso, Mary B; Hamilton, Ronald L; Nikiforova, Marina N

2013-03-01

Point mutations in isocitrate dehydrogenase 1 (IDH1) have been identified in many gliomas. The detection of IDH1 mutations becomes challenging on suboptimal glioma biopsies when a limited number of tumor cells is available for analysis. Coamplification at lower denaturing-polymerase chain reaction (COLD-PCR) is a PCR technique that deliberately lowers the denaturing cycle temperature to selectively favor amplification of mutant alleles, allowing for the sensitive detection of low-abundance mutations. We developed a novel COLD-PCR assay on the LightCycler platform (Roche, Applied Science, Indianapolis, IN), using post-PCR fluorescent melting curve analysis (FMCA) for the detection of mutant IDH1 with a detection limit of 1%. Thirty-five WHO grade I to IV gliomas and 9 non-neoplastic brain and spinal cord biopsies were analyzed with this technique and the results were compared with the conventional real-time PCR and the Sanger sequencing analysis. COLD-PCR/FMCA was able to detect the most common IDH1 R132H mutation and rare mutation types including R132H, R132C, R132L, R132S, and R132G mutations. Twenty-five glioma cases were positive for IDH1 mutations by COLD-PCR/FMCA, and 23 gliomas were positive by the conventional real-time PCR and Sanger sequencing. A pilocytic astrocytoma (PA I) and a glioblastoma multiforme (GBM IV) showed low-abundance IDH1 mutations detected by COLD-PCR/FMCA. The remaining 10 glioma and 9 non-neoplastic samples were negative by all the 3 methods. In summary, we report a novel COLD-PCR/FMCA method that provides rapid and sensitive detection of IDH1 mutations in formalin-fixed paraffin-embedded tissue and can be used in the clinical setting to assess the small brain biopsies.

Chloride interference in the determination of bromate in drinking water by reagent free ion chromatography with mass spectrometry detection.

PubMed

Cavalli, Silvano; Polesello, Stefano; Valsecchi, Sara

2005-08-26

Bromate, a well known by-product of the ozonation of drinking water, has been included among the substances which have to be monitored in the drinking water according to the last EC Directive 251/98 on potable water with a regulated limit of 10 microg l(-1). The need of performing routine analysis at this limit is a driving force for the developing of new simple and sensitive methods of detection, which should be also able to overcome the effect of matrix composition. This work explored the use of mass spectrometry detection with electrospray ionisation hyphenated to a reagent free ion chromatograph with hydroxide gradient elution for the determination of bromate in drinking water. The use of a high capacity hydroxide selective column operated in gradient mode allowed to avoid the interference by carbonate peak, which moved to longer retention times. The effect of increasing chloride concentrations from 0 to 250 mg l(-1), which is the guideline limit for drinking water in Directive 251/98/EC, was to decrease absolute mass spectrometric response and chromatographic efficiency and, on the consequence, to increase the effective detection limits. The effect of the chloride concentration on the detection of bromate is discussed.

Single photon detection and signal analysis for high sensitivity dosimetry based on optically stimulated luminescence with beryllium oxide

NASA Astrophysics Data System (ADS)

Radtke, J.; Sponner, J.; Jakobi, C.; Schneider, J.; Sommer, M.; Teichmann, T.; Ullrich, W.; Henniger, J.; Kormoll, T.

2018-01-01

Single photon detection applied to optically stimulated luminescence (OSL) dosimetry is a promising approach due to the low level of luminescence light and the known statistical behavior of single photon events. Time resolved detection allows to apply a variety of different and independent data analysis methods. Furthermore, using amplitude modulated stimulation impresses time- and frequency information into the OSL light and therefore allows for additional means of analysis. Considering the impressed frequency information, data analysis by using Fourier transform algorithms or other digital filters can be used for separating the OSL signal from unwanted light or events generated by other phenomena. This potentially lowers the detection limits of low dose measurements and might improve the reproducibility and stability of obtained data. In this work, an OSL system based on a single photon detector, a fast and accurate stimulation unit and an FPGA is presented. Different analysis algorithms which are applied to the single photon data are discussed.

How to limit false positives in environmental DNA and metabarcoding?

PubMed

Ficetola, Gentile Francesco; Taberlet, Pierre; Coissac, Eric

2016-05-01

Environmental DNA (eDNA) and metabarcoding are boosting our ability to acquire data on species distribution in a variety of ecosystems. Nevertheless, as most of sampling approaches, eDNA is not perfect. It can fail to detect species that are actually present, and even false positives are possible: a species may be apparently detected in areas where it is actually absent. Controlling false positives remains a main challenge for eDNA analyses: in this issue of Molecular Ecology Resources, Lahoz-Monfort et al. () test the performance of multiple statistical modelling approaches to estimate the rate of detection and false positives from eDNA data. Here, we discuss the importance of controlling for false detection from early steps of eDNA analyses (laboratory, bioinformatics), to improve the quality of results and allow an efficient use of the site occupancy-detection modelling (SODM) framework for limiting false presences in eDNA analysis. © 2016 John Wiley & Sons Ltd.

Breath acetone monitoring by portable Si:WO3 gas sensors

PubMed Central

Righettoni, Marco; Tricoli, Antonio; Gass, Samuel; Schmid, Alex; Amann, Anton; Pratsinis, Sotiris E.

2013-01-01

Breath analysis has the potential for early stage detection and monitoring of illnesses to drastically reduce the corresponding medical diagnostic costs and improve the quality of life of patients suffering from chronic illnesses. In particular, the detection of acetone in the human breath is promising for non-invasive diagnosis and painless monitoring of diabetes (no finger pricking). Here, a portable acetone sensor consisting of flame-deposited and in situ annealed, Si-doped epsilon-WO3 nanostructured films was developed. The chamber volume was miniaturized while reaction-limited and transport-limited gas flow rates were identified and sensing temperatures were optimized resulting in a low detection limit of acetone (~20 ppb) with short response (10–15 s) and recovery times (35–70 s). Furthermore, the sensor signal (response) was robust against variations of the exhaled breath flow rate facilitating application of these sensors at realistic relative humidities (80–90%) as in the human breath. The acetone content in the breath of test persons was monitored continuously and compared to that of state-of-the-art proton transfer reaction mass spectrometry (PTR-MS). Such portable devices can accurately track breath acetone concentration to become an alternative to more elaborate breath analysis techniques. PMID:22790702

Identification of faulty sensor using relative partial decomposition via independent component analysis

NASA Astrophysics Data System (ADS)

Wang, Z.; Quek, S. T.

2015-07-01

Performance of any structural health monitoring algorithm relies heavily on good measurement data. Hence, it is necessary to employ robust faulty sensor detection approaches to isolate sensors with abnormal behaviour and exclude the highly inaccurate data in the subsequent analysis. The independent component analysis (ICA) is implemented to detect the presence of sensors showing abnormal behaviour. A normalized form of the relative partial decomposition contribution (rPDC) is proposed to identify the faulty sensor. Both additive and multiplicative types of faults are addressed and the detectability illustrated using a numerical and an experimental example. An empirical method to establish control limits for detecting and identifying the type of fault is also proposed. The results show the effectiveness of the ICA and rPDC method in identifying faulty sensor assuming that baseline cases are available.

[Exposure to organic halogen compounds in drinking water of 9 Italian regions: exposure to chlorites, chlorates, thrihalomethanes, trichloroethylene and tetrachloroethylene].

PubMed

Fantuzzi, G; Aggazzotti, G; Righi, E; Predieri, G; Giacobazzi, P; Kanitz, S; Barbone, F; Sansebastiano, G; Ricci, C; Leoni, V; Fabiani, L; Triassi, M

2007-01-01

This study investigated the exposure to organohalogens compounds in drinking water from 9 Italian towns (Udine, Genova, Parma, Modena, Siena, Roma, L'Aquila, Napoli and Catania). Overall, 1199 samples collected from 72 waterworks were analyzed. THMs, trichloroethylene and tetrachloroethylene were evaluated using the head-space gas chromatographic technique (detection limit of 0.01 microg/l; chlorite and chlorate analysis was performed by ion chromatography (detection limit of 20 microg/l). THMs were evidenced in 925 samples (77%) (median value: 1.12 micro/l; range: 0.01-54 mciro/l) and 7 were higher than the THMs Italian limit of 30 microg/l. Chlorite and chlorate levels were higher than the detection limit in 45% for chlorite and in 34% for chlorate samples; median values were 221 microg/l and 76 microg/l, respectively. Chlorite values were higher than the chlorite Italian limit (700 microg/l) in 35 samples (8.7%). Trichloroethylene and tetrachloroethylene were measured in 29% and 44% of the investigated samples and showed values lower than the Italian limit (highest levels of 6 microg/l and 9 microg/l, respectively). The low levels detected of THMs, trichloroethylene and tetrachloroethylene have no potentials effects on human health, whereas, the levels of chlorite and chlorates should be further evaluated and their potential effects for the populations using these drinking waters, better understood.

Simultaneous determination of ethyl carbamate and urea in Korean rice wine by ultra-performance liquid chromatography coupled with mass spectrometric detection.

PubMed

Lee, Gyeong-Hweon; Bang, Dae-Young; Lim, Jung-Hoon; Yoon, Seok-Min; Yea, Myeong-Jai; Chi, Young-Min

2017-10-15

In this study, a rapid method for simultaneous detection of ethyl carbamate (EC) and urea in Korean rice wine was developed. To achieve quantitative analysis of EC and urea, the conditions for Ultra-performance liquid chromatography (UPLC) separation and atmospheric-pressure chemical ionization tandem mass spectrometry (APCI-MS/MS) detection were first optimized. Under the established conditions, the detection limit, relative standard deviation and linear range were 2.83μg/L, 3.75-5.96%, and 0.01-10.0mg/L, respectively, for urea; the corresponding values were 0.17μg/L, 1.06-4.01%, and 1.0-50.0μg/L, respectively, for EC. The correlation between the contents of EC and its precursor urea was determined under specific pH (3.5 and 4.5) and temperature (4, 25, and 50°C) conditions using the developed method. As a result, EC content was increased with greater temperature and lower pH. In Korean rice wine, urea was detected 0.19-1.37mg/L and EC was detected 2.0-7.7μg/L. The method developed in this study, which has the advantages of simplified sample preparation, low detection limits, and good selectivity, was successfully applied for the rapid analysis of EC and urea. Copyright © 2017 Elsevier B.V. All rights reserved.

Evaluation of radiochemical neutron activation analysis methods for determination of arsenic in biological materials.

PubMed

Paul, Rick L

2011-01-01

Radiochemical neutron activation analysis (RNAA) with retention on hydrated manganese dioxide (HMD) has played a key role in the certification of As in biological materials at NIST. Although this method provides very high and reproducible yields and detection limits at low microgram/kilogram levels, counting geometry uncertainties may arise from unequal distribution of As in the HMD, and arsenic detection limits may not be optimal due to significant retention of other elements. An alternate RNAA procedure with separation of arsenic by solvent extraction has been investigated. After digestion of samples in nitric and perchloric acids, As(III) is extracted from 2 M sulfuric acid solution into a solution of zinc diethyldithiocarbamate in chloroform. Counting of (76)As allows quantitation of arsenic. Addition of an (77)As tracer solution prior to dissolution allows correction for chemical yield and counting geometries, further improving reproducibility. The HMD and solvent extraction procedures for arsenic were compared through analysis of SRMs 1577c (bovine liver), 1547 (peach leaves), and 1575a (pine needles). Both methods gave As results in agreement with certified values with comparable reproducibility. However, the solvent extraction method yields a factor of 3 improvement in detection limits and is less time-consuming than the HMD method. The new method shows great promise for use in As certification in reference materials.

A compact high resolution ion mobility spectrometer for fast trace gas analysis.

PubMed

Kirk, Ansgar T; Allers, Maria; Cochems, Philipp; Langejuergen, Jens; Zimmermann, Stefan

2013-09-21

Drift tube ion mobility spectrometers (IMS) are widely used for fast trace gas detection in air, but portable compact systems are typically very limited in their resolving power. Decreasing the initial ion packet width improves the resolution, but is generally associated with a reduced signal-to-noise-ratio (SNR) due to the lower number of ions injected into the drift region. In this paper, we present a refined theory of IMS operation which employs a combined approach for the analysis of the ion drift and the subsequent amplification to predict both the resolution and the SNR of the measured ion current peak. This theoretical analysis shows that the SNR is not a function of the initial ion packet width, meaning that compact drift tube IMS with both very high resolution and extremely low limits of detection can be designed. Based on these implications, an optimized combination of a compact drift tube with a length of just 10 cm and a transimpedance amplifier has been constructed with a resolution of 183 measured for the positive reactant ion peak (RIP(+)), which is sufficient to e.g. separate the RIP(+) from the protonated acetone monomer, even though their drift times only differ by a factor of 1.007. Furthermore, the limits of detection (LODs) for acetone are 180 pptv within 1 s of averaging time and 580 pptv within only 100 ms.

A New Method for the Fast Analysis of Trihalomethanes in Tap and Recycled Waters Using Headspace Gas Chromatography with Micro-Electron Capture Detection.

PubMed

Alexandrou, Lydon D; Meehan, Barry J; Morrison, Paul D; Jones, Oliver A H

2017-05-15

Chemical disinfection of water supplies brings significant public health benefits by reducing microbial contamination. The process can however, result in the formation of toxic compounds through interactions between disinfectants and organic material in the source water. These new compounds are termed disinfection by-products (DBPs). The most common are the trihalomethanes (THMs) such as trichloromethane (chloroform), dichlorobromomethane, chlorodibromomethane and tribromomethane (bromoform); these are commonly reported as a single value for total trihalomethanes (TTHMs). Analysis of DBPs is commonly performed via time- and solvent-intensive sample preparation techniques such as liquid-liquid and solid phase extraction. In this study, a method using headspace gas chromatography with micro-electron capture detection was developed and applied for the analysis of THMs in drinking and recycled waters from across Melbourne (Victoria, Australia). The method allowed almost complete removal of the sample preparation step whilst maintaining trace level detection limits (>1 ppb). All drinking water samples had TTHM concentrations below the Australian regulatory limit of 250 µg/L but some were above the U.S. EPA limit of 60 µg/L. The highest TTHM concentration was 67.2 µg/L and lowest 22.9 µg/L. For recycled water, samples taken directly from treatment plants held significantly higher concentrations (153.2 µg/L TTHM) compared to samples from final use locations (4.9-9.3 µg/L).

Proton-proton bremsstrahlung towards the elastic limit

NASA Astrophysics Data System (ADS)

Mahjour-Shafiei, M.; Amir-Ahmadi, H. R.; Bacelar, J. C. S.; Castelijns, R.; Ermisch, K.; van Garderen, E.; Gašparić, I.; Harakeh, M. N.; Kalantar-Nayestanaki, N.; Kiš, M.; Löhner, H.

2005-05-01

In oder to study proton-proton bremsstrahlung moving towards the elastic limit, a detection system, consisting of Plastic-ball and SALAD, was set up and an experiment at 190 MeV incident beam energy was performed. Here, the experimental setup and the data analysis procedure along with some results obtained in the measurement are discussed.

Sensitivity and accuracy of high-throughput metabarcoding methods for early detection of invasive fish species

NASA Astrophysics Data System (ADS)

Hatzenbuhler, Chelsea; Kelly, John R.; Martinson, John; Okum, Sara; Pilgrim, Erik

2017-04-01

High-throughput DNA metabarcoding has gained recognition as a potentially powerful tool for biomonitoring, including early detection of aquatic invasive species (AIS). DNA based techniques are advancing, but our understanding of the limits to detection for metabarcoding complex samples is inadequate. For detecting AIS at an early stage of invasion when the species is rare, accuracy at low detection limits is key. To evaluate the utility of metabarcoding in future fish community monitoring programs, we conducted several experiments to determine the sensitivity and accuracy of routine metabarcoding methods. Experimental mixes used larval fish tissue from multiple “common” species spiked with varying proportions of tissue from an additional “rare” species. Pyrosequencing of genetic marker, COI (cytochrome c oxidase subunit I) and subsequent sequence data analysis provided experimental evidence of low-level detection of the target “rare” species at biomass percentages as low as 0.02% of total sample biomass. Limits to detection varied interspecifically and were susceptible to amplification bias. Moreover, results showed some data processing methods can skew sequence-based biodiversity measurements from corresponding relative biomass abundances and increase false absences. We suggest caution in interpreting presence/absence and relative abundance in larval fish assemblages until metabarcoding methods are optimized for accuracy and precision.

Trace analysis of muramic acid in indoor air using an automated derivatization instrument and GC-MS(2) or GC-MS(3).

PubMed

Harley, William M; Kozar, Michael P; Fox, Alvin

2002-09-01

An automated derivatization instrument has been developed for the preparation of alditol acetates from bacterial hydrolysates for analysis by gas chromatography-mass spectrometry (GC-MS). The current report demonstrates the utility of the automated instrument for the more demanding task of trace analysis of muramic acid (Mur) in airborne dust using gas chromatography-tandem mass spectrometry (GC-MS(2)). Conditions for efficient derivatization of Mur, vital for trace analysis, are rigorous including lactam and imido group formation under anhydrous conditions. Furthermore, as the detection limit is lowered, possible contamination or carry-over of samples becomes an increasingly greater consideration and must not occur. The instrument meets these criteria and was successfully used for assaying the levels of Mur in laboratory air, which were found to be much lower than in the previous studies of heavily occupied schools and agricultural environments. The potential for GC-MS(3) in further lowering the detection limit was also demonstrated.

Development of low level 226Ra analysis for live fish using gamma-ray spectrometry

NASA Astrophysics Data System (ADS)

Chandani, Z.; Prestwich, W. V.; Byun, S. H.

2017-06-01

A low level 226Ra analysis method for live fish was developed using a 4π NaI(Tl) gamma-ray spectrometer. In order to find out the best algorithm for accomplishing the lowest detection limit, the gamma-ray spectrum from a 226Ra point was collected and nine different methods were attempted for spectral analysis. The lowest detection limit of 0.99 Bq for an hour counting occurred when the spectrum was integrated in the energy region of 50-2520 keV. To extend 226Ra analysis to live fish, a Monte Carlo simulation model with a cylindrical fish in a water container was built using the MCNP code. From simulation results, the spatial distribution of the efficiency and the efficiency correction factor for the live fish model were determined. The MCNP model will be able to be conveniently modified when a different fish or container geometry is employed as fish grow up in real experiments.

Sample-morphology effects on x-ray photoelectron peak intensities. II. Estimation of detection limits for thin-film materials

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

Powell, Cedric J., E-mail: cedric.powell@nist.gov; Werner, Wolfgang S. M.; Smekal, Werner

2014-09-01

The authors show that the National Institute of Standards and Technology database for the simulation of electron spectra for surface analysis (SESSA) can be used to determine detection limits for thin-film materials such as a thin film on a substrate or buried at varying depths in another material for common x-ray photoelectron spectroscopy (XPS) measurement conditions. Illustrative simulations were made for a W film on or in a Ru matrix and for a Ru film on or in a W matrix. In the former case, the thickness of a W film at a given depth in the Ru matrix wasmore » varied so that the intensity of the W 4d{sub 5/2} peak was essentially the same as that for a homogeneous RuW{sub 0.001} alloy. Similarly, the thickness of a Ru film at a selected depth in the W matrix was varied so that the intensity of the Ru 3p{sub 3/2} peak matched that from a homogeneous WRu{sub 0.01} alloy. These film thicknesses correspond to the detection limits of each minor component for measurement conditions where the detection limits for a homogeneous sample varied between 0.1 at. % (for the RuW{sub 0.001} alloy) and 1 at. % (for the WRu{sub 0.01} alloy). SESSA can be similarly used to convert estimates of XPS detection limits for a minor species in a homogeneous solid to the corresponding XPS detection limits for that species as a thin film on or buried in the chosen solid.« less

First direct detection limits on sub-GeV dark matter from XENON10.

PubMed

Essig, Rouven; Manalaysay, Aaron; Mardon, Jeremy; Sorensen, Peter; Volansky, Tomer

2012-07-13

The first direct detection limits on dark matter in the MeV to GeV mass range are presented, using XENON10 data. Such light dark matter can scatter with electrons, causing ionization of atoms in a detector target material and leading to single- or few-electron events. We use 15  kg day of data acquired in 2006 to set limits on the dark-matter-electron scattering cross section. The strongest bound is obtained at 100 MeV where σ(e)<3×10(-38)  cm2 at 90% C.L., while dark-matter masses between 20 MeV and 1 GeV are bounded by σ(e)<10(-37)  cm2 at 90% C.L. This analysis provides a first proof of principle that direct detection experiments can be sensitive to dark-matter candidates with masses well below the GeV scale.

Recent advances in chemiluminescence detection coupled with capillary electrophoresis and microchip capillary electrophoresis.

PubMed

Liu, Yuxuan; Huang, Xiangyi; Ren, Jicun

2016-01-01

CE is an ideal analytical method for extremely volume-limited biological microenvironments. However, the small injection volume makes it a challenge to achieve highly sensitive detection. Chemiluminescence (CL) detection is characterized by providing low background with excellent sensitivity because of requiring no light source. The coupling of CL with CE and MCE has become a powerful analytical method. So far, this method has been widely applied to chemical analysis, bioassay, drug analysis, and environment analysis. In this review, we first introduce some developments for CE-CL and MCE-CL systems, and then put the emphasis on the applications in the last 10 years. Finally, we discuss the future prospects. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Polymer microchip capillary electrophoresis of proteins either off- or on-chip labeled with chameleon dye for simplified analysis

PubMed Central

Yu, Ming; Wang, Hsiang-Yu; Woolley, Adam

2009-01-01

Microchip capillary electrophoresis of proteins labeled either off- or on-chip with the “chameleon” CE dye 503 using poly(methyl methacrylate) microchips is presented. A simple dynamic coating using the cationic surfactant cetyltrimethyl ammonium bromide prevented nonspecific adsorption of protein and dye to the channel walls. The labeling reactions for both off- and on-chip labeling proceeded at room temperature without requiring heating steps. In off-chip labeling, a 9 ng/mL concentration detection limit for bovine serum albumin (BSA), corresponding to a ~7 fg (100 zmol) mass detection limit, was obtained. In on-chip tagging, the free dye and protein were placed in different reservoirs of the microchip, and an extra incubation step was not needed. A 1 μg/mL concentration detection limit for BSA, corresponding to a ~700 fg (10 amol) mass detection limit, was obtained from this protocol. The earlier elution time of the BSA peak in on-chip labeling resulted from fewer total labels on each protein molecule. Our on-chip labeling method is an important part of automation in miniaturized devices. PMID:19924700

Predictive inference for best linear combination of biomarkers subject to limits of detection.

PubMed

Coolen-Maturi, Tahani

2017-08-15

Measuring the accuracy of diagnostic tests is crucial in many application areas including medicine, machine learning and credit scoring. The receiver operating characteristic (ROC) curve is a useful tool to assess the ability of a diagnostic test to discriminate between two classes or groups. In practice, multiple diagnostic tests or biomarkers are combined to improve diagnostic accuracy. Often, biomarker measurements are undetectable either below or above the so-called limits of detection (LoD). In this paper, nonparametric predictive inference (NPI) for best linear combination of two or more biomarkers subject to limits of detection is presented. NPI is a frequentist statistical method that is explicitly aimed at using few modelling assumptions, enabled through the use of lower and upper probabilities to quantify uncertainty. The NPI lower and upper bounds for the ROC curve subject to limits of detection are derived, where the objective function to maximize is the area under the ROC curve. In addition, the paper discusses the effect of restriction on the linear combination's coefficients on the analysis. Examples are provided to illustrate the proposed method. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Determination of target detection limits in hyperspectral data using band selection and dimensionality reduction

NASA Astrophysics Data System (ADS)

Gross, W.; Boehler, J.; Twizer, K.; Kedem, B.; Lenz, A.; Kneubuehler, M.; Wellig, P.; Oechslin, R.; Schilling, H.; Rotman, S.; Middelmann, W.

2016-10-01

Hyperspectral remote sensing data can be used for civil and military applications to robustly detect and classify target objects. High spectral resolution of hyperspectral data can compensate for the comparatively low spatial resolution, which allows for detection and classification of small targets, even below image resolution. Hyperspectral data sets are prone to considerable spectral redundancy, affecting and limiting data processing and algorithm performance. As a consequence, data reduction strategies become increasingly important, especially in view of near-real-time data analysis. The goal of this paper is to analyze different strategies for hyperspectral band selection algorithms and their effect on subpixel classification for different target and background materials. Airborne hyperspectral data is used in combination with linear target simulation procedures to create a representative amount of target-to-background ratios for evaluation of detection limits. Data from two different airborne hyperspectral sensors, AISA Eagle and Hawk, are used to evaluate transferability of band selection when using different sensors. The same target objects were recorded to compare the calculated detection limits. To determine subpixel classification results, pure pixels from the target materials are extracted and used to simulate mixed pixels with selected background materials. Target signatures are linearly combined with different background materials in varying ratios. The commonly used classification algorithms Adaptive Coherence Estimator (ACE) is used to compare the detection limit for the original data with several band selection and data reduction strategies. The evaluation of the classification results is done by assuming a fixed false alarm ratio and calculating the mean target-to-background ratio of correctly detected pixels. The results allow drawing conclusions about specific band combinations for certain target and background combinations. Additionally, generally useful wavelength ranges are determined and the optimal amount of principal components is analyzed.

Development of a sensitive GC-C-IRMS method for the analysis of androgens.

PubMed

Polet, Michael; Van Gansbeke, Wim; Deventer, Koen; Van Eenoo, Peter

2013-02-01

The administration of anabolic steroids is one of the most important issues in doping control and is detectable through a change in the carbon isotopic composition of testosterone and/or its metabolites. Gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS), however, remains a very laborious and expensive technique and substantial amounts of urine are needed to meet the sensitivity requirements of the IRMS. This can be problematic because only a limited amount of urine is available for anti-doping analysis on a broad spectrum of substances. In this work we introduce a new type of injection that increases the sensitivity of GC-C-IRMS by a factor of 13 and reduces the limit of detection, simply by using solvent vent injections instead of splitless injection. This drastically reduces the amount of urine required. On top of that, by only changing the injection technique, the detection parameters of the IRMS are not affected and there is no loss in linearity. Copyright © 2012 John Wiley & Sons, Ltd.

Driver gene classification reveals a substantial overrepresentation of tumor suppressors among very large chromatin-regulating proteins.

PubMed

Waks, Zeev; Weissbrod, Omer; Carmeli, Boaz; Norel, Raquel; Utro, Filippo; Goldschmidt, Yaara

2016-12-23

Compiling a comprehensive list of cancer driver genes is imperative for oncology diagnostics and drug development. While driver genes are typically discovered by analysis of tumor genomes, infrequently mutated driver genes often evade detection due to limited sample sizes. Here, we address sample size limitations by integrating tumor genomics data with a wide spectrum of gene-specific properties to search for rare drivers, functionally classify them, and detect features characteristic of driver genes. We show that our approach, CAnceR geNe similarity-based Annotator and Finder (CARNAF), enables detection of potentially novel drivers that eluded over a dozen pan-cancer/multi-tumor type studies. In particular, feature analysis reveals a highly concentrated pool of known and putative tumor suppressors among the <1% of genes that encode very large, chromatin-regulating proteins. Thus, our study highlights the need for deeper characterization of very large, epigenetic regulators in the context of cancer causality.

Determination of patulin in commercial apple juice by micellar electrokinetic chromatography.

PubMed

Murillo, M; González-Peñas, E; Amézqueta, S

2008-01-01

A novel and validated micellar electrokinetic capillary chromatography (MEKC) method using ultraviolet detection (UV) has been applied to the quantitative analysis of patulin (PAT) in commercial apple juice. Patulin was extracted from samples with an ethylacetate solution. The micellar electrokinetic capillary chromatography (MECK) parameters studied for method optimization were buffer composition, voltage, temperature, and a separation between PAT and 5-hydroxymethylfurfural (HMF) (main interference in apple juice PAT analysis) peaks until reaching baseline. The method passes a series of validation tests including selectivity, linearity, limit of detection and quantification (0.7 and 2.5 microgL(-1), respectively), precision (within and between-day variability) and recovery (80.2% RSD=4%), accuracy, and robustness. This method was successfully applied to the measurement of 20 apple juice samples obtained from different supermarkets. One hundred percent of the samples were contaminated with a level greater than the limit of detection, with mean and median values of 41.3 and 35.7 microgL(-1), respectively.

Apricot DNA as an indicator for persipan: detection and quantitation in marzipan using ligation-dependent probe amplification.

PubMed

Luber, Florian; Demmel, Anja; Hosken, Anne; Busch, Ulrich; Engel, Karl-Heinz

2012-06-13

The confectionery ingredient marzipan is exclusively prepared from almond kernels and sugar. The potential use of apricot kernels, so-called persipan, is an important issue for the quality assessment of marzipan. Therefore, a ligation-dependent probe amplification (LPA) assay was developed that enables a specific and sensitive detection of apricot DNA, as an indicator for the presence of persipan. The limit of detection was determined to be 0.1% persipan in marzipan. The suitability of the method was confirmed by the analysis of 20 commercially available food samples. The integration of a Prunus -specific probe in the LPA assay as a reference allowed for the relative quantitation of persipan in marzipan. The limit of quantitation was determined to be 0.5% persipan in marzipan. The analysis of two self-prepared mixtures of marzipan and persipan demonstrated the applicability of the quantitation method at concentration levels of practical relevance for quality control.

Digital photo monitoring for tree crown

Treesearch

Neil Clark; Sang-Mook Lee

2007-01-01

Assessing change in the amount of foliage within a tree’s crown is the goal of crown transparency estimation, a component in many forest health assessment programs. Many sources of variability limit analysis and interpretation of crown condition data. Increased precision is needed to detect more subtle changes that are important for detection of health problems....

Post-capillary reaction detection in capillary electrophoresis based on the streptavidin-biotin interaction. Optimization and application to single cell analysis.

PubMed

Feltus, A; Hentz, N G; Daunert, S

2001-05-25

A class-selective post-capillary reaction detection method for capillary electrophoresis is described in which a streptavidin-fluorescein isothiocyanate (streptavidin-FITC) conjugate is used to detect biotin moieties. The selective binding of biotin moieties to the streptavidin-FITC conjugate causes an enhancement of fluorescence proportional to the concentration of biotin present. After capillary electrophoresis the separated analytes react with streptavidin-FITC in a coaxial reactor and are then detected either by a benchtop spectrofluorometer (2.5 microM detection limit) or by an epi-fluorescence microscope (1 x 10(-7) M detection limit). The method is used to examine biotinylated species in a crude mammalian cell lysate which was found to contain 83+/-3 fmol in 3600 cell volumes. In addition, it is used to examine the uptake of biotin by individual sea urchin oocytes. The results indicate that, in the oocytes, biocytin is the prevalent form of biotin and its concentration varies widely between cells (mean=2+/-2 microM).

Detection of the level of fluoride in the commercially available toothpaste using laser induced breakdown spectroscopy with the marker atomic transition line of neutral fluorine at 731.1 nm

NASA Astrophysics Data System (ADS)

Gondal, M. A.; Maganda, Y. W.; Dastageer, M. A.; Al Adel, F. F.; Naqvi, A. A.; Qahtan, T. F.

2014-04-01

Fourth harmonic of a pulsed Nd:YAG laser (wavelength 266 nm) in combination with high resolution spectrograph equipped with Gated ICCD camera has been employed to design a high sensitive analytical system. This detection system is based on Laser Induced Breakdown Spectroscopy and has been tested first time for analysis of semi-fluid samples to detect fluoride content present in the commercially available toothpaste samples. The experimental parameters were optimized to achieve an optically thin and in local thermo dynamic equilibrium plasma. This improved the limits of detection of fluoride present in tooth paste samples. The strong atomic transition line of fluorine at 731.102 nm was used as the marker line to quantify the fluoride concentration levels. Our LIBS system was able to detect fluoride concentration levels in the range of 1300-1750 ppm with a detection limit of 156 ppm.

Lowering detection limits for 1,2,3-trichloropropane in water using solid phase extraction coupled to purge and trap sample introduction in an isotope dilution GC-MS method.

PubMed

Liao, Wenta; Ghabour, Miriam; Draper, William M; Chandrasena, Esala

2016-09-01

Purge and trap sample introduction (PTI) has been the premier sampling and preconcentration technique for gas chromatographic determination of volatile organic compounds (VOCs) in drinking water for almost 50 years. PTI affords sub parts-per-billion (ppb) detection limits for purgeable VOCs including fixed gases and higher boiling hydrocarbons and halocarbons. In this study the coupling of solid phase extraction (SPE) to PTI was investigated as a means to substantially increase enrichment and lower detection limits for the emerging contaminant, 1,2,3-trichloropropane (TCP). Water samples (500 mL) were dechlorinated, preserved with a biocide, and spiked with the isotope labeled internal standard, d5-TCP. The entire 500 mL sample was extracted with activated carbon or carbon molecular sieve SPE cartridges, and then eluted with dichloromethane -- excess solvent was removed in a nitrogen evaporator and diethylene glycol "keeper" remaining was dispersed in 5 mL of water for PTI GC-MS analysis. The experimental Method Detection Limit (MDL) for TCP was 0.11 ng/L (ppt) and accuracy was 95-103% in sub-ppt determinations. Groundwater samples including impaired California sources and treated water (n = 21) were analyzed with results ranging from below the method reporting limit (0.30 ng/L) to > 250 ng/L. Coupling of SPE with PTI may provide similar reductions in detection limits for other VOCs with appropriate physical-chemical properties. Copyright © 2016 Elsevier Ltd. All rights reserved.

Method and Apparatus for Concentrating Vapors for Analysis

DOEpatents

Grate, Jay W.; Baldwin, David L.; Anheier, Jr., Norman C.

2008-10-07

An apparatus and method are disclosed for pre-concentrating gaseous vapors for analysis. The invention finds application in conjunction with, e.g., analytical instruments where low detection limits for gaseous vapors are desirable. Vapors sorbed and concentrated within the bed of the apparatus can be thermally desorbed achieving at least partial separation of vapor mixtures. The apparatus is suitable, e.g., for preconcentration and sample injection, and provides greater resolution of peaks for vapors within vapor mixtures, yielding detection levels that are 10-10,000 times better than for direct sampling and analysis systems. Features are particularly useful for continuous unattended monitoring applications.

Performance and sensitivity analysis of the generalized likelihood ratio method for failure detection. M.S. Thesis

NASA Technical Reports Server (NTRS)

Bueno, R. A.

1977-01-01

Results of the generalized likelihood ratio (GLR) technique for the detection of failures in aircraft application are presented, and its relationship to the properties of the Kalman-Bucy filter is examined. Under the assumption that the system is perfectly modeled, the detectability and distinguishability of four failure types are investigated by means of analysis and simulations. Detection of failures is found satisfactory, but problems in identifying correctly the mode of a failure may arise. These issues are closely examined as well as the sensitivity of GLR to modeling errors. The advantages and disadvantages of this technique are discussed, and various modifications are suggested to reduce its limitations in performance and computational complexity.

Energy-Dispersive X-Ray Fluorescence Spectrometry: A Long Overdue Addition to the Chemistry Curriculum

ERIC Educational Resources Information Center

Palmer, Peter T.

2011-01-01

Portable Energy-Dispersive X-Ray Fluorescence (XRF) analyzers have undergone significant improvements over the past decade. Salient advantages of XRF for elemental analysis include minimal sample preparation, multielement analysis capabilities, detection limits in the low parts per million (ppm) range, and analysis times on the order of 1 min.…

State-of-the-Art Resources (SOAR) for Software Vulnerability Detection, Test, and Evaluation

DTIC Science & Technology

2014-07-01

preclude in-depth analysis, and widespread use of a Software -as-a- Service ( SaaS ) model that limits data availability and application to DoD systems...provide mobile application analysis using a Software - as-a- Service ( SaaS ) model. In this case, any software to be analyzed must be sent to the...tools are only available through a SaaS model. The widespread use of a Software -as-a- Service ( SaaS ) model as a sole evaluation model limits data

Direct detection of light “Ge-phobic” exothermic dark matter

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

Gelmini, Graciela B.; Georgescu, Andreea; Huh, Ji-Haeng

2014-07-15

We present comparisons of direct dark matter (DM) detection data for light WIMPs with exothermic scattering with nuclei (exoDM), both assuming the Standard Halo Model (SHM) and in a halo model — independent manner. Exothermic interactions favor light targets, thus reducing the importance of upper limits derived from xenon targets, the most restrictive of which is at present the LUX limit. In our SHM analysis the CDMS-II-Si and CoGeNT regions become allowed by these bounds, however the recent SuperCDMS limit rejects both regions for exoDM with isospin-conserving couplings. An isospin-violating coupling of the exoDM, in particular one with a neutronmore » to proton coupling ratio of −0.8 (which we call “Ge-phobic”), maximally reduces the DM coupling to germanium and allows the CDMS-II-Si region to become compatible with all bounds. This is also clearly shown in our halo-independent analysis.« less

The analysis of tetracyclines, quinolones, macrolides, lincosamides, pleuromutilins, and sulfonamides in chicken feathers using UHPLC-MS/MS in order to monitor antibiotic use in the poultry sector.

PubMed

Jansen, Larissa J M; Bolck, Yvette J C; Rademaker, Janneau; Zuidema, Tina; Berendsen, Bjorn J A

2017-08-01

In The Netherlands, all antibiotic treatments should be registered at the farm and in a central database. To enforce correct antibiotic use and registration, and to enforce prudent use of antibiotics, there is a need for methods that are able to detect antibiotic treatments. Ideally, such a method is able to detect antibiotic applications during the entire lifespan of an animal, including treatments administered during the first days of the animals' lives. Monitoring tissue, as is common practice, only provides a limited window of opportunity, as residue levels in tissue soon drop below measurable quantities. The analysis of feathers proves to be a promising tool in this respect. Furthermore, a qualitative confirmatory method was developed for the analyses of six major groups of antibiotics in ground chicken feathers, aiming for a detection limit as low as reasonably possible. The method was validated according to Commission Decision 2002/657/EC. All compounds comply with the criteria and, as a matter of fact, 58% of the compounds could also be quantified according to regulations. Additionally, we demonstrated that a less laborious method, in which whole feathers were analyzed, proved successful in the detection of applied antibiotics. Most compounds could be detected at levels of 2 μg kg -1 or below with the exception of sulfachloropyridazine, tylosin, and tylvalosin. This demonstrates the effectiveness of feather analysis to detect antibiotic use to allow effective enforcement of antibiotic use and prevent the illegal, off-label, and nonregistered use of antibiotics.

Fully automated analytical procedure for propofol determination by sequential injection technique with spectrophotometric and fluorimetric detections.

PubMed

Šrámková, Ivana; Amorim, Célia G; Sklenářová, Hana; Montenegro, Maria C B M; Horstkotte, Burkhard; Araújo, Alberto N; Solich, Petr

2014-01-01

In this work, an application of an enzymatic reaction for the determination of the highly hydrophobic drug propofol in emulsion dosage form is presented. Emulsions represent a complex and therefore challenging matrix for analysis. Ethanol was used for breakage of a lipid emulsion, which enabled optical detection. A fully automated method based on Sequential Injection Analysis was developed, allowing propofol determination without the requirement of tedious sample pre-treatment. The method was based on spectrophotometric detection after the enzymatic oxidation catalysed by horseradish peroxidase and subsequent coupling with 4-aminoantipyrine leading to a coloured product with an absorbance maximum at 485 nm. This procedure was compared with a simple fluorimetric method, which was based on the direct selective fluorescence emission of propofol in ethanol at 347 nm. Both methods provide comparable validation parameters with linear working ranges of 0.005-0.100 mg mL(-1) and 0.004-0.243 mg mL(-1) for the spectrophotometric and fluorimetric methods, respectively. The detection and quantitation limits achieved with the spectrophotometric method were 0.0016 and 0.0053 mg mL(-1), respectively. The fluorimetric method provided the detection limit of 0.0013 mg mL(-1) and limit of quantitation of 0.0043 mg mL(-1). The RSD did not exceed 5% and 2% (n=10), correspondingly. A sample throughput of approx. 14 h(-1) for the spectrophotometric and 68 h(-1) for the fluorimetric detection was achieved. Both methods proved to be suitable for the determination of propofol in pharmaceutical formulation with average recovery values of 98.1 and 98.5%. © 2013 Elsevier B.V. All rights reserved.

Detection limits of quantitative and digital PCR assays and their influence in presence-absence surveys of environmental DNA.

PubMed

Hunter, Margaret E; Dorazio, Robert M; Butterfield, John S S; Meigs-Friend, Gaia; Nico, Leo G; Ferrante, Jason A

2017-03-01

A set of universal guidelines is needed to determine the limit of detection (LOD) in PCR-based analyses of low-concentration DNA. In particular, environmental DNA (eDNA) studies require sensitive and reliable methods to detect rare and cryptic species through shed genetic material in environmental samples. Current strategies for assessing detection limits of eDNA are either too stringent or subjective, possibly resulting in biased estimates of species' presence. Here, a conservative LOD analysis grounded in analytical chemistry is proposed to correct for overestimated DNA concentrations predominantly caused by the concentration plateau, a nonlinear relationship between expected and measured DNA concentrations. We have used statistical criteria to establish formal mathematical models for both quantitative and droplet digital PCR. To assess the method, a new Grass Carp (Ctenopharyngodon idella) TaqMan assay was developed and tested on both PCR platforms using eDNA in water samples. The LOD adjustment reduced Grass Carp occupancy and detection estimates while increasing uncertainty-indicating that caution needs to be applied to eDNA data without LOD correction. Compared to quantitative PCR, digital PCR had higher occurrence estimates due to increased sensitivity and dilution of inhibitors at low concentrations. Without accurate LOD correction, species occurrence and detection probabilities based on eDNA estimates are prone to a source of bias that cannot be reduced by an increase in sample size or PCR replicates. Other applications also could benefit from a standardized LOD such as GMO food analysis and forensic and clinical diagnostics. Published 2016. This article is a U.S. Government work and is in the public domain in the USA.

A method for evaluating the performance of computer-aided detection of pulmonary nodules in lung cancer CT screening: detection limit for nodule size and density

PubMed Central

Kobayashi, Hajime; Ohkubo, Masaki; Narita, Akihiro; Marasinghe, Janaka C; Murao, Kohei; Matsumoto, Toru; Sone, Shusuke

2017-01-01

Objective: We propose the application of virtual nodules to evaluate the performance of computer-aided detection (CAD) of lung nodules in cancer screening using low-dose CT. Methods: The virtual nodules were generated based on the spatial resolution measured for a CT system used in an institution providing cancer screening and were fused into clinical lung images obtained at that institution, allowing site specificity. First, we validated virtual nodules as an alternative to artificial nodules inserted into a phantom. In addition, we compared the results of CAD analysis between the real nodules (n = 6) and the corresponding virtual nodules. Subsequently, virtual nodules of various sizes and contrasts between nodule density and background density (ΔCT) were inserted into clinical images (n = 10) and submitted for CAD analysis. Results: In the validation study, 46 of 48 virtual nodules had the same CAD results as artificial nodules (kappa coefficient = 0.913). Real nodules and the corresponding virtual nodules showed the same CAD results. The detection limits of the tested CAD system were determined in terms of size and density of peripheral lung nodules; we demonstrated that a nodule with a 5-mm diameter was detected when the nodule had a ΔCT > 220 HU. Conclusion: Virtual nodules are effective in evaluating CAD performance using site-specific scan/reconstruction conditions. Advances in knowledge: Virtual nodules can be an effective means of evaluating site-specific CAD performance. The methodology for guiding the detection limit for nodule size/density might be a useful evaluation strategy. PMID:27897029

Streak Imaging Flow Cytometer for Rare Cell Analysis.

PubMed

Balsam, Joshua; Bruck, Hugh Alan; Ossandon, Miguel; Prickril, Ben; Rasooly, Avraham

2017-01-01

There is a need for simple and affordable techniques for cytology for clinical applications, especially for point-of-care (POC) medical diagnostics in resource-poor settings. However, this often requires adapting expensive and complex laboratory-based techniques that often require significant power and are too massive to transport easily. One such technique is flow cytometry, which has great potential for modification due to the simplicity of the principle of optical tracking of cells. However, it is limited in that regard due to the flow focusing technique used to isolate cells for optical detection. This technique inherently reduces the flow rate and is therefore unsuitable for rapid detection of rare cells which require large volume for analysis.To address these limitations, we developed a low-cost, mobile flow cytometer based on streak imaging. In our new configuration we utilize a simple webcam for optical detection over a large area associated with a wide-field flow cell. The new flow cell is capable of larger volume and higher throughput fluorescence detection of rare cells than the flow cells with hydrodynamic focusing used in conventional flow cytometry. The webcam is an inexpensive, commercially available system, and for fluorescence analysis we use a 1 W 450 nm blue laser to excite Syto-9 stained cells with emission at 535 nm. We were able to detect low concentrations of stained cells at high flow rates of 10 mL/min, which is suitable for rapidly analyzing larger specimen volumes to detect rare cells at appropriate concentration levels. The new rapid detection capabilities, combined with the simplicity and low cost of this device, suggest a potential for clinical POC flow cytometry in resource-poor settings associated with global health.

Colorimetric sensing of anions in water using ratiometric indicator-displacement assay.

PubMed

Feng, Liang; Li, Hui; Li, Xiao; Chen, Liang; Shen, Zheng; Guan, Yafeng

2012-09-19

The analysis of anions in water presents a difficult challenge due to their low charge-to-radius ratio, and the ability to discriminate among similar anions often remains problematic. The use of a 3×6 ratiometric indicator-displacement assay (RIDA) array for the colorimetric detection and identification of ten anions in water is reported. The sensor array consists of different combinations of colorimetric indicators and metal cations. The colorimetric indicators chelate with metal cations, forming the color changes. Upon the addition of anions, anions compete with the indicator ligands according to solubility product constants (K(sp)). The indicator-metal chelate compound changes color back dramatically when the competition of anions wins. The color changes of the RIDA array were used as a digital representation of the array response and analyzed with standard statistical methods, including principal component analysis and hierarchical clustering analysis. No confusion or errors in classification by hierarchical clustering analysis were observed in 44 trials. The limit of detection was calculated approximately, and most limits of detections of anions are well below μM level using our RIDA array. The pH effect, temperature influence, interfering anions were also investigated, and the RIDA array shows the feasibility of real sample testing. Copyright © 2012 Elsevier B.V. All rights reserved.

Solid phase extraction of large volume of water and beverage samples to improve detection limits for GC-MS analysis of bisphenol A and four other bisphenols.

PubMed

Cao, Xu-Liang; Popovic, Svetlana

2018-01-01

Solid phase extraction (SPE) of large volumes of water and beverage products was investigated for the GC-MS analysis of bisphenol A (BPA), bisphenol AF (BPAF), bisphenol F (BPF), bisphenol E (BPE), and bisphenol B (BPB). While absolute recoveries of the method were improved for water and some beverage products (e.g. diet cola, iced tea), breakthrough may also have occurred during SPE of 200 mL of other beverages (e.g. BPF in cola). Improvements in method detection limits were observed with the analysis of large sample volumes for all bisphenols at ppt (pg/g) to sub-ppt levels. This improvement was found to be proportional to sample volumes for water and beverage products with less interferences and noise levels around the analytes. Matrix effects and interferences were observed during SPE of larger volumes (100 and 200 mL) of the beverage products, and affected the accurate analysis of BPF. This improved method was used to analyse bisphenols in various beverage samples, and only BPA was detected, with levels ranging from 0.022 to 0.030 ng/g for products in PET bottles, and 0.085 to 0.32 ng/g for products in cans.

Silver(I) Ions Ultrasensitive Detection at Carbon Electrodes—Analysis of Waters, Tobacco Cells and Fish Tissues

PubMed Central

Krizkova, Sona; Krystofova, Olga; Trnkova, Libuse; Hubalek, Jaromir; Adam, Vojtech; Beklova, Miroslava; Horna, Ales; Havel, Ladislav; Kizek, Rene

2009-01-01

We used carbon paste electrodes and a standard potentiostat to detect silver ions. The detection limit (3 Signal/Noise ratio) was estimated as 0.5 μM. A standard electrochemical instrument microanalysis of silver(I) ions was suggested. As a working electrode a carbon tip (1 mL) or carbon pencil was used. Limits of detection estimated by dilution of a standard were 1 (carbon tip) or 10 nM (carbon pencil). Further we employed flow injection analysis coupled with carbon tip to detect silver(I) ions released in various beverages and mineral waters. During first, second and third week the amount of silver(I) ions releasing into water samples was under the detection limit of the technique used for their quantification. At the end of a thirteen weeks long experiment the content of silver(I) ions was several times higher compared to the beginning of release detected in the third week and was on the order of tens of nanomoles. In subsequent experiments the influence of silver(I) ions (0, 5 and 10 μM) on a plant model system (tobacco BY-2 cells) during a four-day exposition was investigated. Silver(I) ions were highly toxic to the cells, which was revealed by a double staining viability assay. Moreover we investigated the effect of silver(I) ions (0, 0.3, 0.6, 1.2 and 2.5 μM) on guppies (Poecilia reticulata). Content of Ag(I) increased with increasing time of the treatment and applied concentrations in fish tissues. It can be concluded that a carbon tip or carbon pencil coupled with a miniaturized potentiostat can be used for detection of silver(I) ions in environmental samples and thus represents a small, portable, low cost and easy-to-use instrument for such purposes. PMID:22399980

Phylogenetic Analysis of Bacteroidales 16S rRNA Genes Unveils Sequences Specific to Diverse Swine Fecal Sources

EPA Science Inventory

Two of the currently available methods to assess swine fecal pollution (Bac1 and PF163) target Bacteroidales 16S rRNA genes. However, these assays have been shown to exhibit poor host-specificity and low detection limits in environmental waters, in part due to the limited number...

2D and 3D Terahertz Imaging and X-Rays CT for Sigillography Study

NASA Astrophysics Data System (ADS)

Fabre, M.; Durand, R.; Bassel, L.; Recur, B.; Balacey, H.; Bou Sleiman, J.; Perraud, J.-B.; Mounaix, P.

2017-04-01

Seals are part of our cultural heritage but the study of these objects is limited because of their fragility. Terahertz and X-Ray imaging are used to analyze a collection of wax seals from the fourteenth to eighteenth centuries. In this work, both techniques are compared in order to discuss their advantages and limits and their complementarity for conservation state study of the samples. Thanks to 3D analysis and reconstructions, defects and fractures are detected with an estimation of their depth position. The path from the parchment tongue inside the seals is also detected.

Survival analysis, or what to do with upper limits in astronomical surveys

NASA Technical Reports Server (NTRS)

Isobe, Takashi; Feigelson, Eric D.

1986-01-01

A field of applied statistics called survival analysis has been developed over several decades to deal with censored data, which occur in astronomical surveys when objects are too faint to be detected. How these methods can assist in the statistical interpretation of astronomical data are reviewed.

Trace-Level Automated Mercury Speciation Analysis

PubMed Central

Taylor, Vivien F.; Carter, Annie; Davies, Colin; Jackson, Brian P.

2011-01-01

An automated system for methyl Hg analysis by purge and trap gas chromatography (GC) was evaluated, with comparison of several different instrument configurations including chromatography columns (packed column or capillary), detector (atomic fluorescence, AFS, or inductively coupled plasma mass spectrometry, ICP-MS, using quadrupole and sector field ICP- MS instruments). Method detection limits (MDL) of 0.042 pg and 0.030 pg for CH3Hg+ were achieved with the automated Hg analysis system configured with AFS and ICPMS detection, respectively. Capillary GC with temperature programming was effective in improving resolution and decreasing retention times of heavier Hg species (in this case C3H7Hg+) although carryover between samples was increased. With capillary GC, the MDL for CH3Hg+ was 0.25 pg for AFS detection and 0.060 pg for ICP-MS detection. The automated system was demonstrated to have high throughput (72 samples analyzed in 8 hours) requiring considerably less analyst time than the manual method for methyl mercury analysis described in EPA 1630. PMID:21572543

Sulphur-bearing Compounds Detected by MSL SAM Evolved Gas Analysis of Materials from Yellowknife Bay, Gale Crater, Mars

NASA Technical Reports Server (NTRS)

McAdam, A. C.; Franz, H. B.; Archer, P. D. Jr.; Sutter, B.; Eigenbrode, J. L.; Freissinet, C.; Atreya, S. K.; Bish, D. L.; Blake, D. F.; Brunner, A.;

Detection of incipient defects in cables by partial discharge signal analysis

NASA Astrophysics Data System (ADS)

Martzloff, F. D.; Simmon, E.; Steiner, J. P.; Vanbrunt, R. J.

1992-07-01

As one of the objectives of a program aimed at assessing test methods for in-situ detection of incipient defects in cables due to aging, a laboratory test system was implemented to demonstrate that the partial discharge analysis method can be successfully applied to low-voltage cables. Previous investigations generally involved cables rated 5 kV or higher, while the objective of the program focused on the lower voltages associated with the safety systems of nuclear power plants. The defect detection system implemented for the project was based on commercially available signal analysis hardware and software packages, customized for the specific purposes of the project. The test specimens included several cables of the type found in nuclear power plants, including artificial defects introduced at various points of the cable. The results indicate that indeed, partial discharge analysis is capable of detecting incipient defects in low-voltage cables. There are, however, some limitations of technical and non-technical nature that need further exploration before this method can be accepted in the industry.

Sensing the deadliest toxin: technologies for botulinum neurotoxin detection.

PubMed

Capek, Petr; Dickerson, Tobin J

2010-01-01

Sensitive and rapid detection of botulinum neurotoxins (BoNTs), the most poisonous substances known to date, is essential for studies of medical applications of BoNTs and detection of poisoned food, as well as for response to potential bioterrorist threats. Currently, the most common method of BoNT detection is the mouse bioassay. While this assay is sensitive, it is slow, quite expensive, has limited throughput and requires sacrificing animals. Herein, we discuss and compare recently developed alternative in vitro detection methods and assess their ability to supplement or replace the mouse bioassay in the analysis of complex matrix samples.

Detection of target-probe oligonucleotide hybridization using synthetic nanopore resistive pulse sensing.

PubMed

Booth, Marsilea Adela; Vogel, Robert; Curran, James M; Harbison, SallyAnn; Travas-Sejdic, Jadranka

2013-07-15

Despite the plethora of DNA sensor platforms available, a portable, sensitive, selective and economic sensor able to rival current fluorescence-based techniques would find use in many applications. In this research, probe oligonucleotide-grafted particles are used to detect target DNA in solution through a resistive pulse nanopore detection technique. Using carbodiimide chemistry, functionalized probe DNA strands are attached to carboxylated dextran-based magnetic particles. Subsequent incubation with complementary target DNA yields a change in surface properties as the two DNA strands hybridize. Particle-by-particle analysis with resistive pulse sensing is performed to detect these changes. A variable pressure method allows identification of changes in the surface charge of particles. As proof-of-principle, we demonstrate that target hybridization is selectively detected at micromolar concentrations (nanomoles of target) using resistive pulse sensing, confirmed by fluorescence and phase analysis light scattering as complementary techniques. The advantages, feasibility and limitations of using resistive pulse sensing for sample analysis are discussed. Copyright © 2013 Elsevier B.V. All rights reserved.

Comparing the detection of iron-based pottery pigment on a carbon-coated sherd by SEM-EDS and by Micro-XRF-SEM.

PubMed

Pendleton, Michael W; Washburn, Dorothy K; Ellis, E Ann; Pendleton, Bonnie B

2014-03-01

The same sherd was analyzed using a scanning electron microscope with energy dispersive spectroscopy (SEM-EDS) and a micro X-ray fluorescence tube attached to a scanning electron microscope (Micro-XRF-SEM) to compare the effectiveness of elemental detection of iron-based pigment. To enhance SEM-EDS mapping, the sherd was carbon coated. The carbon coating was not required to produce Micro-XRF-SEM maps but was applied to maintain an unbiased comparison between the systems. The Micro-XRF-SEM analysis was capable of lower limits of detection than that of the SEM-EDS system, and therefore the Micro-XRF-SEM system could produce elemental maps of elements not easily detected by SEM-EDS mapping systems. Because SEM-EDS and Micro-XRF-SEM have been used for imaging and chemical analysis of biological samples, this comparison of the detection systems should be useful to biologists, especially those involved in bone or tooth (hard tissue) analysis.

Comparing the Detection of Iron-Based Pottery Pigment on a Carbon-Coated Sherd by SEM-EDS and by Micro-XRF-SEM

PubMed Central

Pendleton, Michael W.; Washburn, Dorothy K.; Ellis, E. Ann; Pendleton, Bonnie B.

2014-01-01

The same sherd was analyzed using a scanning electron microscope with energy dispersive spectroscopy (SEM-EDS) and a micro X-ray fluorescence tube attached to a scanning electron microscope (Micro-XRF-SEM) to compare the effectiveness of elemental detection of iron-based pigment. To enhance SEM-EDS mapping, the sherd was carbon coated. The carbon coating was not required to produce Micro-XRF-SEM maps but was applied to maintain an unbiased comparison between the systems. The Micro-XRF-SEM analysis was capable of lower limits of detection than that of the SEM-EDS system, and therefore the Micro-XRF-SEM system could produce elemental maps of elements not easily detected by SEM-EDS mapping systems. Because SEM-EDS and Micro-XRF-SEM have been used for imaging and chemical analysis of biological samples, this comparison of the detection systems should be useful to biologists, especially those involved in bone or tooth (hard tissue) analysis. PMID:24600333

Analytical performance of benchtop total reflection X-ray fluorescence instrumentation for multielemental analysis of wine samples

NASA Astrophysics Data System (ADS)

Dalipi, Rogerta; Marguí, Eva; Borgese, Laura; Bilo, Fabjola; Depero, Laura E.

2016-06-01

Recent technological improvements have led to a widespread adoption of benchtop total reflection X-ray fluorescence systems (TXRF) for analysis of liquid samples. However, benchtop TXRF systems usually present limited sensitivity compared with high-scale instrumentation which can restrict its application in some fields. The aim of the present work was to evaluate and compare the analytical capabilities of two TXRF systems, equipped with low power Mo and W target X-ray tubes, for multielemental analysis of wine samples. Using the Mo-TXRF system, the detection limits for most elements were one order of magnitude lower than those attained using the W-TXRF system. For the detection of high Z elements like Cd and Ag, however, W-TXRF remains a very good option due to the possibility of K-Lines detection. Accuracy and precision of the obtained results have been evaluated analyzing spiked real wine samples and comparing the TXRF results with those obtained by inductively coupled plasma emission spectroscopy (ICP-OES). In general, good agreement was obtained between ICP-OES and TXRF results for the analysis of both red and white wine samples except for light elements (i.e., K) which TXRF concentrations were underestimated. However, a further achievement of analytical quality of TXRF results can be achieved if wine analysis is performed after dilution of the sample with de-ionized water.

Validation of a high-performance liquid chromatographic method with UV detection for the determination of ethopabate residues in poultry liver.

PubMed

Granja, Rodrigo H M M; Niño, Alfredo M Montes; Zucchetti, Roberto A M; Niño, Rosario E Montes; Salerno, Alessandro G

2008-01-01

Ethopabate is frequently used in the prophylaxis and treatment of coccidiosis in poultry. Residues of this drug in food present a potential risk to consumers. A simple, rapid, and sensitive column high-performance liquid chromatographic (HPLC) method with UV detection for determination of ethopabate in poultry liver is presented. The drug is extracted with acetonitrile. After evaporation, the residue is dissolved with an acetone-hexane mixture and cleaned up by solid-phase extraction using Florisil columns. The analyte is then eluted with methanol. LC analysis is carried out on a C18 5 microm Gemini column, 15 cm x 4.6 mm. Ethopabate is quantified by means of UV detection at 270 nm. Parameters such as decision limit, detection capability, precision, recovery, ruggedness, and measurement uncertainty were calculated according to method validation guidelines provided in 2002/657/EC and ISO/IEC 17025:2005. Decision limit and detection capability were determined to be 2 and 3 microg/kg, respectively. Average recoveries from poultry samples fortified with 10, 15, and 20 microg/kg levels of ethopabate were 100-105%. A complete statistical analysis was performed on the results obtained, including an estimation of the method uncertainty. The method is to be implemented into Brazil's residue monitoring and control program for ethopabate.

Analysis of PAEs contaminants in water sources for agriculture, industrial and residential areas from local city district

NASA Astrophysics Data System (ADS)

Chen, Qidan; Chen, Qixian; Wu, Fei; Liao, Jia; Zhao, Xi

2018-02-01

The technology of DEHP and DBP detection by high performance liquid chromatography coupled with ultraviolet detection (HPLC-UV) was developed and applied in analysis of local water sources from agriculture, industrial and residential areas. Under the optimized sample pretreatment and detection conditions, DEHP and DBP were well separated and detected in 4 mins. The detection limit of DBP was 0.002 mg/L and DEHP was 0.006 mg/L, and it meets the Chinese National Standard limitations for drinking water quality. The linear correlation coefficient of DBP and DEHP standard calibration curves was 0.9998 and 0.9995. The linear range of DBP was 0.020 mg/L ∼20.0 mg/L, with the standard deviation of 0.560% ∼5.07%, and the linear range of DEHP was 0.060 mg/L ∼15.0 mg/L, with the standard deviation of 0.546% ∼5.74%. Ten water samples from Jinwan district of Zhuhai in Guangdong province of China were analyzed. However, the PAEs amounts found in the water sources from industrial areas were higher than the agriculture and residential areas, industries grow incredibly fast in the district in recently years and more attention should be paid to the increasing risks of water sources pollution.

A capillary electrophoresis chip for the analysis of print and film photographic developing agents in commercial processing solutions using indirect fluorescence detection.

PubMed

Sirichai, S; de Mello, A J

2001-01-01

The separation and detection of both print and film developing agents (CD-3 and CD-4) in photographic processing solutions using chip-based capillary electrophoresis is presented. For simultaneous detection of both analytes under identical experimental conditions a buffer pH of 11.9 is used to partially ionise the analytes. Detection is made possible by indirect fluorescence, where the ions of the analytes displace the anionic fluorescing buffer ion to create negative peaks. Under optimal conditions, both analytes can be analyzed within 30 s. The limits of detection for CD-3 and CD-4 are 0.17 mM and 0.39 mM, respectively. The applicability of the method for the analysis of seasoned photographic processing developer solutions is also examined.

LAMP-based group specific detection of aflatoxin producers within Aspergillus section Flavi in food raw materials, spices, and dried fruit using neutral red for visible-light signal detection.

PubMed

Niessen, Ludwig; Bechtner, Julia; Fodil, Sihem; Taniwaki, Marta H; Vogel, Rudi F

2018-02-02

Aflatoxins can be produced by 21 species within sections Flavi (16 species), Ochraceorosei (2), and Nidulantes (3) of the fungal genus Aspergillus. They pose risks to human and animal health due to high toxicity and carcinogenicity. Detecting aflatoxin producers can help to assess toxicological risks associated with contaminated commodities. Species specific molecular assays (PCR and LAMP) are available for detection of major producers, but fail to detect species of minor importance. To enable rapid and sensitive detection of several aflatoxin producing species in a single analysis, a nor1 gene-specific LAMP assay was developed. Specificity testing showed that among 128 fungal species from 28 genera, 15 aflatoxigenic species in section Flavi were detected, including synonyms of A. flavus and A. parasiticus. No cross reactions were found with other tested species. The detection limit of the assay was 9.03pg of A. parasiticus genomic DNA per reaction. Visual detection of positive LAMP reactions under daylight conditions was facilitated using neutral red to allow unambiguous distinction between positive and negative assay results. Application of the assay to the detection of A. parasiticus conidia revealed a detection limit of 211 conidia per reaction after minimal sample preparation. The usefulness of the assay was demonstrated in the analysis of aflatoxinogenic species in samples of rice, nuts, raisins, dried figs, as well as powdered spices. Comparison of LAMP results with presence/absence of aflatoxins and aflatoxin producing fungi in 50 rice samples showed good correlation between these parameters. Our study suggests that the developed LAMP assay is a rapid, sensitive and user-friendly tool for surveillance and quality control in our food industry. Copyright © 2017 Elsevier B.V. All rights reserved.

Ultrahigh-Sensitivity Piezoresistive Pressure Sensors for Detection of Tiny Pressure.

PubMed

Li, Hongwei; Wu, Kunjie; Xu, Zeyang; Wang, Zhongwu; Meng, Yancheng; Li, Liqiang

2018-06-20

High-sensitivity pressure sensors are crucial for the ultrasensitive touch technology and E-skin, especially at the tiny-pressure range below 100 Pa. However, it is highly challenging to substantially promote sensitivity beyond the current level at several to 200 kPa -1 and to improve the detection limit lower than 0.1 Pa, which is significant for the development of pressure sensors toward ultrasensitive and highly precise detection. Here, we develop an efficient strategy to greatly improve the sensitivity near to 2000 kPa -1 using short-channel coplanar device structure and sharp microstructure, which is systematically proposed for the first time and rationalized by the mathematic calculation and analysis. Significantly, benefiting from the ultrahigh sensitivity, the detection limit is improved to be as small as 0.075 Pa. The sensitivity and detection limit are both superior to the current levels and far surpass the function of human skin. Furthermore, the sensor shows fast response time (50 μs), excellent reproducibility and stability, and low power consumption. Remarkably, the sensor shows excellent detection capacity in the tiny-pressure range, including light-emitting diode switching with a pressure of 7 Pa, ringtone (2-20 Pa) recognition, and ultrasensitive (0.1 Pa) electronic glove. This work represents a performance and strategic progress in the field of pressure sensing.

Immunostimulatory oligonucleotide-induced metaphase cytogenetics detect chromosomal aberrations in 80% of CLL patients: A study of 132 CLL cases with correlation to FISH, IgVH status, and CD38 expression.

PubMed

Dicker, Frank; Schnittger, Susanne; Haferlach, Torsten; Kern, Wolfgang; Schoch, Claudia

2006-11-01

Compared with fluorescence in situ hybridization (FISH), conventional metaphase cytogenetics play only a minor prognostic role in chronic lymphocytic leukemia (CLL) so far, due to technical problems resulting from limited proliferation of CLL cells in vitro. Here, we present a simple method for in vitro stimulation of CLL cells that overcomes this limitation. In our unselected patient population, 125 of 132 cases could be successfully stimulated for metaphase generation by culture with the immunostimulatory CpG-oligonucleotide DSP30 plus interleukin 2. Of 125 cases, 101 showed chromosomal aberrations. The aberration rate is comparable to the rate detected by parallel interphase FISH. In 47 patients, conventional cytogenetics detected additional aberrations not detected by FISH analysis. A complex aberrant karyotype, defined as one having at least 3 aberrations, was detected in 30 of 125 patients, compared with only one such case as defined by FISH. Conventional cytogenetics frequently detected balanced and unbalanced translocations. A significant correlation of the poor-prognosis unmutated IgV(H) status with unbalanced translocations and of the likewise poor-prognosis CD38 expression to balanced translocations and complex aberrant karyotype was found. We demonstrate that FISH analysis underestimates the complexity of chromosomal aberrations in CLL. Therefore, conventional cytogenetics may define subgroups of patients with high risk of progression.

Maximizing the Biochemical Resolving Power of Fluorescence Microscopy

PubMed Central

Esposito, Alessandro; Popleteeva, Marina; Venkitaraman, Ashok R.

2013-01-01

Most recent advances in fluorescence microscopy have focused on achieving spatial resolutions below the diffraction limit. However, the inherent capability of fluorescence microscopy to non-invasively resolve different biochemical or physical environments in biological samples has not yet been formally described, because an adequate and general theoretical framework is lacking. Here, we develop a mathematical characterization of the biochemical resolution in fluorescence detection with Fisher information analysis. To improve the precision and the resolution of quantitative imaging methods, we demonstrate strategies for the optimization of fluorescence lifetime, fluorescence anisotropy and hyperspectral detection, as well as different multi-dimensional techniques. We describe optimized imaging protocols, provide optimization algorithms and describe precision and resolving power in biochemical imaging thanks to the analysis of the general properties of Fisher information in fluorescence detection. These strategies enable the optimal use of the information content available within the limited photon-budget typically available in fluorescence microscopy. This theoretical foundation leads to a generalized strategy for the optimization of multi-dimensional optical detection, and demonstrates how the parallel detection of all properties of fluorescence can maximize the biochemical resolving power of fluorescence microscopy, an approach we term Hyper Dimensional Imaging Microscopy (HDIM). Our work provides a theoretical framework for the description of the biochemical resolution in fluorescence microscopy, irrespective of spatial resolution, and for the development of a new class of microscopes that exploit multi-parametric detection systems. PMID:24204821

Analysis of Anions in Ambient Aerosols by Microchip Capillary Electrophoresis

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

Liu, Yan; MacDonald, David A.; Yu, Xiao-Ying

2006-10-01

We describe a microchip capillary electrophoresis method for the analysis of nitrate and sulfate in ambient aerosols. Investigating the chemical composition of ambient aerosol particles is essential for understanding their sources and effects. Significant progress has been made towards developing mass spectrometry-based instrumentation for rapid qualitative analysis of aerosols. Alternative methods for rapid quantification of selected high abundance compounds are needed to augment the capacity for widespread routine analysis. Such methods could provide much higher temporal and spatial resolution than can be achieved currently. Inorganic anions comprise a large percentage of particulate mass with nitrate and sulfate among the mostmore » abundant species. While ion chromatography has proven very useful for analyzing extracts of time-integrated ambient aerosol samples collected on filters and for semi-continuous, on-line particle composition measurements, there is a growing need for development of new compact, inexpensive approaches to routine on-line aerosol ion analysis for deployment in spatially dense, atmospheric measurement networks. Microchip capillary electrophoresis provides the necessary speed and portability to address this need. In this report, on-column contact conductivity detection is used with hydrodynamic injection to create a simple microchip instrument for analysis of nitrate and sulfate. On-column contact conductivity detection was achieved using a Pd decoupler placed upstream from the working electrodes. Microchips containing two Au or Pd working electrodes showed a good linear range (5-500 µM) and low limits-of-detection for sulfate and nitrate with Au providing the lowest detection limits (1 µM) for both ions. The completed microchip system was used to analyze ambient aerosol filter samples. Nitrate and sulfate concentrations measured by the microchip matched the concentrations measured by ion chromatography.« less

Comparative Genomic Hybridization–Array Analysis Enhances the Detection of Aneuploidies and Submicroscopic Imbalances in Spontaneous Miscarriages

PubMed Central

Schaeffer, Anthony J. ; Chung, June ; Heretis, Konstantina ; Wong, Andrew ; Ledbetter, David H. ; Lese Martin, Christa 

2004-01-01

Miscarriage is a condition that affects 10%–15% of all clinically recognized pregnancies, most of which occur in the first trimester. Approximately 50% of first-trimester miscarriages result from fetal chromosome abnormalities. Currently, G-banded chromosome analysis is used to determine if large-scale genetic imbalances are the cause of these pregnancy losses. This technique relies on the culture of cells derived from the fetus, a technique that has many limitations, including a high rate of culture failure, maternal overgrowth of fetal cells, and poor chromosome morphology. Comparative genomic hybridization (CGH)–array analysis is a powerful new molecular cytogenetic technique that allows genomewide analysis of DNA copy number. By hybridizing patient DNA and normal reference DNA to arrays of genomic clones, unbalanced gains or losses of genetic material across the genome can be detected. In this study, 41 product-of-conception (POC) samples, which were previously analyzed by G-banding, were tested using CGH arrays to determine not only if the array could identify all reported abnormalities, but also whether any previously undetected genomic imbalances would be discovered. The array methodology detected all abnormalities as reported by G-banding analysis and revealed new abnormalities in 4/41 (9.8%) cases. Of those, one trisomy 21 POC was also mosaic for trisomy 20, one had a duplication of the 10q telomere region, one had an interstitial deletion of chromosome 9p, and the fourth had an interstitial duplication of the Prader-Willi/Angelman syndrome region on chromosome 15q, which, if maternally inherited, has been implicated in autism. This retrospective study demonstrates that the DNA-based CGH-array technology overcomes many of the limitations of routine cytogenetic analysis of POC samples while enhancing the detection of fetal chromosome aberrations. PMID:15127362

Analytical requirements, perspectives and limits of immunological methods for drugs in hair.

PubMed

Cassani, M; Spiehler, V

1993-12-01

The analytical requirements for analysis of drugs in hair are sensitivity in the range of picograms per milligram of hair, specificity for lipophilic drugs and absence of matrix effects with hair digests. These requirements are met by immunoassays which are also inexpensive, rapid and easy to use. However, in applying immunoassays to hair testing, certain limitations of the assay and of interpretation of assay results should be kept in perspective. These limitations are illustrated in this review with examples of the analysis of opiates in hair from patients and opiate addicts. The first requirement for immunological analysis of hair digests is that the digest must not denature the antibody proteins of the immunoassay reagents. For this reason enzymatic digests are better for immunological assay than chemical digests. Strongly acidic or alkaline digests must be brought to a neutral pH before immunoassay. Immunoassays used for analysis of hair should be calibrated with spiked hair digest standards to correct for possible matrix effects. The second requirement is that the immunoassay have the sensitivity and specificity to detect the drug in hair. Drugs of abuse are found in hair in the range of 10 pg-10 ng/mg hair. Radioimmunoassays are capable of detection and quantitation in this concentration range. Although the mechanism of drug incorporation into hair is not known, it is now apparent that primarily the parent drug and lipophilic metabolites are found in hair. For example, the ratio of cocaine/benzoylecgonine averages 10 (range 2-50) in published reports of analysis of hair from cocaine users. Therefore, immunoassays which are highly sensitive for the parent drug are required and results of immunoassays should be expressed as equivalents. When spiking standards for calibration of hair digest immunoassays, parent drug known to be present in hair should be used, e.g. cocaine not benzoylecgonine. With immunoassays which are specific for the lipophilic metabolite found in hair such as 6-MAM, differential radioimmunoassay can be used to discriminate between medical and illicit sources for the opiate drugs found in hair. Because of the low concentrations of drugs encountered in hair, immunoassays for hair have been used at cutoff concentrations at their limits of detection. The limit of detection (LOD) has been determined by calculating the mean and standard deviation (S.D.) for the assay response for a number of negative hair samples. The cutoff was then set at a distance of 2, 3, or 5 S.D.s from the mean response.(ABSTRACT TRUNCATED AT 400 WORDS)

CMOS-MEMS Chemiresistive and Chemicapacitive Chemical Sensor System

NASA Astrophysics Data System (ADS)

Lazarus, Nathan S.

Integrating chemical sensors with testing electronics is a powerful technique with the potential to lower power and cost and allow for lower system limits of detection. This thesis explores the possibility of creating an integrated sensor system intended to be embedded within respirator cartridges to notify the user that hazardous chemicals will soon leak into the face mask. For a chemical sensor designer, this application is particularly challenging due to the need for a very sensitive and cheap sensor that will be exposed to widely varying environmental conditions during use. An octanethiol-coated gold nanoparticle chemiresistor to detect industrial solvents is developed, focusing on characterizing the environmental stability and limits of detection of the sensor. Since the chemiresistor was found to be highly sensitive to water vapor, a series of highly sensitive humidity sensor topologies were developed, with sensitivities several times previous integrated capacitive humidity sensors achieved. Circuit techniques were then explored to reduce the humidity sensor limits of detection, including the analysis of noise, charge injection, jitter and clock feedthrough in a charge-based capacitance measurement (CBCM) circuit and the design of a low noise Colpitts LC oscillator. The characterization of high resistance gold nanoclusters for capacitive chemical sensing was also performed. In the final section, a preconcentrator, a heater element intended to release a brief concentrated pulse of analate, was developed and tested for the purposes of lowering the system limit of detection.

Detection and Resolution of Cryptosporidium Species and Species Mixtures by Genus-Specific Nested PCR-Restriction Fragment Length Polymorphism Analysis, Direct Sequencing, and Cloning ▿

PubMed Central

Ruecker, Norma J.; Hoffman, Rebecca M.; Chalmers, Rachel M.; Neumann, Norman F.

2011-01-01

Molecular methods incorporating nested PCR-restriction fragment length polymorphism (RFLP) analysis of the 18S rRNA gene of Cryptosporidium species were validated to assess performance based on limit of detection (LoD) and for detecting and resolving mixtures of species and genotypes within a single sample. The 95% LoD was determined for seven species (Cryptosporidium hominis, C. parvum, C. felis, C. meleagridis, C. ubiquitum, C. muris, and C. andersoni) and ranged from 7 to 11 plasmid template copies with overlapping 95% confidence limits. The LoD values for genomic DNA from oocysts on microscope slides were 7 and 10 template copies for C. andersoni and C. parvum, respectively. The repetitive nested PCR-RFLP slide protocol had an LoD of 4 oocysts per slide. When templates of two species were mixed in equal ratios in the nested PCR-RFLP reaction mixture, there was no amplification bias toward one species over another. At high ratios of template mixtures (>1:10), there was a reduction or loss of detection of the less abundant species by RFLP analysis, most likely due to heteroduplex formation in the later cycles of the PCR. Replicate nested PCR was successful at resolving many mixtures of Cryptosporidium at template concentrations near or below the LoD. The cloning of nested PCR products resulted in 17% of the cloned sequences being recombinants of the two original templates. Limiting-dilution nested PCR followed by the sequencing of PCR products resulted in no sequence anomalies, suggesting that this method is an effective and accurate way to study the species diversity of Cryptosporidium, particularly for environmental water samples, in which mixtures of parasites are common. PMID:21498746

Combination of electrochemical biosensor and textile threads: A microfluidic device for phenol determination in tap water.

PubMed

Caetano, F R; Carneiro, E A; Agustini, D; Figueiredo-Filho, L C S; Banks, C E; Bergamini, M F; Marcolino-Junior, L H

2018-01-15

Microfluidic devices constructed using low cost materials presents as alternative for conventional flow analysis systems because they provide advantages as low consumption of reagents and samples, high speed of analysis, possibility of portability and the easiness of construction and maintenance. Herein, is described for the first time the use of an electrochemical biosensor for phenol detection combined with a very simple and efficient microfluidic device based on commercial textile threads. Taking advantages of capillary phenomena and gravity forces, the solution transportation is promoted without any external forces or injection pump. Screen printed electrodes were modified with carbon nanotubes/gold nanoparticles followed by covalent binding of tyrosinase. After the biosensor electrochemical characterization by cyclic voltammetry technique, the optimization of relevant parameters such as pH, potential of detection and linear range for the biosensor performance was carried out; the system was evaluated for analytical phenol detection presenting limit of detection and limit of quantification 2.94nmolL -1 and 8.92nmolL -1 respectively. The proposed system was applied on phenol addition and recovery studies in drinking water, obtaining recoveries rates between 90% and 110%. Copyright © 2017 Elsevier B.V. All rights reserved.

Organochlorine pesticide residues in strawberries from integrated pest management and organic farming.

PubMed

Fernandes, Virginia C; Domingues, Valentina F; Mateus, Nuno; Delerue-Matos, Cristina

2011-07-27

A rapid, specific, and sensitive method based on the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) method and a cleanup using dispersive solid-phase extraction with MgSO(4), PSA, and C18 sorbents has been developed for the routine analysis of 14 pesticides in strawberries. The analyses were performed by three different analytical methodologies: gas chromatography (GC) with electron capture detection (ECD), mass spectrometry (MS), and tandem mass spectrometry (MS/MS). The recoveries for all the pesticides studied were from 46 to 128%, with relative standard deviation of <15% in the concentration range of 0.005-0.250 mg/kg. The limit of detection (LOD) for all compounds met maximum residue limits (MRL) accepted in Portugal for organochlorine pesticides (OCP). A survey study of strawberries produced in Portugal in the years 2009-2010 obtained from organic farming (OF) and integrated pest management (IPM) was developed. Lindane and β-endosulfan were detected above the MRL in OF and IPM. Other OCP (aldrin, o,p'-DDT and their metabolites, and methoxychlor) were found below the MRL. The OCP residues detected decreased from 2009 to 2010. The QuEChERS method was successfully applied to the analysis of strawberry samples.

Tacholess order-tracking approach for wind turbine gearbox fault detection

NASA Astrophysics Data System (ADS)

Wang, Yi; Xie, Yong; Xu, Guanghua; Zhang, Sicong; Hou, Chenggang

2017-09-01

Monitoring of wind turbines under variable-speed operating conditions has become an important issue in recent years. The gearbox of a wind turbine is the most important transmission unit; it generally exhibits complex vibration signatures due to random variations in operating conditions. Spectral analysis is one of the main approaches in vibration signal processing. However, spectral analysis is based on a stationary assumption and thus inapplicable to the fault diagnosis of wind turbines under variable-speed operating conditions. This constraint limits the application of spectral analysis to wind turbine diagnosis in industrial applications. Although order-tracking methods have been proposed for wind turbine fault detection in recent years, current methods are only applicable to cases in which the instantaneous shaft phase is available. For wind turbines with limited structural spaces, collecting phase signals with tachometers or encoders is difficult. In this study, a tacholess order-tracking method for wind turbines is proposed to overcome the limitations of traditional techniques. The proposed method extracts the instantaneous phase from the vibration signal, resamples the signal at equiangular increments, and calculates the order spectrum for wind turbine fault identification. The effectiveness of the proposed method is experimentally validated with the vibration signals of wind turbines.

Digital PCR Improves Mutation Analysis in Pancreas Fine Needle Aspiration Biopsy Specimens.

PubMed

Sho, Shonan; Court, Colin M; Kim, Stephen; Braxton, David R; Hou, Shuang; Muthusamy, V Raman; Watson, Rabindra R; Sedarat, Alireza; Tseng, Hsian-Rong; Tomlinson, James S

2017-01-01

Applications of precision oncology strategies rely on accurate tumor genotyping from clinically available specimens. Fine needle aspirations (FNA) are frequently obtained in cancer management and often represent the only source of tumor tissues for patients with metastatic or locally advanced diseases. However, FNAs obtained from pancreas ductal adenocarcinoma (PDAC) are often limited in cellularity and/or tumor cell purity, precluding accurate tumor genotyping in many cases. Digital PCR (dPCR) is a technology with exceptional sensitivity and low DNA template requirement, characteristics that are necessary for analyzing PDAC FNA samples. In the current study, we sought to evaluate dPCR as a mutation analysis tool for pancreas FNA specimens. To this end, we analyzed alterations in the KRAS gene in pancreas FNAs using dPCR. The sensitivity of dPCR mutation analysis was first determined using serial dilution cell spiking studies. Single-cell laser-microdissection (LMD) was then utilized to identify the minimal number of tumor cells needed for mutation detection. Lastly, dPCR mutation analysis was performed on 44 pancreas FNAs (34 formalin-fixed paraffin-embedded (FFPE) and 10 fresh (non-fixed)), including samples highly limited in cellularity (100 cells) and tumor cell purity (1%). We found dPCR to detect mutations with allele frequencies as low as 0.17%. Additionally, a single tumor cell could be detected within an abundance of normal cells. Using clinical FNA samples, dPCR mutation analysis was successful in all preoperative FNA biopsies tested, and its accuracy was confirmed via comparison with resected tumor specimens. Moreover, dPCR revealed additional KRAS mutations representing minor subclones within a tumor that were not detected by the current clinical gold standard method of Sanger sequencing. In conclusion, dPCR performs sensitive and accurate mutation analysis in pancreas FNAs, detecting not only the dominant mutation subtype, but also the additional rare mutation subtypes representing tumor heterogeneity.

Digital PCR Improves Mutation Analysis in Pancreas Fine Needle Aspiration Biopsy Specimens

PubMed Central

Court, Colin M.; Kim, Stephen; Braxton, David R.; Hou, Shuang; Muthusamy, V. Raman; Watson, Rabindra R.; Sedarat, Alireza; Tseng, Hsian-Rong; Tomlinson, James S.

2017-01-01

Applications of precision oncology strategies rely on accurate tumor genotyping from clinically available specimens. Fine needle aspirations (FNA) are frequently obtained in cancer management and often represent the only source of tumor tissues for patients with metastatic or locally advanced diseases. However, FNAs obtained from pancreas ductal adenocarcinoma (PDAC) are often limited in cellularity and/or tumor cell purity, precluding accurate tumor genotyping in many cases. Digital PCR (dPCR) is a technology with exceptional sensitivity and low DNA template requirement, characteristics that are necessary for analyzing PDAC FNA samples. In the current study, we sought to evaluate dPCR as a mutation analysis tool for pancreas FNA specimens. To this end, we analyzed alterations in the KRAS gene in pancreas FNAs using dPCR. The sensitivity of dPCR mutation analysis was first determined using serial dilution cell spiking studies. Single-cell laser-microdissection (LMD) was then utilized to identify the minimal number of tumor cells needed for mutation detection. Lastly, dPCR mutation analysis was performed on 44 pancreas FNAs (34 formalin-fixed paraffin-embedded (FFPE) and 10 fresh (non-fixed)), including samples highly limited in cellularity (100 cells) and tumor cell purity (1%). We found dPCR to detect mutations with allele frequencies as low as 0.17%. Additionally, a single tumor cell could be detected within an abundance of normal cells. Using clinical FNA samples, dPCR mutation analysis was successful in all preoperative FNA biopsies tested, and its accuracy was confirmed via comparison with resected tumor specimens. Moreover, dPCR revealed additional KRAS mutations representing minor subclones within a tumor that were not detected by the current clinical gold standard method of Sanger sequencing. In conclusion, dPCR performs sensitive and accurate mutation analysis in pancreas FNAs, detecting not only the dominant mutation subtype, but also the additional rare mutation subtypes representing tumor heterogeneity. PMID:28125707

Singular value decomposition metrics show limitations of detector design in diffuse fluorescence tomography

PubMed Central

Leblond, Frederic; Tichauer, Kenneth M.; Pogue, Brian W.

2010-01-01

The spatial resolution and recovered contrast of images reconstructed from diffuse fluorescence tomography data are limited by the high scattering properties of light propagation in biological tissue. As a result, the image reconstruction process can be exceedingly vulnerable to inaccurate prior knowledge of tissue optical properties and stochastic noise. In light of these limitations, the optimal source-detector geometry for a fluorescence tomography system is non-trivial, requiring analytical methods to guide design. Analysis of the singular value decomposition of the matrix to be inverted for image reconstruction is one potential approach, providing key quantitative metrics, such as singular image mode spatial resolution and singular data mode frequency as a function of singular mode. In the present study, these metrics are used to analyze the effects of different sources of noise and model errors as related to image quality in the form of spatial resolution and contrast recovery. The image quality is demonstrated to be inherently noise-limited even when detection geometries were increased in complexity to allow maximal tissue sampling, suggesting that detection noise characteristics outweigh detection geometry for achieving optimal reconstructions. PMID:21258566

Capillary ion chromatography with on-column focusing for ultra-trace analysis of methanesulfonate and inorganic anions in limited volume Antarctic ice core samples.

PubMed

Rodriguez, Estrella Sanz; Poynter, Sam; Curran, Mark; Haddad, Paul R; Shellie, Robert A; Nesterenko, Pavel N; Paull, Brett

2015-08-28

Preservation of ionic species within Antarctic ice yields a unique proxy record of the Earth's climate history. Studies have been focused until now on two proxies: the ionic components of sea salt aerosol and methanesulfonic acid. Measurement of the all of the major ionic species in ice core samples is typically carried out by ion chromatography. Former methods, whilst providing suitable detection limits, have been based upon off-column preconcentration techniques, requiring larger sample volumes, with potential for sample contamination and/or carryover. Here, a new capillary ion chromatography based analytical method has been developed for quantitative analysis of limited volume Antarctic ice core samples. The developed analytical protocol applies capillary ion chromatography (with suppressed conductivity detection) and direct on-column sample injection and focusing, thus eliminating the requirement for off-column sample preconcentration. This limits the total sample volume needed to 300μL per analysis, allowing for triplicate sample analysis with <1mL of sample. This new approach provides a reliable and robust analytical method for the simultaneous determination of organic and inorganic anions, including fluoride, methanesulfonate, chloride, sulfate and nitrate anions. Application to composite ice-core samples is demonstrated, with coupling of the capillary ion chromatograph to high resolution mass spectrometry used to confirm the presence and purity of the observed methanesulfonate peak. Copyright © 2015 Elsevier B.V. All rights reserved.

Enantioselective determination of the organochlorine pesticide bromocyclen in spiked fish tissue using solid-phase microextraction coupled to gas chromatography with ECD and ICP-MS detection.

PubMed

Fidalgo-Used, Natalia; Montes-Bayón, Maria; Blanco-González, Elisa; Sanz-Medel, Alfredo

2008-05-15

A method for enantioselective determination of bromocyclen enantiomers in fish tissue has been developed. The enantiomers were resolved by capillary gas chromatography (GC) using a commercial chiral column (CP-Chirasil-Dex CB) and a temperature program from 50 degrees C (held for 1 min), raised to 140 degrees C at 40 degrees C min(-1) and then raised at 0.2 degrees C min(-1) to 155 degrees C. This enantioselective gas chromatographic separation was combined with a clean-up/enrichment procedure based on solid-phase microextraction (SPME). Under SPME optimized conditions, precision, linearity range and detection limits of the developed SPME-enantioselective GC procedure were evaluated and compared using two different detection systems: a classical electron-capture detection (ECD) and an element specific detection using inductively coupled plasma mass spectrometry (ICP-MS). The SPME-GC-ECD method exhibited an excellent sensitivity, with detection limits of 0.2 ng L(-1) for each enantiomer of bromocyclen. Although ICP-MS offered poorer detection limits (7 ng L(-1) as Br, equivalent to 36 ng L(-1) of each enantiomer) than conventional ECD detector, it proved to be clearly superior in terms of selectivity. The relative potential and performance of the two compared methods for real-life analysis has been illustrated by the determination of enantiomers of bromocyclen in spiked tissue extracts of trout.

The detection and analysis of point processes in biological signals

NASA Technical Reports Server (NTRS)

Anderson, D. J.; Correia, M. J.

1977-01-01

A pragmatic approach to the detection and analysis of discrete events in biomedical signals is taken. Examples from both clinical and basic research are provided. Introductory sections discuss not only discrete events which are easily extracted from recordings by conventional threshold detectors but also events embedded in other information carrying signals. The primary considerations are factors governing event-time resolution and the effects limits to this resolution have on the subsequent analysis of the underlying process. The analysis portion describes tests for qualifying the records as stationary point processes and procedures for providing meaningful information about the biological signals under investigation. All of these procedures are designed to be implemented on laboratory computers of modest computational capacity.

Analysis of variation in oil pressure in lubricating system

NASA Astrophysics Data System (ADS)

Sharma, Sumit; Upreti, Mritunjay; Sharma, Bharat; Poddar, Keshav

2018-05-01

Automotive Maintenance for an engine contributes to its reliability, energy efficiency and repair cost reduction. Modeling of engine performance and fault detection require large amount of data, which are usually obtained on test benches. This report presents a methodical study on analysis of variation in lubrication system of various medium speed engines. Further this study is limited to the influence of Engine Oil Pressure on frictional losses, Torque analysis for various Oil Pressures and an analytical analysis of engine Lubrication System. The data collected from various Engines under diagnostics is represented graphically. Finally the illustrated results were used as a viable source for detection and troubleshooting of faults in Lubrication System of regular passenger vehicle.

Supercritical fluid chromatography with photodiode array detection for pesticide analysis in papaya and avocado samples.

PubMed

Pano-Farias, Norma S; Ceballos-Magaña, Silvia G; Gonzalez, Jorge; Jurado, José M; Muñiz-Valencia, Roberto

2015-04-01

To improve the analysis of pesticides in complex food matrices with economic importance, alternative chromatographic techniques, such as supercritical fluid chromatography, can be used. Supercritical fluid chromatography has barely been applied for pesticide analysis in food matrices. In this paper, an analytical method using supercritical fluid chromatography coupled to a photodiode array detection has been established for the first time for the quantification of pesticides in papaya and avocado. The extraction of methyl parathion, atrazine, ametryn, carbofuran, and carbaryl was performed through the quick, easy, cheap, effective, rugged, and safe methodology. The method was validated using papaya and avocado samples. For papaya, the correlation coefficient values were higher than 0.99; limits of detection and quantification ranged from 130-380 and 220-640 μg/kg, respectively; recovery values ranged from 72.8-94.6%; precision was lower than 3%. For avocado, limit of detection values were ˂450 μg/kg; precision was lower than 11%; recoveries ranged from 50.0-94.2%. Method feasibility was tested for lime, banana, mango, and melon samples. Our results demonstrate that the proposed method is applicable to methyl parathion, atrazine, ametryn, and carbaryl, toxics pesticides used worldwide. The methodology presented in this work could be applicable to other fruits. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

From Musical Detectives to DJs: Expanding Aural Skills and Analysis through Engaging Popular Music and Culture

ERIC Educational Resources Information Center

Tobias, Evan S.

2015-01-01

Many music educators address aural skills and analysis by drawing on strategies designed for the realm of Western classical music. Focusing solely on aural skills and analysis within paradigms of Western music can limit students' musical learning and engagement to particular ways of knowing music. To diversify and broaden the types of aural skills…

Hyphenation of ultra performance liquid chromatography (UPLC) with inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of bromine containing preservatives.

PubMed

Bendahl, Lars; Hansen, Steen Honoré; Gammelgaard, Bente; Sturup, Stefan; Nielsen, Camilla

2006-02-24

Ultra performance liquid chromatography (UPLC) was coupled to inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of three bromine-containing preservatives, monitoring the 79Br and 81Br isotopes simultaneously. Due to the efficiency of the 1.7 microm column packing material, the resolution of the test substances was only slightly affected when the linear flow velocity was increased from 0.5 to 1.9 mm s(-1). However, the sensitivity of ICP-MS detection decreased when the linear flow velocity was increased from 0.5 to 1.9 mm s(-1). Analytical figures of merit were determined at an intermediate and at a high linear velocity. The precision was better than 2.2% R.S.D. and regression analysis showed that a linear response was achieved at both flow rates (R2 > 0.9993, n = 36). The analysis time was less than 4.5 min at a flow rate of 50 microL min(-1) and limits of detection and quantification were better than 3.3 and 11 microg BrL(-1), respectively. The analysis time was reduced to 2.7 min when the flow rate was increased to 90 microL min(-1) and limits of detection and quantification were better than 20 and 65 microg BrL(-1), respectively. The method was applied for quantitative analysis of bromine-containing preservatives in commercially available cosmetic products.

A compact in vivo neutron activation analysis system to quantify manganese in human hand bone

NASA Astrophysics Data System (ADS)

Liu, Yingzi

As an urgent issue of correlating cumulative manganese (Mn) exposure to neurotoxicity, bone has emerged as an attractive biomarker for long-term Mn deposition and storage. A novel Deuterium-Deuterium (DD) neutron generator irradiation system has been simulated and constructed, incorporating moderator, reflector and shielding. This neutron activation analysis (NAA) irradiation assembly presents several desirable features, including high neutron flux, improved detection limit and acceptable neutron & photon dose, which would allow it be ready for clinical measurement. Key steps include simulation modeling and verifying, irradiation system design, detector characterization, and neutron flux and dose assessment. Activation foils were also analyzed to reveal the accurate neutron spectrum in the irradiation cave. The detection limit with this system is 0.428 ppm with 36 mSv equivalent hand dose and 52 microSv whole body effective dose.

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

Gorham, P. W.; Allison, P.; Hebert, C. L.

We report initial results of the first flight of the Antarctic Impulsive Transient Antenna (ANITA-1) 2006-2007 Long Duration Balloon flight, which searched for evidence of a diffuse flux of cosmic neutrinos above energies of E{sub {nu}}{approx_equal}3x10{sup 18} eV. ANITA-1 flew for 35 days looking for radio impulses due to the Askaryan effect in neutrino-induced electromagnetic showers within the Antarctic ice sheets. We report here on our initial analysis, which was performed as a blind search of the data. No neutrino candidates are seen, with no detected physics background. We set model-independent limits based on this result. Upper limits derived frommore » our analysis rule out the highest cosmogenic neutrino models. In a background horizontal-polarization channel, we also detect six events consistent with radio impulses from ultrahigh energy extensive air showers.« less

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

Gorham, P.W.; Allison, P.; /Hawaii U.

We report initial results of the first flight of the Antarctic Impulsive Transient Antenna (ANITA-1) 2006-2007 Long Duration Balloon flight, which searched for evidence of a diffuse flux of cosmic neutrinos above energies of E{sub v} = 3 x 10{sup 18} eV. ANITA-1 flew for 35 days looking for radio impulses due to the Askaryan effect in neutrino-induced electromagnetic showers within the Antarctic ice sheets. We report here on our initial analysis, which was performed as a blind search of the data. No neutrino candidates are seen, with no detected physics background. We set model-independent limits based on this result.more » Upper limits derived from our analysis rule out the highest cosmogenic neutrino models. In a background horizontal-polarization channel, we also detect six events consistent with radio impulses from ultrahigh energy extensive air showers.« less

Determination of benzo[a]pyrene in edible oils using phase-transfer-catalyst-assisted saponification and supramolecular solvent microextraction coupled to HPLC with fluorescence detection.

PubMed

Wang, Jin; Liu, Laping; Shi, Ludi; Yi, Tingquan; Wen, Yuxia; Wang, Juanli; Liu, Shuhui

2017-01-01

For the analysis of edible oils, saponification is well known as a useful method for eliminating oil matrices. The conventional approach is conducted with alcoholic alkali; it consumes a large volume of organic solvents and impedes the retrieval of analytes by microextraction. In this study, a low-organic-solvent-consuming method has been developed for the analysis of benzo[a]pyrene in edible oils by high-performance liquid chromatography with fluorescence detection. Sample treatment involves aqueous alkaline saponification, assisted by a phase-transfer catalyst, and selective in situ extraction of the analyte with a supramolecular solvent. Comparison of the chromatograms of the oil extracts obtained by different microextraction methods showed that the supramolecular solvent has a better clean-up effect for the unsaponifiable matter from oil matrices. The method offered excellent linearity over a range of 0.03- 5.0 ng mL -1 (r > 0.999). Recovery rates varied from 94 to 102% (RSDs <5.0%). The detection limit and quantification limit were 0.06 and 0.19 μg kg -1 , respectively. The proposed method was applied for the analysis of 52 edible oils collected online in China; the analyte contents of 23 tested oil samples exceeded the maximum limit of 2 μg kg -1 for benzo[a]pyrene set by the Commission Regulation of the European Union. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A New Method for the Fast Analysis of Trihalomethanes in Tap and Recycled Waters Using Headspace Gas Chromatography with Micro-Electron Capture Detection

PubMed Central

Alexandrou, Lydon D.; Meehan, Barry J.; Morrison, Paul D.; Jones, Oliver A. H.

2017-01-01

Chemical disinfection of water supplies brings significant public health benefits by reducing microbial contamination. The process can however, result in the formation of toxic compounds through interactions between disinfectants and organic material in the source water. These new compounds are termed disinfection by-products (DBPs). The most common are the trihalomethanes (THMs) such as trichloromethane (chloroform), dichlorobromomethane, chlorodibromomethane and tribromomethane (bromoform); these are commonly reported as a single value for total trihalomethanes (TTHMs). Analysis of DBPs is commonly performed via time- and solvent-intensive sample preparation techniques such as liquid–liquid and solid phase extraction. In this study, a method using headspace gas chromatography with micro-electron capture detection was developed and applied for the analysis of THMs in drinking and recycled waters from across Melbourne (Victoria, Australia). The method allowed almost complete removal of the sample preparation step whilst maintaining trace level detection limits (>1 ppb). All drinking water samples had TTHM concentrations below the Australian regulatory limit of 250 µg/L but some were above the U.S. EPA limit of 60 µg/L. The highest TTHM concentration was 67.2 µg/L and lowest 22.9 µg/L. For recycled water, samples taken directly from treatment plants held significantly higher concentrations (153.2 µg/L TTHM) compared to samples from final use locations (4.9–9.3 µg/L). PMID:28505068

Multi-analysis determination of tropane alkaloids in cereals and solanaceaes seeds by liquid chromatography coupled to single stage Exactive-Orbitrap.

PubMed

Marín-Sáez, Jesús; Romero-González, Roberto; Garrido Frenich, Antonia

2017-10-06

Tropane alkaloids are a wide group of substances that comprises more than 200 compounds occurring especially in the Solanaceae family. The main aim of this study is the development of a method for the analysis of the principal tropane alkaloids as atropine, scopolamine, anisodamine, tropane, tropine, littorine, homatropine, apoatropine, aposcopolamine, scopoline, tropinone, physoperuvine, pseudotropine and cuscohygrine in cereals and related matrices. For that, a simple solid-liquid extraction was optimized and a liquid chromatographic method coupled to a single stage Exactive-Orbitrap was developed. The method was validated obtaining recoveries in the range of 60-109% (except for some compounds in soy), precision values (expressed as relative standard deviation) lower than 20% and detection and quantification limits equal to or lower than 2 and 3μg/kg respectively. Finally, the method was applied to the analysis of different types of samples as buckwheat, linseed, soy and millet, obtaining positives for anisodamine, scopolamine, atropine, littorine and tropinone in a millet flour sample above the quantification limits, whereas atropine and scopolamine were detected in a buckwheat sample, below the quantification limit. Contaminated samples with Solanaceaes seeds (Datura Stramonium and Brugmansia Arborea) were also analysed, detecting concentrations up to 693μg/kg (scopolamine) for contaminated samples with Brugmansia seeds and 1847μg/kg (atropine) when samples were contaminated with Stramonium seeds. Copyright © 2017 Elsevier B.V. All rights reserved.

Evolution and Advances in Satellite Analysis of Volcanoes

NASA Astrophysics Data System (ADS)

Dean, K. G.; Dehn, J.; Webley, P.; Bailey, J.

2008-12-01

Over the past 20 years satellite data used for monitoring and analysis of volcanic eruptions has evolved in terms of timeliness, access, distribution, resolution and understanding of volcanic processes. Initially satellite data was used for retrospective analysis but has evolved to proactive monitoring systems. Timely acquisition of data and the capability to distribute large data files paralleled advances in computer technology and was a critical component for near real-time monitoring. The sharing of these data and resulting discussions has improved our understanding of eruption processes and, even more importantly, their impact on society. To illustrate this evolution, critical scientific discoveries will be highlighted, including detection of airborne ash and sulfur dioxide, cloud-height estimates, prediction of ash cloud movement, and detection of thermal anomalies as precursor-signals to eruptions. AVO has been a leader in implementing many of these advances into an operational setting such as, automated eruption detection, database analysis systems, and remotely accessible web-based analysis systems. Finally, limitations resulting from trade-offs between resolution and how they impact some weakness in detection techniques and hazard assessments will be presented.

An Optoelectronic Nose for Detection of Toxic Gases

PubMed Central

Lim, Sung H.; Feng, Liang; Kemling, Jonathan W.; Musto, Christopher J.; Suslick, Kenneth S.

2009-01-01

We have developed a simple colorimetric sensor array (CSA) for the detection of a wide range of volatile analytes and applied it to the detection of toxic gases. The sensor consists of a disposable array of cross-responsive nanoporous pigments whose colors are changed by diverse chemical interactions with analytes. Although no single chemically responsive pigment is specific for any one analyte, the pattern of color change for the array is a unique molecular fingerprint. Clear differentiation among 19 different toxic industrial chemicals (TICs) within two minutes of exposure at IDLH (immediately dangerous to life or health) concentration has been demonstrated. Quantification of each analyte is easily accomplished based on the color change of the array, and excellent detection limits have been demonstrated, generally below the PELs (permissible exposure limits). Identification of the TICs was readily achieved using a standard chemometric approach, i.e., hierarchical clustering analysis (HCA), with no misclassifications over 140 trials. PMID:20160982

Determination of aldehydes and ketones using derivatization with 2,4-dinitrophenylhydrazine and liquid chromatography-atmospheric pressure photoionization-mass spectrometry.

PubMed

van Leeuwen, Suze M; Hendriksen, Laurens; Karst, Uwe

2004-11-26

Atmospheric pressure photoionization-mass spectrometry (APPI-MS) is used for the analysis of aldehydes and ketones after derivatization with 2,4-dinitrophenylhydrazine (DNPH) and liquid chromatographic separation. In the negative ion mode, the [M - H]- pseudomolecular ions are most abundant for the carbonyls. Compared with the established atmospheric pressure chemical ionization (APCI)-MS, limits of detection are typically lower using similar conditions. Automobile exhaust and cigarette exhaust samples were analyzed with APPI-MS and APCI-MS in combination with an ion trap mass analyzer. Due to improved limits of detection, more of the less abundant long-chain carbonyls are detected with APPI-MS in real samples. While 2,4-dinitrophenylazide, a known reaction product of DNPH with nitrogen dioxide, is detected in APCI-MS due to dissociative electron capture, it is not observed at all in APPI-MS.

Automated detection of diabetic retinopathy: barriers to translation into clinical practice.

PubMed

Abramoff, Michael D; Niemeijer, Meindert; Russell, Stephen R

2010-03-01

Automated identification of diabetic retinopathy (DR), the primary cause of blindness and visual loss for those aged 18-65 years, from color images of the retina has enormous potential to increase the quality, cost-effectiveness and accessibility of preventative care for people with diabetes. Through advanced image analysis techniques, retinal images are analyzed for abnormalities that define and correlate with the severity of DR. Translating automated DR detection into clinical practice will require surmounting scientific and nonscientific barriers. Scientific concerns, such as DR detection limits compared with human experts, can be studied and measured. Ethical, legal and political issues can be addressed, but are difficult or impossible to measure. The primary objective of this review is to survey the methods, potential benefits and limitations of automated detection in order to better manage translation into clinical practice, based on extensive experience with the systems we have developed.

Competitive immunoassay of phenobarbital by microchip electrophoresis with laser induced fluorescence detection.

PubMed

Huang, Yong; Zhao, Shulin; Shi, Ming; Liu, Jinwen; Liang, Hong

2011-05-23

A microchip electrophoresis method with laser induced fluorescence detection was developed for the immunoassay of phenobarbital. The detection was based on the competitive immunoreaction between analyte phenobarbital and fluorescein isothiocyanate (FITC) labeled phenobarbital with a limited amount of antibody. The assay was developed by varying the borate concentration, buffer pH, separation voltage, and incubation time. A running buffer system containing 35 mM borate and 15 mM sodium dodecyl sulfate (pH 9.5), and 2800 V separation voltage provided analysis conditions for a high-resolution, sensitive, and repeatable assay of phenobarbital. Free FITC-labeled phenobarbital and immunocomplex were separated within 30s. The calibration curve for phenobarbital had a detection limit of 3.4 nM and a range of 8.6-860.0 nM. The assay could be used to determine the phenobarbital plasma concentration in clinical plasma sample. Copyright © 2011 Elsevier B.V. All rights reserved.

An optoelectronic nose for the detection of toxic gases.

PubMed

Lim, Sung H; Feng, Liang; Kemling, Jonathan W; Musto, Christopher J; Suslick, Kenneth S

2009-10-01

We have developed a simple colorimetric sensor array that detects a wide range of volatile analytes and then applied it to the detection of toxic gases. The sensor consists of a disposable array of cross-responsive nanoporous pigments with colours that are changed by diverse chemical interactions with analytes. Although no single chemically responsive pigment is specific for any one analyte, the pattern of colour change for the array is a unique molecular fingerprint. Clear differentiation among 19 different toxic industrial chemicals (TICs) within two minutes of exposure at concentrations immediately dangerous to life or health were demonstrated. Based on the colour change of the array, quantification of each analyte was accomplished easily, and excellent detection limits were achieved, generally below the permissible exposure limits. Different TICs were identified readily using a standard chemometric approach (hierarchical clustering analysis), with no misclassifications over 140 trials.

Topological characterization and early detection of bifurcations and chaos in complex systems using persistent homology.

PubMed

Mittal, Khushboo; Gupta, Shalabh

2017-05-01

Early detection of bifurcations and chaos and understanding their topological characteristics are essential for safe and reliable operation of various electrical, chemical, physical, and industrial processes. However, the presence of non-linearity and high-dimensionality in system behavior makes this analysis a challenging task. The existing methods for dynamical system analysis provide useful tools for anomaly detection (e.g., Bendixson-Dulac and Poincare-Bendixson criteria can detect the presence of limit cycles); however, they do not provide a detailed topological understanding about system evolution during bifurcations and chaos, such as the changes in the number of subcycles and their positions, lifetimes, and sizes. This paper addresses this research gap by using topological data analysis as a tool to study system evolution and develop a mathematical framework for detecting the topological changes in the underlying system using persistent homology. Using the proposed technique, topological features (e.g., number of relevant k-dimensional holes, etc.) are extracted from nonlinear time series data which are useful for deeper analysis of the system behavior and early detection of bifurcations and chaos. When applied to a Logistic map, a Duffing oscillator, and a real life Op-amp based Jerk circuit, these features are shown to accurately characterize the system dynamics and detect the onset of chaos.

Combining markers with and without the limit of detection

PubMed Central

Dong, Ting; Liu, Catherine Chunling; Petricoin, Emanuel F.; Tang, Liansheng Larry

2014-01-01

In this paper, we consider the combination of markers with and without the limit of detection (LOD). LOD is often encountered when measuring proteomic markers. Because of the limited detecting ability of an equipment or instrument, it is difficult to measure markers at a relatively low level. Suppose that after some monotonic transformation, the marker values approximately follow multivariate normal distributions. We propose to estimate distribution parameters while taking the LOD into account, and then combine markers using the results from the linear discriminant analysis. Our simulation results show that the ROC curve parameter estimates generated from the proposed method are much closer to the truth than simply using the linear discriminant analysis to combine markers without considering the LOD. In addition, we propose a procedure to select and combine a subset of markers when many candidate markers are available. The procedure based on the correlation among markers is different from a common understanding that a subset of the most accurate markers should be selected for the combination. The simulation studies show that the accuracy of a combined marker can be largely impacted by the correlation of marker measurements. Our methods are applied to a protein pathway dataset to combine proteomic biomarkers to distinguish cancer patients from non-cancer patients. PMID:24132938

Trace-level screening of dichlorophenols in processed dairy milk by headspace gas chromatography.

PubMed

Gras, Kaelyn; Luong, Jim; Gras, Ronda; Shellie, Robert A

2016-10-01

A headspace gas chromatographic approach based on flame ionization detection has been successfully developed for the determination of parts-per-billion levels of 2,4-dichlorophenol and 2,6-dichlorophenol in processed dairy milk. Under the right environmental conditions, these compounds are produced as products of the reductive dechlorination of pentachlorophenol. Maintaining a highly inert chromatographic system and employing a recently commercialized inert capillary column permits the analysis of 2,4-dichlorophenol and 2,6-dichlorophenol without derivatization. Further, a detection limit improvement of more than a factor of two was achieved by adding sodium sulfate to substantially decrease the solute partition coefficient in the matrix. A detection limit of 1 ng/g and a limit of quantitation of 2 ng/g were attained, and complete analysis can be conducted in < 13 min. Reproducibility of area counts over a range from 20 to 200 ng/g and over a period of 2 days were found to be less than 6% (n = 20). A linear range from 5 to 500 ng/g with a correlation coefficient of at least 0.9992 was obtained for 2,4-dichlorophenol and 2,6-dichlorophenol. Spike recoveries from 10 to 500 ng/g for all the analytes range from 92 to 102%. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Lab on a Chip

NASA Astrophysics Data System (ADS)

Puget, P.

The reliable and fast detection of chemical or biological molecules, or the measurement of their concentrations in a sample, are key problems in many fields such as environmental analysis, medical diagnosis, or the food industry. There are traditionally two approaches to this problem. The first aims to carry out a measurement in situ in the sample using chemical and biological sensors. The constraints imposed by detection limits, specificity, and in some cases stability are entirely imputed to the sensor. The second approach uses so-called total analysis systems to process the sample according to a protocol made up of different steps, such as extractions, purifications, concentrations, and a final detection stage. The latter is made in better conditions than with the first approach, which may justify the greater complexity of the process. It is this approach that is implemented in most methods for identifying pathogens, whether they be in biological samples (especially for in vitro diagnosis) or samples taken from the environment. The instrumentation traditionally used to carry out these protocols comprises a set of bulky benchtop apparatus, which needs to be plugged into the mains in order to function. However, there are many specific applications (to be discussed in this chapter) for which analysis instruments with the following characteristics are needed: Possibility of use outside the laboratory, i.e., instruments as small as possible, consuming little energy, and largely insensitive to external conditions of temperature, humidity, vibrations, and so on. Possibility of use by non-specialised agents, or even unmanned operation. Possibility of handling a large number of samples in a limited time, typically for high-throughput screening applications. Possibility of handling small samples. At the same time, a high level of performance is required, in particular in terms of (1) the detection limit, which must be as low as possible, (2) specificity, i.e., the ability to detect a particular molecule in a complex mixture, and (3) speed.

Background estimation and player detection in badminton video clips using histogram of pixel values along temporal dimension

NASA Astrophysics Data System (ADS)

Peng, Yahui; Ma, Xiao; Gao, Xinyu; Zhou, Fangxu

2015-12-01

Computer vision is an important tool for sports video processing. However, its application in badminton match analysis is very limited. In this study, we proposed a straightforward but robust histogram-based background estimation and player detection methods for badminton video clips, and compared the results with the naive averaging method and the mixture of Gaussians methods, respectively. The proposed method yielded better background estimation results than the naive averaging method and more accurate player detection results than the mixture of Gaussians player detection method. The preliminary results indicated that the proposed histogram-based method could estimate the background and extract the players accurately. We conclude that the proposed method can be used for badminton player tracking and further studies are warranted for automated match analysis.

Analysis of genetically modified organisms by pyrosequencing on a portable photodiode-based bioluminescence sequencer.

PubMed

Song, Qinxin; Wei, Guijiang; Zhou, Guohua

2014-07-01

A portable bioluminescence analyser for detecting the DNA sequence of genetically modified organisms (GMOs) was developed by using a photodiode (PD) array. Pyrosequencing on eight genes (zSSIIb, Bt11 and Bt176 gene of genetically modified maize; Lectin, 35S-CTP4, CP4EPSPS, CaMV35S promoter and NOS terminator of the genetically modified Roundup ready soya) was successfully detected with this instrument. The corresponding limit of detection (LOD) was 0.01% with 35 PCR cycles. The maize and soya available from three different provenances in China were detected. The results indicate that pyrosequencing using the small size of the detector is a simple, inexpensive, and reliable way in a farm/field test of GMO analysis. Copyright © 2014 Elsevier Ltd. All rights reserved.

Implications of the Fermi-LAT Pass 8 Galactic Center excess on supersymmetric dark matter

NASA Astrophysics Data System (ADS)

Achterberg, Abraham; van Beekveld, Melissa; Caron, Sascha; Gómez-Vargas, Germán A.; Hendriks, Luc; Ruiz de Austri, Roberto

2017-12-01

The Fermi Collaboration has recently updated their analysis of gamma rays from the center of the Galaxy. They reconfirm the presence of an unexplained emission feature which is most prominent in the region of 1–10 GeV, known as the Galactic Center GeV excess (GCE). Although the GCE is now firmly detected, an interpretation of this emission as a signal of self-annihilating dark matter (DM) particles is not unambiguously possible due to systematic effects in the gamma-ray modeling estimated in the Galactic Plane. In this paper we build a covariance matrix, collecting different systematic uncertainties investigated in the Fermi Collaboration's paper that affect the GCE spectrum. We show that models where part of the GCE is due to annihilating DM is still consistent with the new data. We also re-evaluate the parameter space regions of the minimal supersymmetric Standard Model (MSSM) that can contribute dominantly to the GCE via neutralino DM annihilation. All recent constraints from DM direct detection experiments such as PICO, LUX, PandaX and Xenon1T, limits on the annihilation cross section from dwarf spheroidal galaxies and the Large Hadron Collider limits are considered in this analysis. Due to a slight shift in the energy spectrum of the GC excess with respect to the previous Fermi analysis, and the recent limits from direct detection experiments, we find a slightly shifted parameter region of the MSSM, compared to our previous analysis, that is consistent with the GCE. Neutralinos with a mass between 85–220 GeV can describe the excess via annihilation into a pair of W-bosons or top quarks. Remarkably, there are models with low fine-tuning among the regions that we have found. The complete set of solutions will be probed by upcoming direct detection experiments and with dedicated searches in the upcoming data of the Large Hadron Collider.

Urine analysis concerning xenon for doping control purposes.

PubMed

Thevis, Mario; Piper, Thomas; Geyer, Hans; Schaefer, Maximilian S; Schneemann, Julia; Kienbaum, Peter; Schänzer, Wilhelm

2015-01-15

On September 1(st) 2014, a modified Prohibited List as established by the World Anti-Doping Agency (WADA) became effective featuring xenon as a banned substance categorized as hypoxia-inducible factor (HIF) activator. Consequently, the analysis of xenon from commonly provided doping control specimens such as blood and urine is desirable, and first data on the determination of xenon from urine in the context of human sports drug testing, are presented. In accordance to earlier studies utilizing plasma as doping control matrix, urine was enriched to saturation with xenon, sequentially diluted, and the target analyte was detected as supported by the internal standard d6 -cyclohexanone by means of gas chromatography/triple quadrupole mass spectrometry (GC/MS/MS) using headspace injection. Three major xenon isotopes at m/z 128.9, 130.9 and 131.9 were targeted in (pseudo) selected reaction monitoring mode enabling the unambiguous identification of the prohibited substance. Assay characteristics including limit of detection (LOD), intraday/interday precision, and specificity as well as analyte recovery under different storage conditions were determined. Proof-of-concept data were generated by applying the established method to urine samples collected from five patients before, during and after (up to 48 h) xenon-based general anesthesia. Xenon was traceable in enriched human urine samples down to the detection limit of approximately 0.5 nmol/mL. The intraday and interday imprecision values of the method were found below 25%, and specificity was demonstrated by analyzing 20 different blank urine samples that corroborated the fitness-for-purpose of the analytical approach to unequivocally detect xenon at non-physiological concentrations in human urine. The patients' urine specimens returned 'xenon-positive' test results up to 40 h post-anesthesia, indicating the limits of the expected doping control detection window. Since xenon has been considered a prohibited substance according to WADA regulations in September 2014, its analysis from common specimens of routine sports drug testing is desirable. In previous studies, its traceability in whole blood and plasma was shown, and herein a complementary approach utilizing doping control urine samples for the GC/MS/MS analysis of xenon was reported. Copyright © 2014 John Wiley & Sons, Ltd.

Detection of chlorinated and brominated byproducts of drinking water disinfection using electrospray ionization-high-field asymmetric waveform ion mobility spectrometry-mass spectrometry.

PubMed

Ells, B; Barnett, D A; Froese, K; Purves, R W; Hrudey, S; Guevremont, R

1999-10-15

The lower limit of detection for low molecular weight polar and ionic analytes using electrospray ionization-mass spectrometry (ESI-MS) is often severely compromised by an intense background that obscures ions of trace components in solution. Recently, a new technique, referred to as high-field asymmetric waveform ion mobility spectrometry (FAIMS), has been shown to separate gas-phase ions at atmospheric pressure and room temperature. A FAIMS instrument is an ion filter that may be tuned, by control of electrical voltages, to continuously transmit selected ions from a complex mixture. This capability offers significant advantages when FAIMS is coupled with ESI, a source that generates a wide variety of ions, including solvent clusters and salt adducts. In this report, the tandem arrangement of ESI-FAIMS-MS is used for the analysis of haloacetic acids, a class of disinfection byproducts regulated by the US EPA. FAIMS is shown to effectively discriminate against background ions resulting from the electrospray of tap water solutions containing the haloacetic acids. Consequently, mass spectra are simplified, the selectivity of the method is improved, and the limits of detection are lowered compared with conventional ESI-MS. The detection limits of ESI-FAIMS-MS for six haloacetic acids ranged between 0.5 and 4 ng/mL in 9:1 methanol/tap water (5 and 40 ng/mL in the original tap water samples) with no preconcentration, derivatization, or chromatographic separation prior to analysis.

Breath analysis using external cavity diode lasers: a review

NASA Astrophysics Data System (ADS)

Bayrakli, Ismail

2017-04-01

Most techniques that are used for diagnosis and therapy of diseases are invasive. Reliable noninvasive methods are always needed for the comfort of patients. Owing to its noninvasiveness, ease of use, and easy repeatability, exhaled breath analysis is a very good candidate for this purpose. Breath analysis can be performed using different techniques, such as gas chromatography mass spectrometry (MS), proton transfer reaction-MS, and selected ion flow tube-MS. However, these devices are bulky and require complicated procedures for sample collection and preconcentration. Therefore, these are not practical for routine applications in hospitals. Laser-based techniques with small size, robustness, low cost, low response time, accuracy, precision, high sensitivity, selectivity, low detection limit, real-time, and point-of-care detection have a great potential for routine use in hospitals. In this review paper, the recent advances in the fields of external cavity lasers and breath analysis for detection of diseases are presented.

Sensitive and inexpensive digital DNA analysis by microfluidic enrichment of rolling circle amplified single-molecules

PubMed Central

Kühnemund, Malte; Hernández-Neuta, Iván; Sharif, Mohd Istiaq; Cornaglia, Matteo; Gijs, Martin A.M.

2017-01-01

Abstract Single molecule quantification assays provide the ultimate sensitivity and precision for molecular analysis. However, most digital analysis techniques, i.e. droplet PCR, require sophisticated and expensive instrumentation for molecule compartmentalization, amplification and analysis. Rolling circle amplification (RCA) provides a simpler means for digital analysis. Nevertheless, the sensitivity of RCA assays has until now been limited by inefficient detection methods. We have developed a simple microfluidic strategy for enrichment of RCA products into a single field of view of a low magnification fluorescent sensor, enabling ultra-sensitive digital quantification of nucleic acids over a dynamic range from 1.2 aM to 190 fM. We prove the broad applicability of our analysis platform by demonstrating 5-plex detection of as little as ∼1 pg (∼300 genome copies) of pathogenic DNA with simultaneous antibiotic resistance marker detection, and the analysis of rare oncogene mutations. Our method is simpler, more cost-effective and faster than other digital analysis techniques and provides the means to implement digital analysis in any laboratory equipped with a standard fluorescent microscope. PMID:28077562

Determination of some aldehydes by using solid-phase microextraction and high-performance liquid chromatography with UV detection.

PubMed

Kumar, Ashwini; Singh, Baldev; Malik, Ashok Kumar; Tiwary, Dhananjay K

2007-01-01

A new approach has been developed for the extraction and determination of aldehydes such as veratraldehyde, m-nitrobenzaldehyde, cinnamaldehyde, benzaldehyde, and p-chlorobenzaldehyde by using solid-phase microextraction (SPME) and high-performance liquid chromatography with UV detection (HPLC/UV). The method involves adsorption of the aldehydes on polydimethylsiloxane/divinylbenzene-coated fiber, followed by desorption in the desorption chamber of the SPME-HPLC interface, using acetonitrile-water (70 + 30) as the mobile phase; UV detection was at 254 nm. A good separation of 5 aldehydes was obtained on a C18 column. The detection limits of veratraldehyde, m-nitrobenzaldehyde, cinnamaldehyde, benzaldehyde, and p-chlorobenzaldehyde are 25, 41, 13, 12, and 11 pg/mL, respectively, which are about 100 times better than the detection limits for other SPME methods using gas chromatography. The proposed method was validated by determining benzaldehyde in bitter almonds and cinnamaldehyde in cinnamon bark. The recoveries of the 5 analytes were determined by analysis of spiked drinking water.

Signal averaging limitations in heterodyne- and direct-detection laser remote sensing measurements

NASA Technical Reports Server (NTRS)

Menyuk, N.; Killinger, D. K.; Menyuk, C. R.

1983-01-01

The improvement in measurement uncertainty brought about by the averaging of increasing numbers of pulse return signals in both heterodyne- and direct-detection lidar systems is investigated. A theoretical analysis is presented which shows the standard deviation of the mean measurement to decrease as the inverse square root of the number of measurements, except in the presence of temporal correlation. Experimental measurements based on a dual-hybrid-TEA CO2 laser differential absorption lidar system are reported which demonstrate that the actual reduction in the standard deviation of the mean in both heterodyne- and direct-detection systems is much slower than the inverse square-root dependence predicted for uncorrelated signals, but is in agreement with predictions in the event of temporal correlation. Results thus favor the use of direct detection at relatively short range where the lower limit of the standard deviation of the mean is about 2 percent, but advantages of heterodyne detection at longer ranges are noted.

Early Oscillation Detection for Hybrid DC/DC Converter Fault Diagnosis

NASA Technical Reports Server (NTRS)

Wang, Bright L.

2011-01-01

This paper describes a novel fault detection technique for hybrid DC/DC converter oscillation diagnosis. The technique is based on principles of feedback control loop oscillation and RF signal modulations, and Is realized by using signal spectral analysis. Real-circuit simulation and analytical study reveal critical factors of the oscillation and indicate significant correlations between the spectral analysis method and the gain/phase margin method. A stability diagnosis index (SDI) is developed as a quantitative measure to accurately assign a degree of stability to the DC/DC converter. This technique Is capable of detecting oscillation at an early stage without interfering with DC/DC converter's normal operation and without limitations of probing to the converter.

Bienzymatic Biosensor for Rapid Detection of Aspartame by Flow Injection Analysis

PubMed Central

Radulescu, Maria-Cristina; Bucur, Bogdan; Bucur, Madalina-Petruta; Radu, Gabriel Lucian

2014-01-01

A rapid, simple and stable biosensor for aspartame detection was developed. Alcohol oxidase (AOX), carboxyl esterase (CaE) and bovine serum albumin (BSA) were immobilised with glutaraldehyde (GA) onto screen-printed electrodes modified with cobalt-phthalocyanine (CoPC). The biosensor response was fast. The sample throughput using a flow injection analysis (FIA) system was 40 h−1 with an RSD of 2.7%. The detection limits for both batch and FIA measurements were 0.1 μM for methanol and 0.2 μM for aspartame, respectively. The enzymatic biosensor was successfully applied for aspartame determination in different sample matrices/commercial products (liquid and solid samples) without any pre-treatment step prior to measurement. PMID:24412899

Bienzymatic biosensor for rapid detection of aspartame by flow injection analysis.

PubMed

Radulescu, Maria-Cristina; Bucur, Bogdan; Bucur, Madalina-Petruta; Radu, Gabriel Lucian

2014-01-09

A rapid, simple and stable biosensor for aspartame detection was developed. Alcohol oxidase (AOX), carboxyl esterase (CaE) and bovine serum albumin (BSA) were immobilised with glutaraldehyde (GA) onto screen-printed electrodes modified with cobalt-phthalocyanine (CoPC). The biosensor response was fast. The sample throughput using a flow injection analysis (FIA) system was 40 h⁻¹ with an RSD of 2.7%. The detection limits for both batch and FIA measurements were 0.1 µM for methanol and 0.2 µM for aspartame, respectively. The enzymatic biosensor was successfully applied for aspartame determination in different sample matrices/commercial products (liquid and solid samples) without any pre-treatment step prior to measurement.

Method and apparatus for concentrating vapors for analysis

DOEpatents

Grate, Jay W [West Richland, WA; Baldwin, David L [Kennewick, WA; Anheier, Jr., Norman C.

2012-06-05

A pre-concentration device and a method are disclosed for concentrating gaseous vapors for analysis. Vapors sorbed and concentrated within the bed of the pre-concentration device are thermally desorbed, achieving at least partial separation of the vapor mixtures. The pre-concentration device is suitable, e.g., for pre-concentration and sample injection, and provides greater resolution of peaks for vapors within vapor mixtures, yielding detection levels that are 10-10,000 times better than direct sampling and analysis systems. Features are particularly useful for continuous unattended monitoring applications. The invention finds application in conjunction with, e.g., analytical instruments where low detection limits for gaseous vapors are desirable.

Analysis of carbendazim, benomyl, thiophanate methyl and 2,4-dichlorophenoxyacetic acid in fruits and vegetables after supercritical fluid extraction.

PubMed

Anastassiades, M; Schwack, W

1998-10-30

Simple methods for the analysis of carbendazim, benomyl and thiophanate methyl in fruits and vegetables and of 2,4-D in citrus fruits are presented. Sample preparation involves supercritical fluid extraction with carbon dioxide and further analysis is performed without any additional clean-up by GC-MS after derivatisation or directly by HPLC-diode array detection. The SFE methods presented are clearly faster and more cost effective than traditional solvent based approaches. The recoveries, detection limits and repeatabilities achieved, meet the needs of tolerance level monitoring of these compounds in fruits and vegetables.

Quantitative analysis of trace levels of surface contamination by X-ray photoelectron spectroscopy Part I: statistical uncertainty near the detection limit.

PubMed

Hill, Shannon B; Faradzhev, Nadir S; Powell, Cedric J

2017-12-01

We discuss the problem of quantifying common sources of statistical uncertainties for analyses of trace levels of surface contamination using X-ray photoelectron spectroscopy. We examine the propagation of error for peak-area measurements using common forms of linear and polynomial background subtraction including the correlation of points used to determine both background and peak areas. This correlation has been neglected in previous analyses, but we show that it contributes significantly to the peak-area uncertainty near the detection limit. We introduce the concept of relative background subtraction variance (RBSV) which quantifies the uncertainty introduced by the method of background determination relative to the uncertainty of the background area itself. The uncertainties of the peak area and atomic concentration and of the detection limit are expressed using the RBSV, which separates the contributions from the acquisition parameters, the background-determination method, and the properties of the measured spectrum. These results are then combined to find acquisition strategies that minimize the total measurement time needed to achieve a desired detection limit or atomic-percentage uncertainty for a particular trace element. Minimization of data-acquisition time is important for samples that are sensitive to x-ray dose and also for laboratories that need to optimize throughput.

Simplified RP-HPLC method for multi-residue analysis of abamectin, emamectin benzoate and ivermectin in rice.

PubMed

Xie, Xianchuan; Gong, Shu; Wang, Xiaorong; Wu, Yinxing; Zhao, Li

2011-01-01

A rapid, reliable and sensitive reverse-phase high-performance liquid chromatography method with fluorescence detection (RP-FLD-HPLC) was developed and validated for simultaneous analysis of the abamectin (ABA), emamectin (EMA) benzoate and ivermectin (IVM) residues in rice. After extraction with acetonitrile/water (2 : 1) with sonication, the avermectin (AVMs) residues were directly derivatised by N-methylimidazole (N-NMIM) and trifluoroacetic anhydride (TFAA) and then analysed on RP-FLD-HPLC. A good linear relationship (r(2 )> 0.99) was obtained for three AVMs ranging from 0.01 to 5 microg ml(-1), i.e. 0.01-5.0 microg g(-1) in rice matrix. The limit of detection (LOD) and the limit of quantification (LOQ) were between 0.001 and 0.002 microg g(-1) and between 0.004 and 0.006 microg g(-1), respectively. Recoveries were from 81.9% to 105.4% and precision less than 12.4%. The proposed method was successfully applied to routine analysis of the AVMs residues in rice.

Development and Validation of an HPLC Method for Karanjin in Pongamia pinnata linn. Leaves.

PubMed

Katekhaye, S; Kale, M S; Laddha, K S

2012-01-01

A rapid, simple and specific reversed-phase HPLC method has been developed for analysis of karanjin in Pongamia pinnata Linn. leaves. HPLC analysis was performed on a C(18) column using an 85:13.5:1.5 (v/v) mixtures of methanol, water and acetic acid as isocratic mobile phase at a flow rate of 1 ml/min. UV detection was at 300 nm. The method was validated for accuracy, precision, linearity, specificity. Validation revealed the method is specific, accurate, precise, reliable and reproducible. Good linear correlation coefficients (r(2)>0.997) were obtained for calibration plots in the ranges tested. Limit of detection was 4.35 μg and limit of quantification was 16.56 μg. Intra and inter-day RSD of retention times and peak areas was less than 1.24% and recovery was between 95.05 and 101.05%. The established HPLC method is appropriate enabling efficient quantitative analysis of karanjin in Pongamia pinnata leaves.

Development and Validation of an HPLC Method for Karanjin in Pongamia pinnata linn. Leaves

PubMed Central

Katekhaye, S; Kale, M. S.; Laddha, K. S.

2012-01-01

A rapid, simple and specific reversed-phase HPLC method has been developed for analysis of karanjin in Pongamia pinnata Linn. leaves. HPLC analysis was performed on a C18 column using an 85:13.5:1.5 (v/v) mixtures of methanol, water and acetic acid as isocratic mobile phase at a flow rate of 1 ml/min. UV detection was at 300 nm. The method was validated for accuracy, precision, linearity, specificity. Validation revealed the method is specific, accurate, precise, reliable and reproducible. Good linear correlation coefficients (r2>0.997) were obtained for calibration plots in the ranges tested. Limit of detection was 4.35 μg and limit of quantification was 16.56 μg. Intra and inter-day RSD of retention times and peak areas was less than 1.24% and recovery was between 95.05 and 101.05%. The established HPLC method is appropriate enabling efficient quantitative analysis of karanjin in Pongamia pinnata leaves. PMID:23204626

Advances in ultrasensitive mass spectrometry of organic molecules.

PubMed

Kandiah, Mathivathani; Urban, Pawel L

2013-06-21

Ultrasensitive mass spectrometric analysis of organic molecules is important for various branches of chemistry, and other fields including physics, earth and environmental sciences, archaeology, biomedicine, and materials science. It finds applications--as an enabling tool--in systems biology, biological imaging, clinical analysis, and forensics. Although there are a number of technical obstacles associated with the analysis of samples by mass spectrometry at ultratrace level (for example analyte losses during sample preparation, insufficient sensitivity, ion suppression), several noteworthy developments have been made over the years. They include: sensitive ion sources, loss-free interfaces, ion optics components, efficient mass analyzers and detectors, as well as "smart" sample preparation strategies. Some of the mass spectrometric methods published to date can achieve sensitivity which is by several orders of magnitude higher than that of alternative approaches. Femto- and attomole level limits of detection are nowadays common, while zepto- and yoctomole level limits of detection have also been reported. We envision that the ultrasensitive mass spectrometric assays will soon contribute to new discoveries in bioscience and other areas.

The application of supported liquid extraction in the analysis of benzodiazepines using surface enhanced Raman spectroscopy.

PubMed

Doctor, Erika L; McCord, Bruce

2015-11-01

Benzodiazepines are among the most frequently prescribed medicines for anxiety disorders and are present in many toxicological screens. These drugs are often administered in the commission of drug facilitated sexual assaults due their effects on the central nervous system. Due to the potency of the drugs, only small amounts are usually given to victims; therefore, the target detection limit for these compounds in biological samples has been set at 50 ng/mL. Currently the standard screening method for detection of this class of drug is the immunoassay; however, screening methods that are more sensitive and selective than immunoassays are needed to encompass the wide range of structural variants of this class of compounds. Surface enhanced Raman spectroscopy (SERS) can be highly sensitive and has been shown to permit analysis of various benzodiazepines with limits of detection as low as 6 ng/mL. This technique permits analytical results in less than 2 min when used on pure drug samples. For biological samples, a key issue for analysis by SERS is removal of exogenous salts and matrix components. In this paper we examine supported liquid extraction as a useful preparation technique for SERS detection. Supported liquid extraction has many of the benefits of liquid-liquid extraction along with the ability to be automated. This technique provides a fast and clean extraction for benzodiazepines from urine at a pH of 5.0, and does not produce large quantities of solvent waste. To validate this procedure we have determined figures of merit and examined simulated urine samples prepared with commonly appearing interferences. It was shown that at a pH 5.0 many drugs that are prevalent in urine samples can be removed, permitting a selective detection of the benzodiazepine of interest. This technique has been shown to provide rapid (less than 20 min), sensitive, and specific detection of benzodiazepines with limits of detection between 32 and 600 ng/mL and dynamic range of 32-25,000 ng/mL. It provides the forensic community with a sensitive and specific screening technique for the detection of benzodiazepines in drug facilitated assault cases. Copyright © 2015 Elsevier B.V. All rights reserved.

Ultrasensitive detection of phenolic antioxidants by surface enhanced Raman spectroscopy

NASA Astrophysics Data System (ADS)

Ornelas-Soto, N.; Aguilar-Hernández, I. A.; Afseth, N.; López-Luke, T.; Contreras-Torres, F. F.; Wold, J. P.

2017-08-01

Surface-Enhanced Raman Spectroscopy (SERS) is a powerful surface-sensitive technique to study the vibrational properties of analytes at very low concentrations. In this study, ferulic acid, p-coumaric acid, caffeic acid and sinapic acid were analyzed by SERS using Ag colloids. Analytes were detected up to 2.5x10-9M. For caffeic acid and coumaric acid, this detection limit has been reached for the first time, as well as the SERS analysis of sinapic acid using silver colloids.

An Epidemiologic Analysis of Chlamydia trachomatis and Neisseria gonorrhoeae Infections in Female Federal Prisoners

DTIC Science & Technology

2002-01-01

compared to culture.70,72 Use of PCR to detect GC has yielded sensitivities between 92-100% and specificities ranging from 96-99% on endocervical...specimen.73,74 With use of urine specimens, PCR has yielded sensitivities ranging from 65 to 92% and 96-99% respectively, for GC detection .74...21 An important limitation of PCR and LCR is that the tests may detect CT or GC nucleic acid remaining after therapy has been administered

Protein-binding aptamer assisted signal amplification for the detection of influenza A (H1N1) DNA sequences based on quantum dot fluorescence polarization analysis.

PubMed

Zhang, Juanni; Tian, Jianniao; He, Yanlong; Chen, Sheng; Jiang, Yixuan; Zhao, Yanchun; Zhao, Shulin

2013-09-07

We report a fluorescence polarization platform for H1N1 detection based on the construction of a DNA functional QD fluorescence polarization probe and a bi-functional protein binding aptamer (Apt-DNA). The assay has a linear range from 10 nM to 100 nM with a detection limit of 3.45 nM and is selective over the mismatched bases.

[Analysis of Cr in soil by LIBS based on conical spatial confinement of plasma].

PubMed

Lin, Yong-Zeng; Yao, Ming-Yin; Chen, Tian-Bing; Li, Wen-Bing; Zheng, Mei-Lan; Xu, Xue-Hong; Tu, Jian-Ping; Liu, Mu-Hua

2013-11-01

The present study is to improve the sensitivity of detection and reduce the limit of detection in detecting heavy metal of soil by laser induced breakdown spectroscopy (LIBS). The Cr element of national standard soil was regarded as the research object. In the experiment, a conical cavity with small diameter end of 20 mm and large diameter end of 45 mm respectively was installed below the focusing lens near the experiment sample to mainly confine the signal transmitted by plasma and to some extent to confine the plasma itself in the LIBS setup. In detecting Cr I 425.44 nm, the beast delay time gained from experiment is 1.3 micros, and the relative standard deviation is below 10%. Compared with the setup of non-spatial confinement, the spectral intensity of Cr in the soil sample was enhanced more than 7%. Calibration curve was established in the Cr concentration range from 60 to 400 microg x g(-1). Under the condition of spatial confinement, the liner regression coefficient and the limit of detection were 0.997 71 and 18.85 microg x g(-1) respectively, however, the regression coefficient and the limit of detection were 0.991 22 and 36.99 microg x g(-1) without spatial confinement. So, this shows that conical spatial confinement can/improve the sensitivity of detection and enhance the spectral intensity. And it is a good auxiliary function in detecting Cr in the soil by laser induced breakdown spectroscopy.

Carbohydrate and alditol analysis by high-performance anion-exchange chromatography coupled with electrochemical detection at a cobalt-modified electrode.

PubMed

Casella, Innocenzo G; Contursi, Michela

2003-07-01

A cobalt oxyhydroxide film dispersed on a carbon electrode surface was characterized and proposed as an amperometric sensor for determination of alditols and carbohydrates in flowing streams. Complex mixtures of carbohydrates were separated by anion-exchange chromatography using a moderately alkaline solution as mobile phase. The cobalt modified electrode (GC-Co) was employed under a constant applied potential of 0.5 V (vs Ag/AgCl). Under these experimental conditions the detection limits (S/N=3) for all analyzed electroactive molecules ranged between 0.3 micromol L(-1) and 1.5 micromol L(-1) and the dynamic linear ranges spanned generally three orders of magnitude above the relevant detection limits. Analytical determinations of carbohydrates and alditols in red and white wines, are reported.

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.

On the age and mass function of the globular cluster M 4: A different interpretation of recent deep HST observations

NASA Astrophysics Data System (ADS)

De Marchi, G.; Paresce, F.; Straniero, O.; Prada Moroni, P. G.

2004-03-01

Very deep images of the Galactic globular cluster M 4 (NGC 6121) through the F606W and F814W filters were taken in 2001 with the WFPC2 on board the HST. A first published analysis of this data set (Richer et al. \\cite{Richer2002}) produced the result that the age of M 4 is 12.7± 0.7 Gyr (Hansen et al. \\cite{Hansen2002}), thus setting a robust lower limit to the age of the universe. In view of the great astronomical importance of getting this number right, we have subjected the same data set to the simplest possible photometric analysis that completely avoids uncertain assumptions about the origin of the detected sources. This analysis clearly reveals both a thin main sequence, from which can be deduced the deepest statistically complete mass function yet determined for a globular cluster, and a white dwarf (WD) sequence extending all the way down to the 5 \\sigma detection limit at I ≃ 27. The WD sequence is abruptly terminated at exactly this limit as expected by detection statistics. Using our most recent theoretical WD models (Prada Moroni & Straniero \\cite{Prada2002}) to obtain the expected WD sequence for different ages in the observed bandpasses, we find that the data so far obtained do not reach the peak of the WD luminosity function, thus only allowing one to set a lower limit to the age of M 4 of ˜9 Gyr. Thus, the problem of determining the absolute age of a globular cluster and, therefore, the onset of GC formation with cosmologically significant accuracy remains completely open. Only observations several magnitudes deeper than the limit obtained so far would allow one to approach this objective. Based on observations with the NASA/ESA Hubble Space Telescope, obtained at the Space Telescope Science Institute, which is operated by AURA for NASA under contract NAS5-26555.

Method validation for the determination of ochratoxin A in green and soluble coffee by immunoaffinity column cleanup and liquid chromatography.

PubMed

Diaz, G J; Ariza, D; Perilla, N S

2004-06-01

A method was validated for the determination of ochratoxin A (OTA) in soluble and green coffee. Performance parameters evaluated included selectivity, accuracy, intermediate precision, linearity, limit of detection, limit of quantitation, and ruggedness. The method was found to be selective for OTA in both matrices tested. Recovery rates from soluble coffee samples ranged from 73.5 to 91.2%, and from green coffee samples from 68.7 to 84.5%. The intermediate precision (RSDr) was between 9.1 and 9.4% for soluble coffee and between 14.3 and 15.5% for green coffee analysis. The linearity of the standard calibration curve (r(2)) was <0.999 for OTA levels of 1.0-20.0 μg/kg in coffee samples. The limit of detection was determined to be 0.01 ng of OTA on column, while the limit of quantitation was found to be 0.03 ng on column. The limit of quantitation is equivalent to 0.6 μg/kg in soluble coffee samples and 0.3 μg/kg in green coffee samples. The results of the ruggedness trial showed two factors are critical for soluble coffee analysis: the extraction method, and the flow rate of the mobile phase. For green coffee analysis two critical factors detected were the extraction method and the storage temperature of the immunoaffinity column.Five samples of soluble coffee and 42 of green coffee were analysed using the validated method. All soluble coffee samples contained OTA at levels that ranged from 8.4 to 13.9 μg/kg. Six of the 42 green coffee samples analysed (14.3%) contained OTA at levels ranging from 0.9 to 19.4 μg/kg. The validated method can be used to monitor OTA levels in Colombian coffee for export or for local consumption.

Plasmonic trace sensing below the photon shot noise limit

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

Pooser, Raphael C.; Lawrie, Benjamin J.

Plasmonic sensors are important detectors of biochemical trace compounds, but those that utilize optical readout are approaching their absolute limits of detection as defined by the Heisenberg uncertainty principle in both differential intensity and phase readout. However, the use of more general minimum uncertainty states in the form of squeezed light can push the noise floor in these sensors below the shot noise limit (SNL) in one analysis variable at the expense of another. Here, we demonstrate a quantum plasmonic sensor whose noise floor is reduced below the SNL in order to perform index of refraction measurements with sensitivities unobtainablemore » with classical plasmonic sensors. The increased signal-to-noise ratio can result in faster detection of analyte concentrations that were previously lost in the noise. As a result, these benefits are the hallmarks of a sensor exploiting quantum readout fields in order to manipulate the limits of the Heisenberg uncertainty principle.« less

Plasmonic trace sensing below the photon shot noise limit

DOE PAGES

Pooser, Raphael C.; Lawrie, Benjamin J.

2015-12-09

Plasmonic sensors are important detectors of biochemical trace compounds, but those that utilize optical readout are approaching their absolute limits of detection as defined by the Heisenberg uncertainty principle in both differential intensity and phase readout. However, the use of more general minimum uncertainty states in the form of squeezed light can push the noise floor in these sensors below the shot noise limit (SNL) in one analysis variable at the expense of another. Here, we demonstrate a quantum plasmonic sensor whose noise floor is reduced below the SNL in order to perform index of refraction measurements with sensitivities unobtainablemore » with classical plasmonic sensors. The increased signal-to-noise ratio can result in faster detection of analyte concentrations that were previously lost in the noise. As a result, these benefits are the hallmarks of a sensor exploiting quantum readout fields in order to manipulate the limits of the Heisenberg uncertainty principle.« less

Analysis of Android Device-Based Solutions for Fall Detection

PubMed Central

Casilari, Eduardo; Luque, Rafael; Morón, María-José

2015-01-01

Falls are a major cause of health and psychological problems as well as hospitalization costs among older adults. Thus, the investigation on automatic Fall Detection Systems (FDSs) has received special attention from the research community during the last decade. In this area, the widespread popularity, decreasing price, computing capabilities, built-in sensors and multiplicity of wireless interfaces of Android-based devices (especially smartphones) have fostered the adoption of this technology to deploy wearable and inexpensive architectures for fall detection. This paper presents a critical and thorough analysis of those existing fall detection systems that are based on Android devices. The review systematically classifies and compares the proposals of the literature taking into account different criteria such as the system architecture, the employed sensors, the detection algorithm or the response in case of a fall alarms. The study emphasizes the analysis of the evaluation methods that are employed to assess the effectiveness of the detection process. The review reveals the complete lack of a reference framework to validate and compare the proposals. In addition, the study also shows that most research works do not evaluate the actual applicability of the Android devices (with limited battery and computing resources) to fall detection solutions. PMID:26213928

Analysis of Android Device-Based Solutions for Fall Detection.

PubMed

Casilari, Eduardo; Luque, Rafael; Morón, María-José

2015-07-23

Falls are a major cause of health and psychological problems as well as hospitalization costs among older adults. Thus, the investigation on automatic Fall Detection Systems (FDSs) has received special attention from the research community during the last decade. In this area, the widespread popularity, decreasing price, computing capabilities, built-in sensors and multiplicity of wireless interfaces of Android-based devices (especially smartphones) have fostered the adoption of this technology to deploy wearable and inexpensive architectures for fall detection. This paper presents a critical and thorough analysis of those existing fall detection systems that are based on Android devices. The review systematically classifies and compares the proposals of the literature taking into account different criteria such as the system architecture, the employed sensors, the detection algorithm or the response in case of a fall alarms. The study emphasizes the analysis of the evaluation methods that are employed to assess the effectiveness of the detection process. The review reveals the complete lack of a reference framework to validate and compare the proposals. In addition, the study also shows that most research works do not evaluate the actual applicability of the Android devices (with limited battery and computing resources) to fall detection solutions.

Of Detection Limits and Effective Mitigation: The Use of Infrared Cameras for Methane Leak Detection

NASA Astrophysics Data System (ADS)

Ravikumar, A. P.; Wang, J.; McGuire, M.; Bell, C.; Brandt, A. R.

2017-12-01

Mitigating methane emissions, a short-lived and potent greenhouse gas, is critical to limiting global temperature rise to two degree Celsius as outlined in the Paris Agreement. A major source of anthropogenic methane emissions in the United States is the oil and gas sector. To this effect, state and federal governments have recommended the use of optical gas imaging systems in periodic leak detection and repair (LDAR) surveys to detect for fugitive emissions or leaks. The most commonly used optical gas imaging systems (OGI) are infrared cameras. In this work, we systematically evaluate the limits of infrared (IR) camera based OGI system for use in methane leak detection programs. We analyze the effect of various parameters that influence the minimum detectable leak rates of infrared cameras. Blind leak detection tests were carried out at the Department of Energy's MONITOR natural gas test-facility in Fort Collins, CO. Leak sources included natural gas wellheads, separators, and tanks. With an EPA mandated 60 g/hr leak detection threshold for IR cameras, we test leak rates ranging from 4 g/hr to over 350 g/hr at imaging distances between 5 ft and 70 ft from the leak source. We perform these experiments over the course of a week, encompassing a wide range of wind and weather conditions. Using repeated measurements at a given leak rate and imaging distance, we generate detection probability curves as a function of leak-size for various imaging distances, and measurement conditions. In addition, we estimate the median detection threshold - leak-size at which the probability of detection is 50% - under various scenarios to reduce uncertainty in mitigation effectiveness. Preliminary analysis shows that the median detection threshold varies from 3 g/hr at an imaging distance of 5 ft to over 150 g/hr at 50 ft (ambient temperature: 80 F, winds < 4 m/s). Results from this study can be directly used to improve OGI based LDAR protocols and reduce uncertainty in estimated mitigation effectiveness. Furthermore, detection limits determined in this study can be used as standards to compare new detection technologies.

A practical approach to tramway track condition monitoring: vertical track defects detection and identification using time-frequency processing technique

NASA Astrophysics Data System (ADS)

Bocz, Péter; Vinkó, Ákos; Posgay, Zoltán

2018-03-01

This paper presents an automatic method for detecting vertical track irregularities on tramway operation using acceleration measurements on trams. For monitoring of tramway tracks, an unconventional measurement setup is developed, which records the data of 3-axes wireless accelerometers mounted on wheel discs. Accelerations are processed to obtain the vertical track irregularities to determine whether the track needs to be repaired. The automatic detection algorithm is based on time-frequency distribution analysis and determines the defect locations. Admissible limits (thresholds) are given for detecting moderate and severe defects using statistical analysis. The method was validated on frequented tram lines in Budapest and accurately detected severe defects with a hit rate of 100%, with no false alarms. The methodology is also sensitive to moderate and small rail surface defects at the low operational speed.

Novel CE-MS technique for detection of high explosives using perfluorooctanoic acid as a MEKC and mass spectrometric complexation reagent.

PubMed

Brensinger, Karen; Rollman, Christopher; Copper, Christine; Genzman, Ashton; Rine, Jacqueline; Lurie, Ira; Moini, Mehdi

2016-01-01

To address the need for the forensic analysis of high explosives, a novel capillary electrophoresis mass spectrometry (CE-MS) technique has been developed for high resolution, sensitivity, and mass accuracy detection of these compounds. The technique uses perfluorooctanoic acid (PFOA) as both a micellar electrokinetic chromatography (MEKC) reagent for separation of neutral explosives and as the complexation reagent for mass spectrometric detection of PFOA-explosive complexes in the negative ion mode. High explosives that formed complexes with PFOA included RDX, HMX, tetryl, and PETN. Some nitroaromatics were detected as molecular ions. Detection limits in the high parts per billion range and linear calibration responses over two orders of magnitude were obtained. For proof of concept, the technique was applied to the quantitative analysis of high explosives in sand samples. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.

Development of an automated on-line electrochemical chlorite ion sensor.

PubMed

Myers, John N; Steinecker, William H; Sandlin, Zechariah D; Cox, James A; Gordon, Gilbert; Pacey, Gilbert E

2012-05-30

A sensor system for the automatic, in-line, determination of chlorite ion is reported. Electroanalytical measurements were performed in electrolyte-free liquids by using an electrochemical probe (EC), which enables in-line detection in high-resistance media such as disinfected water. Cyclic voltammetry scan rate studies suggest that the current arising from the oxidation of chlorite ion at an EC probe is mass-transfer limited. By coupling FIA with an EC probe amperometric cell, automated analysis was achieved. This sensor is intended to fulfill the daily monitoring requirements of the EPA DBP regulations for chlorite ion. Detection limits of 0.02-0.13 mg/L were attained, which is about one order of magnitude below the MRDL. The sensor showed no faradaic signal for perchlorate, chlorate, or nitrate. The lifetime and stability of the sensor were investigated by measuring calibration curves over time under constant-flow conditions. Detection limits of <0.1 mg/L were repeatedly achieved over a period of three weeks. Copyright © 2012 Elsevier B.V. All rights reserved.

“Development of an Automated On-line Electrochemical Chlorite Ion Sensor”

PubMed Central

Myers, John N.; Steinecker, William H.; Sandlin, Zechariah D.; Cox, James A.; Gordon, Gilbert; Pacey, Gilbert E.

2012-01-01

A sensor system for the automatic, in-line, determination of chlorite ion is reported. Electroanalytical measurements were performed in electrolyte-free liquids by using an electrochemical probe (EC), which enables in-line detection in high-resistance media such as disinfected water. Cyclic voltammetry scan rate studies suggest that the current arising from the oxidation of chlorite ion at an EC probe is mass-transfer limited. By coupling FIA with an EC probe amperometric cell, automated analysis was achieved. This sensor is intended to fulfill the daily monitoring requirements of the EPA DBP regulations for chlorite ion. Detection limits of 0.02-0.13 mg/L were attained, which is about one order of magnitude below the MRDL. The sensor showed no faradaic signal for perchlorate, chlorate, or nitrate. The lifetime and stability of the sensor were investigated by measuring calibration curves over time under constant-flow conditions. Detection limits of <0.1 mg/L were repeatedly achieved over a period of three weeks. PMID:22608440

Analysis of nanoliter samples of electrolytes using a flow-through microfluorometer.

PubMed

Zhelyaskov, V R; Liu, S; Broderick, M P

2000-04-01

Several techniques have been developed to study the transport properties of nanoliter samples of renal tubule segments, such as continuous flow colorimetry and continuous fluorometry. We have extended the capability of the NANOFLO, a flow-through microfluorometer, designed for measurement of carbon dioxide, urea, ammonia, glucose, lactate, etc., to analyze sodium, calcium and chloride ions, using three commercially available fluorescent indicators for intracellular and extracellular measurements. The selection of fluorescent indicator for each electrolyte was dependent on the optimal match of the dissociation constant and the analyte concentration range of interest. Using Fluo-3 dye we achieved a detection limit for Ca2+ of 0.1 pmol and selectivity over Mg2+ of between 7:1 to 10:1. Using sodium green dye we achieved detection limit for Na+ of 12 pmol and a selectivity over K+ of 40:1. The detection limit for Cl- using lucigenin dye was 10 pmol. This technique can be readily adapted for the measurement of other physiologically important ultralow volume.

Detection of calcium phosphate crystals in the joint fluid of patients with osteoarthritis – analytical approaches and challenges

PubMed Central

Yavorskyy, Alexander; Hernandez-Santana, Aaron; McCarthy, Geraldine

2008-01-01

Clinically, osteoarthritis (OA) is characterised by joint pain, stiffness after immobility, limitation of movement and, in many cases, the presence of basic calcium phosphate (BCP) crystals in the joint fluid. The detection of BCP crystals in the synovial fluid of patients with OA is fraught with challenges due to the submicroscopic size of BCP, the complex nature of the matrix in which they are found and the fact that other crystals can co-exist with them in cases of mixed pathology. Routine analysis of joint crystals still relies almost exclusively on the use of optical microscopy, which has limited applicability for BCP crystal identification due to limited resolution and the inherent subjectivity of the technique. The purpose of this Critical Review is to present an overview of some of the main analytical tools employed in the detection of BCP to date and the potential of emerging technologies such as atomic force microscopy (AFM) and Raman microspectroscopy for this purpose. PMID:18299743

Automatic adventitious respiratory sound analysis: A systematic review

PubMed Central

Bowyer, Stuart; Rodriguez-Villegas, Esther

2017-01-01

Background Automatic detection or classification of adventitious sounds is useful to assist physicians in diagnosing or monitoring diseases such as asthma, Chronic Obstructive Pulmonary Disease (COPD), and pneumonia. While computerised respiratory sound analysis, specifically for the detection or classification of adventitious sounds, has recently been the focus of an increasing number of studies, a standardised approach and comparison has not been well established. Objective To provide a review of existing algorithms for the detection or classification of adventitious respiratory sounds. This systematic review provides a complete summary of methods used in the literature to give a baseline for future works. Data sources A systematic review of English articles published between 1938 and 2016, searched using the Scopus (1938-2016) and IEEExplore (1984-2016) databases. Additional articles were further obtained by references listed in the articles found. Search terms included adventitious sound detection, adventitious sound classification, abnormal respiratory sound detection, abnormal respiratory sound classification, wheeze detection, wheeze classification, crackle detection, crackle classification, rhonchi detection, rhonchi classification, stridor detection, stridor classification, pleural rub detection, pleural rub classification, squawk detection, and squawk classification. Study selection Only articles were included that focused on adventitious sound detection or classification, based on respiratory sounds, with performance reported and sufficient information provided to be approximately repeated. Data extraction Investigators extracted data about the adventitious sound type analysed, approach and level of analysis, instrumentation or data source, location of sensor, amount of data obtained, data management, features, methods, and performance achieved. Data synthesis A total of 77 reports from the literature were included in this review. 55 (71.43%) of the studies focused on wheeze, 40 (51.95%) on crackle, 9 (11.69%) on stridor, 9 (11.69%) on rhonchi, and 18 (23.38%) on other sounds such as pleural rub, squawk, as well as the pathology. Instrumentation used to collect data included microphones, stethoscopes, and accelerometers. Several references obtained data from online repositories or book audio CD companions. Detection or classification methods used varied from empirically determined thresholds to more complex machine learning techniques. Performance reported in the surveyed works were converted to accuracy measures for data synthesis. Limitations Direct comparison of the performance of surveyed works cannot be performed as the input data used by each was different. A standard validation method has not been established, resulting in different works using different methods and performance measure definitions. Conclusion A review of the literature was performed to summarise different analysis approaches, features, and methods used for the analysis. The performance of recent studies showed a high agreement with conventional non-automatic identification. This suggests that automated adventitious sound detection or classification is a promising solution to overcome the limitations of conventional auscultation and to assist in the monitoring of relevant diseases. PMID:28552969

Analysis of LANDSAT-4 TM Data for Lithologic and Image Mapping Purpose

NASA Technical Reports Server (NTRS)

Podwysocki, M. H.; Salisbury, J. W.; Bender, L. V.; Jones, O. D.; Mimms, D. L.

1984-01-01

Lithologic mapping techniques using the near infrared bands of the Thematic Mapper onboard the LANDSAT 4 satellite are investigated. These methods are coupled with digital masking to test the capability of mapping geologic materials. Data are examined under medium to low Sun angle illumination conditions to determine the detection limits of materials with absorption features. Several detection anomalies are observed and explained.

Track Score Processing of Multiple Dissimilar Sensors

DTIC Science & Technology

2007-06-01

sensors ( infrared and light detection and ranging system) and one radio frenquency sensor (radar). The signal to noise ratio and design considerations...categorized as Johnson noise , shot noise , generation-recombination noise , temperature noise , microphonic noise , 1/f noise , and finally electronic...of 2.1 µm. The values of detectivity in this figure were derived from an analysis of commercial detectors , under background- limited conditions, at

Adaptive Non-Interventional Heuristics for Covariation Detection in Causal Induction: Model Comparison and Rational Analysis

ERIC Educational Resources Information Center

Hattori, Masasi; Oaksford, Mike

2007-01-01

In this article, 41 models of covariation detection from 2 x 2 contingency tables were evaluated against past data in the literature and against data from new experiments. A new model was also included based on a limiting case of the normative phi-coefficient under an extreme rarity assumption, which has been shown to be an important factor in…

Lesion detection performance: comparative analysis of low-dose CT data of the chest on two hybrid imaging systems.

PubMed

Jessop, Maryam; Thompson, John D; Coward, Joanne; Sanderud, Audun; Jorge, José; de Groot, Martijn; Lança, Luís; Hogg, Peter

2015-03-01

Incidental findings on low-dose CT images obtained during hybrid imaging are an increasing phenomenon as CT technology advances. Understanding the diagnostic value of incidental findings along with the technical limitations is important when reporting image results and recommending follow-up, which may result in an additional radiation dose from further diagnostic imaging and an increase in patient anxiety. This study assessed lesions incidentally detected on CT images acquired for attenuation correction on two SPECT/CT systems. An anthropomorphic chest phantom containing simulated lesions of varying size and density was imaged on an Infinia Hawkeye 4 and a Symbia T6 using the low-dose CT settings applied for attenuation correction acquisitions in myocardial perfusion imaging. Twenty-two interpreters assessed 46 images from each SPECT/CT system (15 normal images and 31 abnormal images; 41 lesions). Data were evaluated using a jackknife alternative free-response receiver-operating-characteristic analysis (JAFROC). JAFROC analysis showed a significant difference (P < 0.0001) in lesion detection, with the figures of merit being 0.599 (95% confidence interval, 0.568, 0.631) and 0.810 (95% confidence interval, 0.781, 0.839) for the Infinia Hawkeye 4 and Symbia T6, respectively. Lesion detection on the Infinia Hawkeye 4 was generally limited to larger, higher-density lesions. The Symbia T6 allowed improved detection rates for midsized lesions and some lower-density lesions. However, interpreters struggled to detect small (5 mm) lesions on both image sets, irrespective of density. Lesion detection is more reliable on low-dose CT images from the Symbia T6 than from the Infinia Hawkeye 4. This phantom-based study gives an indication of potential lesion detection in the clinical context as shown by two commonly used SPECT/CT systems, which may assist the clinician in determining whether further diagnostic imaging is justified. © 2015 by the Society of Nuclear Medicine and Molecular Imaging, Inc.

Reconnaissance investigations of potential ground-water and sediment contamination at three former underground storage tank locations, Fort Jackson, South Carolina, 1994

USGS Publications Warehouse

Robertson, J.F.; Nagle, Douglas D.; Rhodes, Liesl C.

1994-01-01

Investigations to provide initial qualitative delineation of petroleum hydrocarbon contamination at three former underground storage tank locations at Fort Jackson, South Carolina, were made during March 1994. Ground-water and sediment samples were collected using direct-push technology and analyzed on-site with a gas chromatograph, which provided real-time, semi-quantitative data. In addition, ground-water and sediment samples were collected at selected sites for laboratory analyses to provide a confirmation of the on-site data. These analyses provided qualitative data on the lateral distri- bution of petroleum hydrocarbons. Petroleum hydrocarbons were detected by on-site analysis in ground-water samples from nine locations at Site 1062, suggesting the presence of a contaminant plume. Concentrations ranged from less than the minimum detection limit to 4,511 mg/L (micrograms per liter) for benzene, 15,594 mg/L for toluene, 16,501 mg/L for ethylbenzene, and 19,391 mg/L for total xylenes. Concentrations of Total Petroleum Hydrocarbons-Gasoline Range Organics ranged from 323 mg/L to 3,364 mg/L; Total Petroleum Hydrocarbons-Diesel Range Organics were not detected. Three samples from this site were analyzed for benzene, toluene, ethylbenzene, and total xylenes at a laboratory and results showed concentrations ranging from less than the minimum detection limit to 1,070 mg/L for benzene, 7,930 mg/L for toluene, 6,890 mg/L for ethylbenzene, and 1,524 mg/L for total xylenes. Petroleum hydro- carbons were detected by on-site analysis in only one sample at Site 2438. A concentration of 131,000 micrograms per kilogram Total Petroleum Hydrocarbons-Diesel Range Organics was detected in sample number GP-2-4-13.5. Petroleum hydrocarbons were detected by on-site analysis in only one ground-water sample from Site 2444. A concentration of 3,145 mg/L Total Petroleum Hydrocarbons-Gasoline Range Organics was detected at sampling location GP-3-2.

Airborne Doppler radar detection of low altitude windshear

NASA Technical Reports Server (NTRS)

Bracalente, Emedio M.; Jones, William R.; Britt, Charles L.

1990-01-01

As part of an integrated windshear program, the Federal Aviation Administration, jointly with NASA, is sponsoring a research effort to develop airborne sensor technology for the detection of low altitude windshear during aircraft take-off and landing. One sensor being considered is microwave Doppler radar operating at X-band or above. Using a Microburst/Clutter/Radar simulation program, a preliminary feasibility study was conducted to assess the performance of Doppler radars for this application. Preliminary results from this study are presented. Analysis show, that using bin-to-bin Automatic Gain Control (AGC), clutter filtering, limited detection range, and suitable antenna tilt management, windshear from a wet microburst can be accurately detected 10 to 65 seconds (.75 to 5 km) in front of the aircraft. Although a performance improvement can be obtained at higher frequency, the baseline X-band system that was simulated detected the presence of a windshear hazard for the dry microburst. Although this study indicates the feasibility of using an airborne Doppler radar to detect low altitude microburst windshear, further detailed studies, including future flight experiments, will be required to completely characterize the capabilities and limitations.

Hair analysis for long-term monitoring of buprenorphine intake in opiate withdrawal.

PubMed

Pirro, Valentina; Fusari, Ivana; Di Corcia, Daniele; Gerace, Enrico; De Vivo, Enrico; Salomone, Alberto; Vincenti, Marco

2014-12-01

Buprenorphine (BUP) is a psychoactive pharmaceutical drug largely used to treat opiate addiction. Short-term therapeutic monitoring is supported by toxicological analysis of blood and urine samples, whereas long-term monitoring by means of hair analysis is rarely used. Aim of this work was to develop and validate a highly sensitive ultrahigh-performance liquid chromatography tandem mass spectrometry method to detect BUP and norbuprenorphine (NBUP) in head hair. Interindividual correlation between oral dosage of BUP and head hair concentration was investigated. Furthermore, an intra-individual study by means of segmental analysis was performed on subjects with variable maintenance dosage. Hair samples from a population of 79 patients in treatment for opiate addiction were analyzed. The validated ultrahigh-performance liquid chromatography tandem mass spectrometry protocol allowed to obtain limits of detection and quantification at 0.6 and 2.2 pg/mg for BUP and 5.0 and 17 pg/mg for NBUP, respectively. Validation criteria were satisfied, assuring selective analyte identification, high detection capability, and precise and accurate quantification. Significant positive correlation was found between constant oral BUP dosage (1-32 mg/d) and the summed up head hair concentrations of BUP and NBUP. Nevertheless, substantial interindividual variability limits the chance to predict the oral dosage taken by each subject from the measured concentrations in head hair. In contrast, strong correlation was observed in the results of intra-individual segmental analysis, which proved reliable to detect oral dosage variations during therapy. Remarkably, all hair samples yielded BUP concentrations higher than 10 pg/mg, even when the lowest dosage was administered. Thus, these results support the selection of 10 pg/mg as a cutoff value.

Detection of chitinase activity by 2-aminobenzoic acid labeling of chito-oligosaccharides.

PubMed

Ghauharali-van der Vlugt, Karen; Bussink, Anton P; Groener, Johanna E M; Boot, Rolf G; Aerts, Johannes M F G

2009-01-01

Chitinases are hydrolases capable of hydrolyzing the abundant natural polysaccharide chitin. Next to artificial fluorescent substrates, more physiological chito-oligomers are commonly used in chitinase assays. Analysis of chito-oligosaccharides products is generally accomplished by UV detection. However, the relatively poor sensitivity poses a serious limitation. Here we report on a novel, much more sensitive assay for the detection of chito-oligosaccharide reaction products released by chitinases, based on fluorescent detection, following chemical labeling by 2-aminobenzoic acid. Comparison with existing UV-based assays, shows that the novel assay offers the same advantages yet allows detection of chito-oligosaccharides in the low picomolar range.

Collaborative ring trial of the papaya endogenous reference gene and its polymerase chain reaction assays for genetically modified organism analysis.

PubMed

Wei, Jiaojun; Li, Feiwu; Guo, Jinchao; Li, Xiang; Xu, Junfeng; Wu, Gang; Zhang, Dabing; Yang, Litao

2013-11-27

The papaya (Carica papaya L.) Chymopapain (CHY) gene has been reported as a suitable endogenous reference gene for genetically modified (GM) papaya detection in previous studies. Herein, we further validated the use of the CHY gene and its qualitative and quantitative polymerase chain reaction (PCR) assays through an interlaboratory collaborative ring trial. A total of 12 laboratories working on detection of genetically modified organisms participated in the ring trial and returned test results. Statistical analysis of the returned results confirmed the species specificity, low heterogeneity, and single-copy number of the CHY gene among different papaya varieties. The limit of detection of the CHY qualitative PCR assay was 0.1%, while the limit of quantification of the quantitative PCR assay was ∼25 copies of haploid papaya genome with acceptable PCR efficiency and linearity. The differences between the tested and true values of papaya content in 10 blind samples ranged from 0.84 to 6.58%. These results indicated that the CHY gene was suitable as an endogenous reference gene for the identification and quantification of GM papaya.

Identification, characterization, synthesis and HPLC quantification of new process-related impurities and degradation products in retigabine.

PubMed

Douša, Michal; Srbek, Jan; Rádl, Stanislav; Cerný, Josef; Klecán, Ondřej; Havlíček, Jaroslav; Tkadlecová, Marcela; Pekárek, Tomáš; Gibala, Petr; Nováková, Lucie

2014-06-01

Two new impurities were described and determined using gradient HPLC method with UV detection in retigabine (RET). Using LC-HRMS, NMR and IR analysis the impurities were identified as RET-dimer I: diethyl {4,4'-diamino-6,6'-bis[(4-fluorobenzyl)amino]biphenyl-3,3'-diyl}biscarbamate and RET-dimer II: ethyl {2-amino-5-[{2-amino-4-[(4-fluorobenzyl) amino] phenyl} (ethoxycarbonyl) amino]-4-[(4-fluorobenzyl)amino] phenyl}carbamate. Reference standards of these impurities were synthesized followed by semipreparative HPLC purification. The mechanism of the formation of these impurities is also discussed. An HPLC method was optimized in order to separate, selectively detect and quantify all process-related impurities and degradation products of RET. The presented method, which was validated in terms of linearity, limit of detection (LOD), limit of quantification (LOQ) and selectivity is very quick (less than 11min including re-equilibration time) and therefore highly suitable for routine analysis of RET related substances as well as stability studies. Copyright © 2014 Elsevier B.V. All rights reserved.

Electrochemical aptasensor for detecting tetracycline in milk

NASA Astrophysics Data System (ADS)

Hanh Le, Thi; Phuc Pham, Van; Huyen La, Thi; Binh Phan, Thi; Huan Le, Quang

2016-03-01

A rapid, simple and sensitive biosensor system for tetracycline detection is very important in food safety. In this paper we developed a label-free aptasensor for electrochemical detection of tetracycline. According to the electrochemical impendence spectroscopy (EIS) analysis, there was a linear relationship between the concentration of tetracycline and the electron transfer resistance from 10 to 3000 ng ml-1 of the tetracycline concentration. The detection limit was 10 ng ml-1 in 15 min detection duration. The prepared aptasensor showed a good reproducibility with an acceptable stability in tetracycline detection. The recoveries of tetracycline in spiked milk samples were in the range of 88.1%-94.2%. The aptasensor has sensitivity 98% and specificity of 100%.

Breath Analysis Using Laser Spectroscopic Techniques: Breath Biomarkers, Spectral Fingerprints, and Detection Limits

PubMed Central

Wang, Chuji; Sahay, Peeyush

2009-01-01

Breath analysis, a promising new field of medicine and medical instrumentation, potentially offers noninvasive, real-time, and point-of-care (POC) disease diagnostics and metabolic status monitoring. Numerous breath biomarkers have been detected and quantified so far by using the GC-MS technique. Recent advances in laser spectroscopic techniques and laser sources have driven breath analysis to new heights, moving from laboratory research to commercial reality. Laser spectroscopic detection techniques not only have high-sensitivity and high-selectivity, as equivalently offered by the MS-based techniques, but also have the advantageous features of near real-time response, low instrument costs, and POC function. Of the approximately 35 established breath biomarkers, such as acetone, ammonia, carbon dioxide, ethane, methane, and nitric oxide, 14 species in exhaled human breath have been analyzed by high-sensitivity laser spectroscopic techniques, namely, tunable diode laser absorption spectroscopy (TDLAS), cavity ringdown spectroscopy (CRDS), integrated cavity output spectroscopy (ICOS), cavity enhanced absorption spectroscopy (CEAS), cavity leak-out spectroscopy (CALOS), photoacoustic spectroscopy (PAS), quartz-enhanced photoacoustic spectroscopy (QEPAS), and optical frequency comb cavity-enhanced absorption spectroscopy (OFC-CEAS). Spectral fingerprints of the measured biomarkers span from the UV to the mid-IR spectral regions and the detection limits achieved by the laser techniques range from parts per million to parts per billion levels. Sensors using the laser spectroscopic techniques for a few breath biomarkers, e.g., carbon dioxide, nitric oxide, etc. are commercially available. This review presents an update on the latest developments in laser-based breath analysis. PMID:22408503

Detecting depression stigma on social media: A linguistic analysis.

PubMed

Li, Ang; Jiao, Dongdong; Zhu, Tingshao

2018-05-01

Efficient detection of depression stigma in mass media is important for designing effective stigma reduction strategies. Using linguistic analysis methods, this paper aims to build computational models for detecting stigma expressions in Chinese social media posts (Sina Weibo). A total of 15,879 Weibo posts with keywords were collected and analyzed. First, a content analysis was conducted on all 15,879 posts to determine whether each of them reflected depression stigma or not. Second, using four algorithms (Simple Logistic Regression, Multilayer Perceptron Neural Networks, Support Vector Machine, and Random Forest), two groups of classification models were built based on selected linguistic features; one for differentiating between posts with and without depression stigma, and one for differentiating among posts with three specific types of depression stigma. First, 967 of 15,879 posts (6.09%) indicated depression stigma. 39.30%, 15.82%, and 14.99% of them endorsed the stigmatizing view that "People with depression are unpredictable", "Depression is a sign of personal weakness", and "Depression is not a real medical illness", respectively. Second, the highest F-Measure value for differentiating between stigma and non-stigma reached 75.2%. The highest F-Measure value for differentiating among three specific types of stigma reached 86.2%. Due to the limited and imbalanced dataset of Chinese Weibo posts, the findings of this study might have limited generalizability. This paper confirms that incorporating linguistic analysis methods into online detection of stigma can be beneficial to improve the performance of stigma reduction programs. Copyright © 2018 Elsevier B.V. All rights reserved.

Aqueous nitrite ion determination by selective reduction and gas phase nitric oxide chemiluminescence

NASA Technical Reports Server (NTRS)

Dunham, A. J.; Barkley, R. M.; Sievers, R. E.; Clarkson, T. W. (Principal Investigator)

1995-01-01

An improved method of flow injection analysis for aqueous nitrite ion exploits the sensitivity and selectivity of the nitric oxide (NO) chemilluminescence detector. Trace analysis of nitrite ion in a small sample (5-160 microL) is accomplished by conversion of nitrite ion to NO by aqueous iodide in acid. The resulting NO is transported to the gas phase through a semipermeable membrane and subsequently detected by monitoring the photoemission of the reaction between NO and ozone (O3). Chemiluminescence detection is selective for measurement of NO, and, since the detection occurs in the gas-phase, neither sample coloration nor turbidity interfere. The detection limit for a 100-microL sample is 0.04 ppb of nitrite ion. The precision at the 10 ppb level is 2% relative standard deviation, and 60-180 samples can be analyzed per hour. Samples of human saliva and food extracts were analyzed; the results from a standard colorimetric measurement are compared with those from the new chemiluminescence method in order to further validate the latter method. A high degree of selectivity is obtained due to the three discriminating steps in the process: (1) the nitrite ion to NO conversion conditions are virtually specific for nitrite ion, (2) only volatile products of the conversion will be swept to the gas phase (avoiding turbidity or color in spectrophotometric methods), and (3) the NO chemiluminescence detector selectively detects the emission from the NO + O3 reaction. The method is free of interferences, offers detection limits of low parts per billion of nitrite ion, and allows the analysis of up to 180 microL-sized samples per hour, with little sample preparation and no chromatographic separation. Much smaller samples can be analyzed by this method than in previously reported batch analysis methods, which typically require 5 mL or more of sample and often need chromatographic separations as well.

From Pacemaker to Wearable: Techniques for ECG Detection Systems.

PubMed

Kumar, Ashish; Komaragiri, Rama; Kumar, Manjeet

2018-01-11

With the alarming rise in the deaths due to cardiovascular diseases (CVD), present medical research scenario places notable importance on techniques and methods to detect CVDs. As adduced by world health organization, technological proceeds in the field of cardiac function assessment have become the nucleus and heart of all leading research studies in CVDs in which electrocardiogram (ECG) analysis is the most functional and convenient tool used to test the range of heart-related irregularities. Most of the approaches present in the literature of ECG signal analysis consider noise removal, rhythm-based analysis, and heartbeat detection to improve the performance of a cardiac pacemaker. Advancements achieved in the field of ECG segments detection and beat classification have a limited evaluation and still require clinical approvals. In this paper, approaches on techniques to implement on-chip ECG detector for a cardiac pacemaker system are discussed. Moreover, different challenges regarding the ECG signal morphology analysis deriving from medical literature is extensively reviewed. It is found that robustness to noise, wavelet parameter choice, numerical efficiency, and detection performance are essential performance indicators required by a state-of-the-art ECG detector. Furthermore, many algorithms described in the existing literature are not verified using ECG data from the standard databases. Some ECG detection algorithms show very high detection performance with the total number of detected QRS complexes. However, the high detection performance of the algorithm is verified using only a few datasets. Finally, gaps in current advancements and testing are identified, and the primary challenge remains to be implementing bullseye test for morphology analysis evaluation.

Flower-like ZnO decorated polyaniline/reduced graphene oxide nanocomposites for simultaneous determination of dopamine and uric acid.

PubMed

Ghanbari, Kh; Moloudi, M

2016-11-01

A novel sensor was fabricated by electrochemical deposition of ZnO flower-like/polyaniline nanofiber/reduced graphene oxide nanocomposite (ZnO/PANI/RGO) on glassy carbon electrode (GCE) for direct detection of dopamine (DA) and uric acid (UA) in the presence of fixed concentration of ascorbic acid (AA). Surface morphology and characterization of the modified electrodes were confirmed by field emission scanning microscopy (FE-SEM), X-ray diffraction (XRD), Raman and FT-IR spectroscopies. For individual detection, the linear responses were in the two concentration ranges of 0.001-1 μM and 1-1000 μM with detection limit 0.8 nM (S/N = 3) for DA, and also 0.1-100 μM and 100-1000 μM with detection limit 0.042 μM (S/N = 3) for UA. Simultaneous determination of these species in their mixture solution showed the linear responses in the two concentration ranges of 0.1-90 μM and 90-1000 μM with detection limit 0.017 μM (S/N = 3) for DA and also showed two linear range of 0.5-90 μM and 100-1000 μM with detection limit 0.12 μM (S/N = 3) for UA, with coexistence of 1000 μM AA. The applicability of sensor for the analysis of DA, and UA in dopamine injection solution, human serum and human urine samples was successfully demonstrated. Copyright © 2016 Elsevier Inc. All rights reserved.

Simultaneous quantitative analysis of arsenic, bismuth, selenium, and tellurium in soil samples using multi-channel hydride-generation atomic fluorescence spectrometry.

PubMed

Wang, Fang; Zhang, Gai

2011-03-01

The basic principles and the application of hydride-generation multi-channel atomic fluorescence spectrometry (HG-MC-AFS) in soil analysis are described. It is generally understood that only one or two elements can be simultaneously detected by commonly used one- or two-channel HG-AFS. In this work, a new sample-sensitive and effective method for the analysis of arsenic, bismuth, tellurium, and selenium in soil samples by simultaneous detection using HG-MC-AFS was developed. The method detection limits for arsenic, bismuth, tellurium, and selenium are 0.19 μg/g, 0.10 μg/g, 0.11 μg/g, and 0.08 μg/g, respectively. This method was successfully applied to the simultaneous determination of arsenic, bismuth, tellurium, and selenium in soil samples.

Detecting chaos in particle accelerators through the frequency map analysis method.

PubMed

Papaphilippou, Yannis

2014-06-01

The motion of beams in particle accelerators is dominated by a plethora of non-linear effects, which can enhance chaotic motion and limit their performance. The application of advanced non-linear dynamics methods for detecting and correcting these effects and thereby increasing the region of beam stability plays an essential role during the accelerator design phase but also their operation. After describing the nature of non-linear effects and their impact on performance parameters of different particle accelerator categories, the theory of non-linear particle motion is outlined. The recent developments on the methods employed for the analysis of chaotic beam motion are detailed. In particular, the ability of the frequency map analysis method to detect chaotic motion and guide the correction of non-linear effects is demonstrated in particle tracking simulations but also experimental data.

Fast and simultaneous determination of 12 polyphenols in apple peel and pulp by using chemometrics-assisted high-performance liquid chromatography with diode array detection.

PubMed

Wang, Tong; Wu, Hai-Long; Xie, Li-Xia; Zhu, Li; Liu, Zhi; Sun, Xiao-Dong; Xiao, Rong; Yu, Ru-Qin

2017-04-01

In this work, a smart chemometrics-enhanced strategy, high-performance liquid chromatography, and diode array detection coupled with second-order calibration method based on alternating trilinear decomposition algorithm was proposed to simultaneously quantify 12 polyphenols in different kinds of apple peel and pulp samples. The proposed strategy proved to be a powerful tool to solve the problems of coelution, unknown interferences, and chromatographic shifts in the process of high-performance liquid chromatography analysis, making it possible for the determination of 12 polyphenols in complex apple matrices within 10 min under simple conditions of elution. The average recoveries with standard deviations, and figures of merit including sensitivity, selectivity, limit of detection, and limit of quantitation were calculated to validate the accuracy of the proposed method. Compared to the quantitative analysis results from the classic high-performance liquid chromatography method, the statistical and graphical analysis showed that our proposed strategy obtained more reliable results. All results indicated that our proposed method used in the quantitative analysis of apple polyphenols was an accurate, fast, universal, simple, and green one, and it was expected to be developed as an attractive alternative method for simultaneous determination of multitargeted analytes in complex matrices. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analysis of volatile organic compounds from illicit cocaine samples

NASA Astrophysics Data System (ADS)

Robins, W. H.; Wright, Bob W.

1994-10-01

Detection of illicit cocaine hydrochloride shipments can be improved if there is a greater understanding of the identity and quantity of volatile compounds present. This study provides preliminary data concerning the volatile organic compounds detected in a limited set of cocaine hydrochloride samples. In all cases, cocaine was one of the major volatile compounds detected. Other tropeines were detected in almost all samples. Low concentrations of compounds which may be residues of processing solvents were observed in some samples. The equilibrium emissivity of cocaine from cocaine hydrochloride was investigated and a value of 83 parts-per-trillion was determined.

Influence of sample preparation on lipidomics analysis of polar lipids in adipose tissue.

PubMed

López-Bascón, M A; Calderón-Santiago, M; Sánchez-Ceinos, J; Fernández-Vega, A; Guzmán-Ruiz, R; López-Miranda, J; Malagon, M M; Priego-Capote, F

2018-01-15

The main limitations of lipidomics analysis are the chemical complexity of the lipids, the range of concentrations at which they exist, and the variety of samples usually analyzed. These limitations particularly affect the characterization of polar lipids owing to the interference of neutral lipids, essentially acylglycerides, which are at high concentration and suppress ionization of low concentrated lipids in mass spectrometry detection. The influence of sample preparation on lipidomics analysis of polar lipids in adipose tissue by LC-MS/MS was the aim of this research. Two common extractants used for lipids isolation, methanol:chloroform (MeOH:CHCl 3 ) and methyl tert-butyl ether (MTBE), were qualitatively and quantitatively compared for the extraction of the main families of lipids. The obtained results showed that each family of lipids is influenced differently by the extractant used. However, as a general trend, the use of MTBE as extractant led to higher extraction efficiency for unsaturated fatty acids, glycerophospholipids and ceramides, while MeOH:CHCl 3 favored the isolation of saturated fatty acids and plasmalogens. The implementation of a solid-phase extraction (SPE) step for selective isolation of glycerophospholipids prior to LC-MS/MS analysis was assayed to evaluate its influence on lipids detection coverage as compared to direct analysis. This step was critical to enhance the detection coverage of glycerophospholipids by removal of ionization suppression effects caused by acylglycerides. Copyright © 2017 Elsevier B.V. All rights reserved.

Empirically Optimized Flow Cytometric Immunoassay Validates Ambient Analyte Theory

PubMed Central

Parpia, Zaheer A.; Kelso, David M.

2010-01-01

Ekins’ ambient analyte theory predicts, counter intuitively, that an immunoassay’s limit of detection can be improved by reducing the amount of capture antibody. In addition, it also anticipates that results should be insensitive to the volume of sample as well as the amount of capture antibody added. The objective of this study is to empirically validate all of the performance characteristics predicted by Ekins’ theory. Flow cytometric analysis was used to detect binding between a fluorescent ligand and capture microparticles since it can directly measure fractional occupancy, the primary response variable in ambient analyte theory. After experimentally determining ambient analyte conditions, comparisons were carried out between ambient and non-ambient assays in terms of their signal strengths, limits of detection, and their sensitivity to variations in reaction volume and number of particles. The critical number of binding sites required for an assay to be in the ambient analyte region was estimated to be 0.1VKd. As predicted, such assays exhibited superior signal/noise levels and limits of detection; and were not affected by variations in sample volume and number of binding sites. When the signal detected measures fractional occupancy, ambient analyte theory is an excellent guide to developing assays with superior performance characteristics. PMID:20152793

Gravitational Wave Detection in the Introductory Lab

NASA Astrophysics Data System (ADS)

Burko, Lior M.

2017-01-01

Great physics breakthroughs are rarely included in the introductory physics course. General relativity and binary black hole coalescence are no different, and can be included in the introductory course only in a very limited sense. However, we can design activities that directly involve the detection of GW150914, the designation of the Gravitation Wave signal detected on September 14, 2015, thereby engage the students in this exciting discovery directly. The activities naturally do not include the construction of a detector or the detection of gravitational waves. Instead, we design it to include analysis of the data from GW150914, which includes some interesting analysis activities for students of the introductory course. The same activities can be assigned either as a laboratory exercise or as a computational project for the same population of students. The analysis tools used here are simple and available to the intended student population. It does not include the sophisticated analysis tools, which were used by LIGO to carefully analyze the detected signal. However, these simple tools are sufficient to allow the student to get important results. We have successfully assigned this lab project for students of the introductory course with calculus at Georgia Gwinnett College.

Application of Cavity Enhanced Absorption Spectroscopy to the Detection of Nitric Oxide, Carbonyl Sulphide, and Ethane—Breath Biomarkers of Serious Diseases

PubMed Central

Wojtas, Jacek

2015-01-01

The paper presents one of the laser absorption spectroscopy techniques as an effective tool for sensitive analysis of trace gas species in human breath. Characterization of nitric oxide, carbonyl sulphide and ethane, and the selection of their absorption lines are described. Experiments with some biomarkers showed that detection of pathogenic changes at the molecular level is possible using this technique. Thanks to cavity enhanced spectroscopy application, detection limits at the ppb-level and short measurements time (<3 s) were achieved. Absorption lines of reference samples of the selected volatile biomarkers were probed using a distributed feedback quantum cascade laser and a tunable laser system consisting of an optical parametric oscillator and difference frequency generator. Setup using the first source provided a detection limit of 30 ppb for nitric oxide and 250 ppb for carbonyl sulphide. During experiments employing a second laser, detection limits of 0.9 ppb and 0.3 ppb were obtained for carbonyl sulphide and ethane, respectively. The conducted experiments show that this type of diagnosis would significantly increase chances for effective therapy of some diseases. Additionally, it offers non-invasive and real time measurements, high sensitivity and selectivity as well as minimizing discomfort for patients. For that reason, such sensors can be used in screening for early detection of serious diseases. PMID:26091398

Fast methods for analysis of neurotransmitters from single cell and monitoring their releases in central nervous system by capillary electrophoresis, fluorescence microscopy and luminescence imaging

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

Wang, Ziqiang

1999-12-10

Fast methods for separation and detection of important neurotransmitters and the releases in central nervous system (CNS) were developed. Enzyme based immunoassay combined with capillary electrophoresis was used to analyze the contents of amino acid neurotransmitters from single neuron cells. The release of amino acid neurotransmitters from neuron cultures was monitored by laser induced fluorescence imaging method. The release and signal transduction of adenosine triphosphate (ATP) in CNS was studied with sensitive luminescence imaging method. A new dual-enzyme on-column reaction method combined with capillary electrophoresis has been developed for determining the glutamate content in single cells. Detection was based onmore » monitoring the laser-induced fluorescence of the reaction product NADH, and the measured fluorescence intensity was related to the concentration of glutamate in each cell. The detection limit of glutamate is down to 10 -8 M level, which is 1 order of magnitude lower than the previously reported detection limit based on similar detection methods. The mass detection limit of a few attomoles is far superior to that of any other reports. Selectivity for glutamate is excellent over most of amino acids. The glutamate content in single human erythrocyte and baby rat brain neurons were determined with this method and results agreed well with literature values.« less

Application of Cavity Enhanced Absorption Spectroscopy to the Detection of Nitric Oxide, Carbonyl Sulphide, and Ethane--Breath Biomarkers of Serious Diseases.

PubMed

Wojtas, Jacek

2015-06-17

The paper presents one of the laser absorption spectroscopy techniques as an effective tool for sensitive analysis of trace gas species in human breath. Characterization of nitric oxide, carbonyl sulphide and ethane, and the selection of their absorption lines are described. Experiments with some biomarkers showed that detection of pathogenic changes at the molecular level is possible using this technique. Thanks to cavity enhanced spectroscopy application, detection limits at the ppb-level and short measurements time (<3 s) were achieved. Absorption lines of reference samples of the selected volatile biomarkers were probed using a distributed feedback quantum cascade laser and a tunable laser system consisting of an optical parametric oscillator and difference frequency generator. Setup using the first source provided a detection limit of 30 ppb for nitric oxide and 250 ppb for carbonyl sulphide. During experiments employing a second laser, detection limits of 0.9 ppb and 0.3 ppb were obtained for carbonyl sulphide and ethane, respectively. The conducted experiments show that this type of diagnosis would significantly increase chances for effective therapy of some diseases. Additionally, it offers non-invasive and real time measurements, high sensitivity and selectivity as well as minimizing discomfort for patients. For that reason, such sensors can be used in screening for early detection of serious diseases.

Use of a capillary electrophoresis instrument with laser-induced fluorescence detection for DNA quantitation. Comparison of YO-PRO-1 and PicoGreen assays.

PubMed

Guillo, Christelle; Ferrance, Jerome P; Landers, James P

2006-04-28

Highly selective and sensitive assays are required for detection and quantitation of the small masses of DNA typically encountered in clinical and forensic settings. High detection sensitivity is achieved using fluorescent labeling dyes and detection techniques such as spectrofluorometers, microplate readers and cytometers. This work describes the use of a laser-induced fluorescence (LIF) detector in conjunction with a commercial capillary electrophoresis instrument for DNA quantitation. PicoGreen and YO-PRO-1, two fluorescent DNA labeling dyes, were used to assess the potential of the system for routine DNA analysis. Linearity, reproducibility, sensitivity, limits of detection and quantitation, and sample stability were examined for the two assays. The LIF detector response was found to be linear (R2 > 0.999) and reproducible (RSD < 9%) in both cases. The PicoGreen assay displayed lower limits of detection and quantitation (20 pg and 60 pg, respectively) than the YO-PRO-1 assay (60 pg and 260 pg, respectively). Although a small variation in fluorescence was observed for the DNA/dye complexes over time, quantitation was not significantly affected and the solutions were found to be relatively stable for 80 min. The advantages of the technique include a 4- to 40-fold reduction in the volume of sample required compared to traditional assays, a 2- to 20-fold reduction in the volume of reagents consumed, fast and automated analysis, and low cost (no specific instrumentation required).

Development of a lab-on-chip electrochemical biosensor for water quality analysis based on microalgal photosynthesis.

PubMed

Tsopela, A; Laborde, A; Salvagnac, L; Ventalon, V; Bedel-Pereira, E; Séguy, I; Temple-Boyer, P; Juneau, P; Izquierdo, R; Launay, J

2016-05-15

The present work was dedicated to the development of a lab-on-chip device for water toxicity analysis and more particularly herbicide detection in water. It consists in a portable system for on-site detection composed of three-electrode electrochemical microcells, integrated on a fluidic platform constructed on a glass substrate. The final goal is to yield a system that gives the possibility of conducting double, complementary detection: electrochemical and optical and therefore all materials used for the fabrication of the lab-on-chip platform were selected in order to obtain a device compatible with optical technology. The basic detection principle consisted in electrochemically monitoring disturbances in metabolic photosynthetic activities of algae induced by the presence of Diuron herbicide. Algal response, evaluated through oxygen (O2) monitoring through photosynthesis was different for each herbicide concentration in the examined sample. A concentration-dependent inhibition effect of the herbicide on photosynthesis was demonstrated. Herbicide detection was achieved through a range (blank - 1 µM Diuron herbicide solution) covering the limit of maximum acceptable concentration imposed by Canadian government (0.64 µM), using a halogen white light source for the stimulation of algal photosynthetic apparatus. Superior sensitivity results (limit of detection of around 0.1 µM) were obtained with an organic light emitting diode (OLED), having an emission spectrum adapted to algal absorption spectrum and assembled on the final system. Copyright © 2015 Elsevier B.V. All rights reserved.

Monitoring of Total Type II Pyrethroid Pesticides in Citrus Oils and Water by Converting to a Common Product 3-Phenoxybenzoic Acid

PubMed Central

McCoy, Mark R.; Yang, Zheng; Fu, Xun; Ahn, Ki Chang; Gee, Shirley J.; Bom, David C.; Zhong, Ping; Chang, Dan; Hammock, Bruce D.

2012-01-01

Pyrethroids are a class of insecticides that are becoming increasingly popular in agricultural and home use applications. Sensitive assays for pyrethroid insecticides in complex matrices are difficult both with instrumental and immunochemical methods. Environmental analysis of the pyrethroids by immunoassay requires either knowing which pyrethroids contaminate the source or the use of non-specific antibodies with cross reactivities to a class of compounds. We describe an alternative method that converts the type-II-pyrethroids to a common chemical product, 3-phenoxybenzoic acid (3-PBA), prior to analysis. This method is much more sensitive than detecting the parent compound, and it is much easier to detect a single compound rather than an entire class of compounds. This is useful in screening for pyrethroids as a class or in situations where a single type of pyrethroid is used. We demonstrated this technique in both citrus oils and environmental water samples with conversion rates of the pyrethroid to 3-PBA that range from 45%-75% and methods that require no extraction steps for either the immunoassay or LC-MS/MS techniques. Limits of detection for this technique applied to orange oil are 5 nM, 2 μM, and 0.8 μM when detected by LC-MS/MS, GC-MS, and immunoassay respectively. The limit of detection for pyrethroids in water when detected by immunoassay was 2 nM. PMID:22486225

Development of a one-step immunochromatographic strip test using gold nanoparticles for the rapid detection of Salmonella typhi in human serum.

PubMed

Preechakasedkit, Pattarachaya; Pinwattana, Kulwadee; Dungchai, Wijitar; Siangproh, Weena; Chaicumpa, Wanpen; Tongtawe, Pongsri; Chailapakul, Orawon

2012-01-15

An immunochromatographic strip test using gold nanoparticles was developed for the rapid detection of Salmonella typhi (S. typhi) in human serum. The strip test based on the principle of sandwich immunoassay by the specific binding of antigens from S. typhi O901 and antibody of S. typhi O901 on a nitrocellulose membrane. Antibody-gold nanoparticle conjugate was used as the label and was coated onto a glass fiber membrane, which was used as a conjugate pad. To create a test and control zone, antibody of S. typhi O901 and an anti-IgG were dotted on the nitrocellulose membrane, respectively. Positive samples were displayed as red dots at the test and control zones of the nitrocellulose membrane, while negative samples resulted in a red dot only in the control zone. The limit of detection (LOD) was found to be 1.14×10(5) cfu mL(-1), which could be visually detected by the naked eye within 15 min. This strip test provided a lower detection limit and analysis time than a dot blot immunoassay (8.88×10(6) cfu mL(-1) for LOD and 110 min for reaction time). In addition, our immunochromatographic strip test was employed to detect S. typhi in human serum effectively, with high accuracy. This strip test offers great promise for a rapid, simple and low-cost analysis of S. typhi. Copyright © 2011 Elsevier B.V. All rights reserved.

Detection of particle flow patterns in tumor by directional spatial frequency analysis

NASA Astrophysics Data System (ADS)

Russell, Stewart; Camara, Hawa; Shi, Lingyan; Hoopes, P. Jack; Kaufman, Peter; Pogue, Brian; Alfano, Robert

2016-04-01

Drug delivery to tumors is well known to be chaotic and limited, partly from dysfunctional vasculature, but also because of microscopic regional variations in composition. Modeling the of transport of nanoparticle therapeutics, therefore must include not only a description of vascular permeability, but also of the movement of the drug as suspended in tumor interstitial fluid (TIF) once it leaves the blood vessel. Understanding of this area is limited because we currently lack the tools and analytical methods to characterize it. We have previously shown that directional anisotropy of drug delivery can be detected using Directional Fourier Spatial Frequency (DFSF) Analysis. Here we extend this approach to generate flow line maps of nanoparticle transport in TIF relative to tumor ultrastructure, and show that features of tumor spatial heterogeneity can be identified that are directly related to local flow isometries. The identification of these regions of limited flow may be used as a metric for determining response to therapy, or for the optimization of adjuvant therapies such as radiation pre-treatment, or enzymatic degradation.

A liquid chromatography-mass spectrometric method for the determination of oak moss allergens atranol and chloroatranol in perfumes.

PubMed

Bossi, Rossana; Rastogi, Suresh C; Bernard, Guillaume; Gimenez-Arnau, Elena; Johansen, Jeanne D; Lepoittevin, Jean-Pierre; Menné, Torkil

2004-05-01

This paper describes a validated liquid chromatographic-tandem mass spectrometric method for quantitative analysis of the potential oak moss allergens atranol and chloroatranol in perfumes and similar products. The method employs LC-MS-MS with electrospray ionization (ESI) in negative mode. The compounds are analysed by selective reaction monitoring (SRM) of 2 or 3 ions for each compound in order to obtain high selectivity and sensitivity. The method has been validated for the following parameters: linearity; repeatability; recovery; limit of detection; and limit of quantification. The limits of detection, 5.0 ng/mL and 2.4 ng/mL, respectively, for atranol and chloroatranol, achieved by this method allowed identification of these compounds at concentrations below those causing allergic skin reactions in oak-moss-sensitive patients. The recovery of chloratranol from spiked perfumes was 96+/-4%. Low recoveries (49+/-5%) were observed for atranol in spiked perfumes, indicating ion suppression caused by matrix components. The method has been applied to the analysis of 10 randomly selected perfumes and similar products.

APPLICATIONS OF ELECTROCHEMICAL IMMUNOSENSORS TO ENVIRONMENTAL MONITORING

EPA Science Inventory

This paper discusses basic electrochemical immunoassay technology. Factors limiting the practical application of antibodies to anlaytical problems are also presented. It addresses the potential use of immunoassay methods based on electrochemical detection for the analysis of env...

Portable device for the detection of colorimetric assays

PubMed Central

Nowak, E.; Kawchuk, J.; Hoorfar, M.; Najjaran, H.

2017-01-01

In this work, a low-cost, portable device is developed to detect colorimetric assays for in-field and point-of-care (POC) analysis. The device can rapidly detect both pH values and nitrite concentrations of five different samples, simultaneously. After mixing samples with specific reagents, a high-resolution digital camera collects a picture of the sample, and a single-board computer processes the image in real time to identify the hue–saturation–value coordinates of the image. An internal light source reduces the effect of any ambient light so the device can accurately determine the corresponding pH values or nitrite concentrations. The device was purposefully designed to be low-cost, yet versatile, and the accuracy of the results have been compared to those from a conventional method. The results obtained for pH values have a mean standard deviation of 0.03 and a correlation coefficient R2 of 0.998. The detection of nitrites is between concentrations of 0.4–1.6 mg l−1, with a low detection limit of 0.2 mg l−1, and has a mean standard deviation of 0.073 and an R2 value of 0.999. The results represent great potential of the proposed portable device as an excellent analytical tool for POC colorimetric analysis and offer broad accessibility in resource-limited settings. PMID:29291093

Integrated optical detection of autonomous capillary microfluidic immunoassays:a hand-held point-of-care prototype.

PubMed

Novo, P; Chu, V; Conde, J P

2014-07-15

The miniaturization of biosensors using microfluidics has potential in enabling the development of point-of-care devices, with the added advantages of reduced time and cost of analysis with limits-of-detection comparable to those obtained through traditional laboratory techniques. Interfacing microfluidic devices with the external world can be difficult especially in aspects involving fluid handling and the need for simple sample insertion that avoids special equipment or trained personnel. In this work we present a point-of-care prototype system by integrating capillary microfluidics with a microfabricated photodiode array and electronic instrumentation into a hand-held unit. The capillary microfluidic device is capable of autonomous and sequential fluid flow, including control of the average fluid velocity at any given point of the analysis. To demonstrate the functionality of the prototype, a model chemiluminescence ELISA was performed. The performance of the integrated optical detection in the point-of-care prototype is equal to that obtained with traditional bench-top instrumentation. The photodiode signals were acquired, displayed and processed by a simple graphical user interface using a computer connected to the microcontroller through USB. The prototype performed integrated chemiluminescence ELISA detection in about 15 min with a limit-of-detection of ≈2 nM with an antibody-antigen affinity constant of ≈2×10(7) M(-1). Copyright © 2014 Elsevier B.V. All rights reserved.

Effects of Phasor Measurement Uncertainty on Power Line Outage Detection

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

Chen, Chen; Wang, Jianhui; Zhu, Hao

2014-12-01

Phasor measurement unit (PMU) technology provides an effective tool to enhance the wide-area monitoring systems (WAMSs) in power grids. Although extensive studies have been conducted to develop several PMU applications in power systems (e.g., state estimation, oscillation detection and control, voltage stability analysis, and line outage detection), the uncertainty aspects of PMUs have not been adequately investigated. This paper focuses on quantifying the impact of PMU uncertainty on power line outage detection and identification, in which a limited number of PMUs installed at a subset of buses are utilized to detect and identify the line outage events. Specifically, the linemore » outage detection problem is formulated as a multi-hypothesis test, and a general Bayesian criterion is used for the detection procedure, in which the PMU uncertainty is analytically characterized. We further apply the minimum detection error criterion for the multi-hypothesis test and derive the expected detection error probability in terms of PMU uncertainty. The framework proposed provides fundamental guidance for quantifying the effects of PMU uncertainty on power line outage detection. Case studies are provided to validate our analysis and show how PMU uncertainty influences power line outage detection.« less

Liquid chromatographic separation of zalcitabine and its stereoisomers.

PubMed

Scypinski, S; Ross, A J

1994-10-01

A liquid chromatographic method capable of separating and quantitating the stereoisomers of zalcitabine has been developed and validated. The separation was achieved with an Astec Cyclobond I--RSP column and a mobile phase of 0.25% triethylamine in water adjusted to a pH of 6.5 with glacial acetic acid. All enantiomers were found to exhibit a linear response in the range of 0.1-10% in the presence of 100% zalcitabine. Precision of analysis was found to be less than 1.5% at a level of 1% relative to zalcitabine. The limit of detection for two of the three enantiomeric impurities was determined to be 0.05% relative to zalcitabine. The detection limit for the third was found to be 0.1%. This method was successfully applied to the analysis of reference standards and several production scale batches. All of these materials were found to be stereochemically pure to a level of 99.8% or better.

Geometrical analysis of an optical fiber bundle displacement sensor

NASA Astrophysics Data System (ADS)

Shimamoto, Atsushi; Tanaka, Kohichi

1996-12-01

The performance of a multifiber optical lever was geometrically analyzed by extending the Cook and Hamm model [Appl. Opt. 34, 5854-5860 (1995)] for a basic seven-fiber optical lever. The generalized relationships between sensitivity and the displacement detection limit to the fiber core radius, illumination irradiance, and coupling angle were obtained by analyses of three various types of light source, i.e., a parallel beam light source, an infinite plane light source, and a point light source. The analysis of the point light source was confirmed by a measurement that used the light source of a light-emitting diode. The sensitivity of the fiber-optic lever is inversely proportional to the fiber core radius, whereas the receiving light power is proportional to the number of illuminating and receiving fibers. Thus, the bundling of the finer fiber with the larger number of illuminating and receiving fibers is more effective for improving sensitivity and the displacement detection limit.

ICL-based TDLAS sensor for real-time breath gas analysis of carbon monoxide isotopes.

PubMed

Ghorbani, Ramin; Schmidt, Florian M

2017-05-29

We present a compact sensor for carbon monoxide (CO) in air and exhaled breath based on a room temperature interband cascade laser (ICL) operating at 4.69 µm, a low-volume circular multipass cell and wavelength modulation absorption spectroscopy. A fringe-limited (1σ) sensitivity of 6.5 × 10 -8 cm -1 Hz -1/2 and a detection limit of 9 ± 5 ppbv at 0.07 s acquisition time are achieved, which constitutes a 25-fold improvement compared to direct absorption spectroscopy. Integration over 10 s increases the precision to 0.6 ppbv. The setup also allows measuring the stable isotope 13 CO in breath. We demonstrate quantification of indoor air CO and real-time detection of CO expirograms from healthy non-smokers and a healthy smoker before and after smoking. Isotope ratio analysis indicates depletion of 13 CO in breath compared to natural abundance.

Environmental applications of single collector high resolution ICP-MS.

PubMed

Krachler, Michael

2007-08-01

The number of environmental applications of single collector high resolution ICP-MS (HR-ICP-MS) has increased rapidly in recent years. There are many factors that contribute to make HR-ICP-MS a very powerful tool in environmental analysis. They include the extremely low detection limits achievable, tremendously high sensitivity, the ability to separate ICP-MS signals of the analyte from spectral interferences, enabling the reliable determination of many trace elements, and the reasonable precision of isotope ratio measurements. These assets are improved even further using high efficiency sample introduction systems. Therefore, external factors such as the stability of laboratory blanks are frequently the limiting factor in HR-ICP-MS analysis rather than the detection power. This review aims to highlight the most recent applications of HR-ICP-MS in this sector, focusing on matrices and applications where the superior capabilities of the instrumental technique are most useful and often ultimately required.

Authenticity analysis of pear juice employing chromatographic fingerprinting.

PubMed

Willems, Jamie L; Low, Nicholas H

2014-12-03

Pear juice is predominately composed of carbohydrates/polyols (>95% of the total soluble solids), making it susceptible to adulteration by the addition of less expensive commercial sweeteners. In this research, the major carbohydrate and polyol (fructose, glucose, sucrose, and sorbitol) content of 32 pure pear juices representing five world producing regions and three years of production was determined. Additionally, methods employing oligosaccharide profiling to detect the debasing of these samples with four commercial sweeteners (HFCS 55 and 90, TIS, and HIS) were developed using capillary gas chromatography with flame ionization detection (CGC-FID) and high-performance liquid chromatography with pulsed amperometric detection (HPAE-PAD). Detection limits for the four commercial sweeteners ranged from 0.5 to 5.0% (v/v). In addition, the developed CGC-FID method could be used to (a) detect the addition of pear to apple juice via arbutin detection and (b) determine if a pear juice was produced using enzymatic liquefaction via the presence of O-β-d-glucopyranosyl-(1→4)-d-glucopyranose (cellobiose), all within a single chromatographic analysis.

Co-occurrence of the cyanotoxins BMAA, DABA and anatoxin-a in Nebraska reservoirs, fish, and aquatic plants.

PubMed

Al-Sammak, Maitham Ahmed; Hoagland, Kyle D; Cassada, David; Snow, Daniel D

2014-01-28

Several groups of microorganisms are capable of producing toxins in aquatic environments. Cyanobacteria are prevalent blue green algae in freshwater systems, and many species produce cyanotoxins which include a variety of chemical irritants, hepatotoxins and neurotoxins. Production and occurrence of potent neurotoxic cyanotoxins β-N-methylamino-L-alanine (BMAA), 2,4-diaminobutyric acid dihydrochloride (DABA), and anatoxin-a are especially critical with environmental implications to public and animal health. Biomagnification, though not well understood in aquatic systems, is potentially relevant to both human and animal health effects. Because little is known regarding their presence in fresh water, we investigated the occurrence and potential for bioaccumulation of cyanotoxins in several Nebraska reservoirs. Collection and analysis of 387 environmental and biological samples (water, fish, and aquatic plant) provided a snapshot of their occurrence. A sensitive detection method was developed using solid phase extraction (SPE) in combination with high pressure liquid chromatography-fluorescence detection (HPLC/FD) with confirmation by liquid chromatography-tandem mass spectrometry (LC/MS/MS). HPLC/FD detection limits ranged from 5 to 7 µg/L and LC/MS/MS detection limits were <0.5 µg/L, while detection limits for biological samples were in the range of 0.8-3.2 ng/g depending on the matrix. Based on these methods, measurable levels of these neurotoxic compounds were detected in approximately 25% of the samples, with detections of BMAA in about 18.1%, DABA in 17.1%, and anatoxin-a in 11.9%.

Co-occurrence of the Cyanotoxins BMAA, DABA and Anatoxin-a in Nebraska Reservoirs, Fish, and Aquatic Plants

PubMed Central

Al-Sammak, Maitham Ahmed; Hoagland, Kyle D.; Cassada, David; Snow, Daniel D.

2014-01-01

Several groups of microorganisms are capable of producing toxins in aquatic environments. Cyanobacteria are prevalent blue green algae in freshwater systems, and many species produce cyanotoxins which include a variety of chemical irritants, hepatotoxins and neurotoxins. Production and occurrence of potent neurotoxic cyanotoxins β-N-methylamino-l-alanine (BMAA), 2,4-diaminobutyric acid dihydrochloride (DABA), and anatoxin-a are especially critical with environmental implications to public and animal health. Biomagnification, though not well understood in aquatic systems, is potentially relevant to both human and animal health effects. Because little is known regarding their presence in fresh water, we investigated the occurrence and potential for bioaccumulation of cyanotoxins in several Nebraska reservoirs. Collection and analysis of 387 environmental and biological samples (water, fish, and aquatic plant) provided a snapshot of their occurrence. A sensitive detection method was developed using solid phase extraction (SPE) in combination with high pressure liquid chromatography-fluorescence detection (HPLC/FD) with confirmation by liquid chromatography-tandem mass spectrometry (LC/MS/MS). HPLC/FD detection limits ranged from 5 to 7 µg/L and LC/MS/MS detection limits were <0.5 µg/L, while detection limits for biological samples were in the range of 0.8–3.2 ng/g depending on the matrix. Based on these methods, measurable levels of these neurotoxic compounds were detected in approximately 25% of the samples, with detections of BMAA in about 18.1%, DABA in 17.1%, and anatoxin-a in 11.9%. PMID:24476710

On-Chip Photothermal Analyte Detection Using Integrated Luminescent Temperature Sensors.

PubMed

Pfeiffer, Simon A; Nagl, Stefan

2017-09-05

Optical absorbance detection based on attenuated light transmission is limited in sensitivity due to short path lengths in microfluidic and other miniaturized platforms. An alternative is detection using the photothermal effect. Herein we introduce a new kind of photothermal absorbance measurement using integrated luminescent temperature sensor spots inside microfluidic channels. The temperature sensors were photopolymerized inside the channels from NOA 81 UV-curable thiolene prepolymer doped with a tris(1,10-phenanthroline)ruthenium(II) temperature probe. The polymerized sensing structures were as small as 26 ± 3 μm in diameter and displayed a temperature resolution of better than 0.3 K between 20 and 50 °C. The absorbance from 532 nm laser excitation of the food dye Amaranth as a model analyte was quantified using these spots, and the influence of the flow rate, laser power, and concentration was investigated. Calibration yielded a linear relationship between analyte concentration and the temperature signal in the channels. The limit of detection for the azo-dye Amaranth (E123) in this setup was 13 μM. A minimal detectable absorbance of 3.2 × 10 -3 AU was obtained using an optical path length of 125 μm in this initial study. A microreactor with integrated temperature sensors was then employed for an absorbance-based miniaturized nitrite analysis, yielding a detection limit of 26 μM at a total assay time of only 75 s. This technique is very promising for sensitive, and potentially spatially resolved, optical absorbance detection on the micro- and nanoscale.

Mobile flow cytometer for mHealth.

PubMed

Balsam, Joshua; Bruck, Hugh Alan; Rasooly, Avraham

2015-01-01

Flow cytometry is used for cell counting and analysis in numerous clinical and environmental applications. However flow cytometry is not used in mHealth mainly because current flow cytometers are large, expensive, power-intensive devices designed to operate in a laboratory. Their design results in a lack of portability and makes them unsuitable for mHealth applications. Another limitation of current technology is the low volumetric throughput rates that are not suitable for rapid detection of rare cells.To address these limitations, we describe here a novel, low-cost, mobile flow cytometer based on wide-field imaging with a webcam for large volume and high throughput fluorescence detection of rare cells as a simulation for circulating tumor cells (CTCs) detection. The mobile flow cytometer uses a commercially available webcam capable of 187 frames per second video capture at a resolution of 320 × 240 pixels. For fluorescence detection, a 1 W 450 nm blue laser is used for excitation of Syto-9 fluorescently stained cells detected at 535 nm. A wide-field flow cell was developed for large volume analysis that allows for the linear velocity of target cells to be lower than in conventional hydrodynamic focusing flow cells typically used in cytometry. The mobile flow cytometer was found to be capable of detecting low concentrations at flow rates of 500 μL/min, suitable for rare cell detection in large volumes. The simplicity and low cost of this device suggests that it may have a potential clinical use for mHealth flow cytometry for resource-poor settings associated with global health.

Wide-field surface plasmon microscopy of nano- and microparticles: features, benchmarking, limitations, and bioanalytical applications

NASA Astrophysics Data System (ADS)

Nizamov, Shavkat; Scherbahn, Vitali; Mirsky, Vladimir M.

2017-05-01

Detection of nano- and micro-particles is an important task for chemical analytics, food industry, biotechnology, environmental monitoring and many other fields of science and industry. For this purpose, a method based on the detection and analysis of minute signals in surface plasmon resonance images due to adsorption of single nanopartciles was developed. This new technology allows one a real-time detection of interaction of single nano- and micro-particles with sensor surface. Adsorption of each nanoparticle leads to characteristic diffraction image whose intensity depends on the size and chemical composition of the particle. The adsorption rate characterizes volume concentration of nano- and micro-particles. Large monitored surface area of sensor enables a high dynamic range of counting and to a correspondingly high dynamic range in concentration scale. Depending on the type of particles and experimental conditions, the detection limit for aqueous samples can be below 1000 particles per microliter. For application of method in complex media, nanoparticle images are discriminated from image perturbations due to matrix components. First, the characteristic SPRM images of nanoparticles (templates) are collected in aqueous suspensions or spiked real samples. Then, the detection of nanoparticles in complex media using template matching is performed. The detection of various NPs in consumer products like cosmetics, mineral water, juices, and wines was shown at sub-ppb level. The method can be applied for ultrasensitive detection and analysis of nano- and micro-particles of biological (bacteria, viruses, endosomes), biotechnological (liposomes, protein nanoparticles for drug delivery) or technical origin.

Analysis of aldehydes in beer by gas-diffusion microextraction: characterization by high-performance liquid chromatography-diode-array detection-atmospheric pressure chemical ionization-mass spectrometry.

PubMed

Gonçalves, Luís Moreira; Magalhães, Paulo Jorge; Valente, Inês Maria; Pacheco, João Grosso; Dostálek, Pavel; Sýkora, David; Rodrigues, José António; Barros, Aquiles Araújo

2010-06-11

In this work, a recently developed extraction technique for sample preparation aiming the analysis of volatile and semi-volatile compounds named gas-diffusion microextraction (GDME) is applied in the chromatographic analysis of aldehydes in beer. Aldehydes-namely acetaldehyde (AA), methylpropanal (MA) and furfural (FA)-were simultaneously extracted and derivatized with 2,4-dinitrophenylhydrazine (DNPH), then the derivatives were separated and analyzed by high-performance liquid chromatography with spectrophotometric detection (HPLC-UV). The identity of the eluted compounds was confirmed by high-performance liquid chromatography-atmospheric pressure chemical ionization-mass-spectrometry detection in the negative ion mode (HPLC-APCI-MS). The developed methodology showed good repeatability (ca. 5%) and linearity as well as good limits of detection (AA-12.3, FA-1.5 and MA 5.4microgL(-1)) and quantification (AA-41, FA-4.9 and MA 18microgL(-1)); it also appears to be competitive in terms of speed and cost of analysis. Copyright 2010 Elsevier B.V. All rights reserved.

Analysis of glycosaminoglycan-derived disaccharides by capillary electrophoresis using laser-induced fluorescence detection

PubMed Central

Chang, Yuqing; Yang, Bo; Zhao, Xue; Linhardt, Robert J.

2012-01-01

A quantitative and highly sensitive method for the analysis of glycosaminoglycan (GAG)-derived disaccharides is presented that relies on capillary electrophoresis (CE) with laser-induced fluorescence (LIF) detection. This method enables complete separation of seventeen GAG-derived disaccharides in a single run. Unsaturated disaccharides were derivatized with 2-aminoacridone (AMAC) to improve sensitivity. The limit of detection was at the attomole level and about 100-fold more sensitive than traditional CE-ultraviolet detection. A CE separation timetable was developed to achieve complete resolution and shorten analysis time. The RSD of migration time and peak areas at both low and high concentrations of unsaturated disaccharides are all less than 2.7% and 3.2%, respectively, demonstrating that this is a reproducible method. This analysis was successfully applied to cultured Chinese hamster ovary cell samples for determination of GAG disaccharides. The current method simplifies GAG extraction steps, and reduces inaccuracy in calculating ratios of heparin/heparan sulfate to chondroitin sulfate/dermatan sulfate, resulting from the separate analyses of a single sample. PMID:22609076

Detection of l-Cysteine in wheat flour by Raman microspectroscopy combined chemometrics of HCA and PCA.

PubMed

Cebi, Nur; Dogan, Canan Ekinci; Develioglu, Ayşen; Yayla, Mediha Esra Altuntop; Sagdic, Osman

2017-08-01

l-Cysteine is deliberately added to various flour types since l-Cysteine has enabled favorable baking conditions such as low viscosity, increased elasticity and rise during baking. In Turkey, usage of l-Cysteine as a food additive isn't allowed in wheat flour according to the Turkish Food Codex Regulation on food additives. There is an urgent need for effective methods to detect l-Cysteine in wheat flour. In this study, for the first time, a new, rapid, effective, non-destructive and cost-effective method was developed for detection of l-Cysteine in wheat flour using Raman microscopy. Detection of l-Cysteine in wheat flour was accomplished successfully using Raman microscopy combined chemometrics of PCA (Principal Component Analysis) and HCA (Hierarchical Cluster Analysis). In this work, 500-2000cm -1 spectral range (fingerprint region) was determined to perform PCA and HCA analysis. l-Cysteine and l-Cystine were determined with detection limit of 0.125% (w/w) in different wheat flour samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

The Condensate Database for Big Data Analysis

NASA Astrophysics Data System (ADS)

Gallaher, D. W.; Lv, Q.; Grant, G.; Campbell, G. G.; Liu, Q.

2014-12-01

Although massive amounts of cryospheric data have been and are being generated at an unprecedented rate, a vast majority of the otherwise valuable data have been ``sitting in the dark'', with very limited quality assurance or runtime access for higher-level data analytics such as anomaly detection. This has significantly hindered data-driven scientific discovery and advances in the polar research and Earth sciences community. In an effort to solve this problem we have investigated and developed innovative techniques for the construction of ``condensate database'', which is much smaller than the original data yet still captures the key characteristics (e.g., spatio-temporal norm and changes). In addition we are taking advantage of parallel databases that make use of low cost GPU processors. As a result, efficient anomaly detection and quality assurance can be achieved with in-memory data analysis or limited I/O requests. The challenges lie in the fact that cryospheric data are massive and diverse, with normal/abnomal patterns spanning a wide range of spatial and temporal scales. This project consists of investigations in three main areas: (1) adaptive neighborhood-based thresholding in both space and time; (2) compressive-domain pattern detection and change analysis; and (3) hybrid and adaptive condensation of multi-modal, multi-scale cryospheric data.

Trace lead analysis based on carbon-screen-printed-electrodes modified via 4-carboxy-phenyl diazonium salt electroreduction.

PubMed

Bouden, Sarra; Chaussé, Annie; Dorbes, Stephane; El Tall, Omar; Bellakhal, Nizar; Dachraoui, Mohamed; Vautrin-Ul, Christine

2013-03-15

This paper describes the use of 4-carboxyphenyl-grafted screen-printed carbon electrodes (4-CP-SPEs) for trace lead analysis. These novel and simple use of electrodes were easily prepared by the electrochemical reduction of the corresponding diazonium salt. Pb detection was then performed by a three-steps method in order to avoid oxygen interference: (i) immersion of the grafted screen-printed electrode (SPE) in the sample and adsorption of Pb(II), (ii) reduction of adsorbed Pb(II) by chronoamperometry (CA), and (iii) oxidation of Pb by Anodic Square Wave Voltammetry (SWV). The reoxidation response was exploited for lead detection and quantification. In order to optimize the analytical responses, the influence of the adsorption medium pH and the adsorption time were investigated. Moreover, an interference study was carried out with Cu(II), Hg(II), Al(III), Mn(II), Zn(II), Cd(II) and no major interference can be expected to quantify Pb(II). The described method provided a limit of detection and a limit of quantification of 1.2 × 10(-9)M and 4.1 × 10(-9)M, respectively. These performances indicate that the 4-CP-SPE could be considered as an efficient tool for environmental analysis. Copyright © 2013 Elsevier B.V. All rights reserved.

Detection of titanium in human tissues after craniofacial surgery.

PubMed

Jorgenson, D S; Mayer, M H; Ellenbogen, R G; Centeno, J A; Johnson, F B; Mullick, F G; Manson, P N

1997-04-01

Generally, titanium fixation plates are not removed after osteosynthesis, because they have high biocompatability and high corrosion resistance characteristics. Experiments with laboratory animals, and limited studies of analyses of human tissues, have reported evidence of titanium release into local and distant tissues. This study summarizes our results of the analysis of soft tissues for titanium in four patients with titanium microfixation plates. Energy dispersive x-ray analysis, scanning electron microscopy, and electrothermal atomic absorption spectrophotometry were used to detect trace amounts of titanium in surrounding soft tissues. A single metal inclusion was detected by scanning electron microscopy and energy dispersive x-ray analysis in one patient, whereas, electrothermal atomic absorption spectrophotometry analyses revealed titanium present in three of four specimens in levels ranging from 7.92 to 31.8 micrograms/gm of dry tissue. Results from this study revealed trace amounts of titanium in tissues surrounding craniofacial plates. At the atomic level, electrothermal atomic absorption spectrophotometry appears to be a sensitive tool to quantitatively detect ultra-trace amounts of metal in human tissue.

Advances in on-chip photodetection for applications in miniaturized genetic analysis systems

NASA Astrophysics Data System (ADS)

Namasivayam, Vijay; Lin, Rongsheng; Johnson, Brian; Brahmasandra, Sundaresh; Razzacki, Zafar; Burke, David T.; Burns, Mark A.

2004-01-01

Microfabrication techniques have become increasingly popular in the development of next generation DNA analysis devices. Improved on-chip fluorescence detection systems may have applications in developing portable hand-held instruments for point-of-care diagnostics. Miniaturization of fluorescence detection involves construction of ultra-sensitive photodetectors that can be integrated onto a fluidic platform combined with the appropriate optical emission filters. We have previously demonstrated integration PIN photodiodes onto a microfabricated electrophoresis channel for separation and detection of DNA fragments. In this work, we present an improved detector structure that uses a PINN+ photodiode with an on-chip interference filter and a robust liquid barrier layer. This new design yields high sensitivity (detection limit of 0.9 ng µl-1 of DNA), low-noise (S/N ~ 100/1) and enhanced quantum efficiencies (>80%) over the entire visible spectrum. Applications of these photodiodes in various areas of DNA analysis such as microreactions (PCR), separations (electrophoresis) and microfluidics (drop sensing) are presented.

Knowledge-Base Semantic Gap Analysis for the Vulnerability Detection

NASA Astrophysics Data System (ADS)

Wu, Raymond; Seki, Keisuke; Sakamoto, Ryusuke; Hisada, Masayuki

Web security became an alert in internet computing. To cope with ever-rising security complexity, semantic analysis is proposed to fill-in the gap that the current approaches fail to commit. Conventional methods limit their focus to the physical source codes instead of the abstraction of semantics. It bypasses new types of vulnerability and causes tremendous business loss.

Is It Necessary to Dry Primary Standards before Analysis?

ERIC Educational Resources Information Center

Spraggins, Jeffrey M., II; Williams, Theodore R.

2005-01-01

The thermal gravimetric analysis (TGA) data suggests that the quantity of volatile components in primary standards is less than 1% of the initial weight and differential scanning calorimetry (DSC) data shows that water present in the same chemicals is below the limit of detection of the instrumentation. This suggests that the 1-2 hour drying…

Polarization-dependent optical reflection ultrasonic detection

NASA Astrophysics Data System (ADS)

Zhu, Xiaoyi; Huang, Zhiyu; Wang, Guohe; Li, Wenzhao; Li, Changhui

2017-03-01

Although ultrasound transducers based on commercial piezoelectric-material have been widely used, they generally have limited bandwidth centered at the resonant frequency. Currently, several pure-optical ultrasonic detection methods have gained increasing interest due to their wide bandwidth and high sensitivity. However, most of them require customized components (such as micro-ring, SPR, Fabry-Perot film, etc), which limit their broad implementations. In this study, we presented a simple pure-optical ultrasound detection method, called "Polarization-dependent Reflection Ultrasonic Detection" (PRUD). It detects the intensity difference between two polarization components of the probe beam that is modulated by ultrasound waves. PRUD detect the two components by using a balanced detector, which effectively suppressed much of the unwanted noise. We have achieved the sensitivity (noise equivalent pressure) to be 1.7kPa, and this can be further improved. In addition, like many other pure-optical ultrasonic detection methods, PRUD also has a flat and broad bandwidth from almost zero to over 100MHz. Besides theoretical analysis, we did a phantom study by imaging a tungsten filament to demonstrate the performance of PRUD. We believe this simple and economic method will attract both researchers and engineers in optical and ultrasound fields.

Multiresidue analysis of 22 sulfonamides and their metabolites in animal tissues using quick, easy, cheap, effective, rugged, and safe extraction and high resolution mass spectrometry (hybrid linear ion trap-Orbitrap).

PubMed

Abdallah, H; Arnaudguilhem, C; Jaber, F; Lobinski, R

2014-08-15

A new high performance liquid chromatography-high resolution mass spectrometry (HPLC-HRMS) method was developed for a simultaneous multi-residue analysis of 22 sulfonamides (SAs) and their metabolites in edible animal (pig, beef, sheep and chicken) tissues. Sample preparation was optimized on the basis of the "QuEChERS" protocol. The analytes were identified using their LC retention times and accurate mass; the identification was further confirmed by multi-stage high mass accuracy (<5ppm) mass spectrometry. The performance of the method was evaluated according to the EU guidelines for the validation of screening methods for the analysis of veterinary drugs residues. Acceptable values were obtained for: linearity (R(2)<0.99), limit of detection (LOD, 3-26μg/kg), limit of quantification (LOQ, 11-88μg/kg), accuracy (recovery 88-112%), intra- and inter-day precision 1-14 and 1-17%, respectively, decision limit (CCα) and detection capability (CCβ) around the maximum residue limits (MRL) of SAs (100μg/kg). The method was validated by analysis of a reference material FAPAS-02188 "Pig kidney" with ǀ Z-scoreǀ<0.63. The method was applied to various matrices (kidney, liver, muscle) originated from pig, beef, sheep, and chicken) allowing the simultaneous quantification of target sulfonamides at concentration levels above the MRL/2 and the identification of untargeted compounds such as N(4)-acetyl metabolites using multi-stage high mass accuracy mass spectrometry. Copyright © 2014 Elsevier B.V. All rights reserved.

Assessing carotid atherosclerosis by fiber-optic multispectral photoacoustic tomography

NASA Astrophysics Data System (ADS)

Hui, Jie; Li, Rui; Wang, Pu; Phillips, Evan; Bruning, Rebecca; Liao, Chien-Sheng; Sturek, Michael; Goergen, Craig J.; Cheng, Ji-Xin

2015-03-01

Atherosclerotic plaque at the carotid bifurcation is the underlying cause of the majority of ischemic strokes. Noninvasive imaging and quantification of the compositional changes preceding gross anatomic changes within the arterial wall is essential for diagnosis of disease. Current imaging modalities such as duplex ultrasound, computed tomography, positron emission tomography are limited by the lack of compositional contrast and the detection of flow-limiting lesions. Although high-resolution magnetic resonance imaging has been developed to characterize atherosclerotic plaque composition, its accessibility for wide clinical use is limited. Here, we demonstrate a fiber-based multispectral photoacoustic tomography system for excitation of lipids and external acoustic detection of the generated ultrasound. Using sequential ultrasound imaging of ex vivo preparations we achieved ~2 cm imaging depth and chemical selectivity for assessment of human arterial plaques. A multivariate curve resolution alternating least squares analysis method was applied to resolve the major chemical components, including intravascular lipid, intramuscular fat, and blood. These results show the promise of detecting carotid plaque in vivo through esophageal fiber-optic excitation of lipids and external acoustic detection of the generated ultrasound. This imaging system has great potential for serving as a point-ofcare device for early diagnosis of carotid artery disease in the clinic.

Lock-in thermography as a rapid and reproducible thermal characterization method for magnetic nanoparticles

NASA Astrophysics Data System (ADS)

Lemal, Philipp; Geers, Christoph; Monnier, Christophe A.; Crippa, Federica; Daum, Leopold; Urban, Dominic A.; Rothen-Rutishauser, Barbara; Bonmarin, Mathias; Petri-Fink, Alke; Moore, Thomas L.

2017-04-01

Lock-in thermography (LIT) is a sensitive imaging technique generally used in engineering and materials science (e.g. detecting defects in composite materials). However, it has recently been expanded for investigating the heating power of nanomaterials, such as superparamagnetic iron oxide nanoparticles (SPIONs). Here we implement LIT as a rapid and reproducible method that can evaluate the heating potential of various sizes of SPIONs under an alternating magnetic field (AMF), as well as the limits of detection for each particle size. SPIONs were synthesized via thermal decomposition and stabilized in water via a ligand transfer process. Thermographic measurements of SPIONs were made by stimulating particles of varying sizes and increasing concentrations under an AMF. Furthermore, a commercially available SPION sample was included as an external reference. While the size dependent heating efficiency of SPIONs has been previously described, our objective was to probe the sensitivity limits of LIT. For certain size regimes it was possible to detect signals at concentrations as low as 0.1 mg Fe/mL. Measuring at different concentrations enabled a linear regression analysis and extrapolation of the limit of detection for different size nanoparticles.

Mass spectrometer characterization of halogen gases in air at atmospheric pressure.

PubMed

Ivey, Michelle M; Foster, Krishna L

2005-03-01

We have developed a new interface for a commercial ion trap mass spectrometer equipped with APCI capable of real-time measurements of gaseous compounds with limits of detection on the order of pptv. The new interface has been tested using the detection of Br2 and Cl2 over synthetic seawater ice at atmospheric pressure as a model system. A mechanical pump is used to draw gaseous mixtures through a glass manifold into the corona discharge area, where the molecules are ionized. Analysis of bromine and chlorine in dry air show that ion intensity is affected by the pumping rate and the position of the glass manifold. The mass spectrometer signals for Br2 are linear in the 0.1-10.6 ppbv range, and the estimated 3sigma detection limit is 20 pptv. The MS signals for Cl2 are linear in the 0.2-25 ppbv range, and the estimated 3sigma detection limit is 1 ppbv. This new interface advances the field of analytical chemistry by introducing a practical modification to a commercially available ion trap mass spectrometer that expands the available methods for performing highly specific and sensitive measurements of gases in air at atmospheric pressure.

Pressure-Dependent Detection of Carbon Monoxide Employing Wavelength Modulation Spectroscopy Using a Herriott-Type Cell.

PubMed

Li, Chuanliang; Wu, Yingfa; Qiu, Xuanbing; Wei, Jilin; Deng, Lunhua

2017-05-01

Wavelength modulation spectroscopy (WMS) combined with a multipass absorption cell has been used to measure a weak absorption line of carbon monoxide (CO) at 1.578 µm. A 0.95m Herriott-type cell provides an effective absorption path length of 55.1 m. The WMS signals from the first and second harmonic output of a lock-in amplifier (WMS-1 f and 2 f, respectively) agree with the Beer-Lambert law, especially at low concentrations. After boxcar averaging, the minimum detection limit achieved is 4.3 ppm for a measurement time of 0.125 s. The corresponding normalized detection limit is 84 ppm m Hz -1/2 . If the integrated time is increased to 88 s, the minimum detectable limit of CO can reach to 0.29 ppm based on an Allan variation analysis. The pressure-dependent relationship is validated after accounting for the pressure factor in data processing. Finally, a linear correlation between the WMS-2 f amplitudes and gas concentrations is obtained at concentration ratios less than 15.5%, and the accuracy is better than 92% at total pressure less than 62.7 Torr.

Glyphosate analysis using sensors and electromigration separation techniques as alternatives to gas or liquid chromatography.

PubMed

Gauglitz, Günter; Wimmer, Benedikt; Melzer, Tanja; Huhn, Carolin

2018-01-01

Since its introduction in 1974, the herbicide glyphosate has experienced a tremendous increase in use, with about one million tons used annually today. This review focuses on sensors and electromigration separation techniques as alternatives to chromatographic methods for the analysis of glyphosate and its metabolite aminomethyl phosphonic acid. Even with the large number of studies published, glyphosate analysis remains challenging. With its polar and depending on pH even ionic functional groups lacking a chromophore, it is difficult to analyze with chromatographic techniques. Its analysis is mostly achieved after derivatization. Its purification from food and environmental samples inevitably results incoextraction of ionic matrix components, with a further impact on analysis derivatization. Its purification from food and environmental samples inevitably results in coextraction of ionic matrix components, with a further impact on analysis and also derivatization reactions. Its ability to form chelates with metal cations is another obstacle for precise quantification. Lastly, the low limits of detection required by legislation have to be met. These challenges preclude glyphosate from being analyzed together with many other pesticides in common multiresidue (chromatographic) methods. For better monitoring of glyphosate in environmental and food samples, further fast and robust methods are required. In this review, analytical methods are summarized and discussed from the perspective of biosensors and various formats of electromigration separation techniques, including modes such as capillary electrophoresis and micellar electrokinetic chromatography, combined with various detection techniques. These methods are critically discussed with regard to matrix tolerance, limits of detection reached, and selectivity.

Pushing the limits: Quantification of chromophores in real-world paper samples by GC-ECD and EI-GC-MS.

PubMed

Schedl, A; Zweckmair, T; Kikul, F; Bacher, M; Rosenau, T; Potthast, A

2018-03-01

Widening the methodology of chromophore analysis in pulp and paper science, a sensitive gas-chromatographic approach with electron-capture detection is presented and applied to model samples and real-world historic paper material. Trifluoroacetic anhydride was used for derivatization of the chromophore target compounds. The derivative formation was confirmed by NMR and accurate mass analysis. The method successfully detects and quantifies hydroxyquinones which are key chromophores in cellulosic matrices. The analytical figures of merit appeared to be in an acceptable range with an LOD down to approx. 60ng/g for each key chromophore, which allows for their successful detection in historic sample material. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of thermoelastic material properties by differential heterodyne detection of impulsive stimulated thermal scattering

PubMed Central

Verstraeten, B.; Sermeus, J.; Salenbien, R.; Fivez, J.; Shkerdin, G.; Glorieux, C.

2015-01-01

The underlying working principle of detecting impulsive stimulated scattering signals in a differential configuration of heterodyne diffraction detection is unraveled by involving optical scattering theory. The feasibility of the method for the thermoelastic characterization of coating-substrate systems is demonstrated on the basis of simulated data containing typical levels of noise. Besides the classical analysis of the photoacoustic part of the signals, which involves fitting surface acoustic wave dispersion curves, the photothermal part of the signals is analyzed by introducing thermal wave dispersion curves to represent and interpret their grating wavelength dependence. The intrinsic possibilities and limitations of both inverse problems are quantified by making use of least and most squares analysis. PMID:26236643

Hand-Held Femtogram Detection of Hazardous Picric Acid with Hydrophobic Ag Nanopillar SERS Substrates and Mechanism of Elasto-Capillarity.

PubMed

Hakonen, Aron; Wang, FengChao; Andersson, Per Ola; Wingfors, Håkan; Rindzevicius, Tomas; Schmidt, Michael Stenbæk; Soma, Venugopal Rao; Xu, Shicai; Li, YingQi; Boisen, Anja; Wu, HengAn

2017-02-24

Picric acid (PA) is a severe environmental and security risk due to its unstable, toxic, and explosive properties. It is also challenging to detect in trace amounts and in situ because of its highly acidic and anionic character. Here, we assess sensing of PA under nonlaboratory conditions using surface-enhanced Raman scattering (SERS) silver nanopillar substrates and hand-held Raman spectroscopy equipment. The advancing elasto-capillarity effects are explained by molecular dynamics simulations. We obtain a SERS PA detection limit on the order of 20 ppt, corresponding attomole amounts, which together with the simple analysis methodology demonstrates that the presented approach is highly competitive for ultrasensitive analysis in the field.

Direct analysis of environmental and biological samples for total mercury with comparison of sequential atomic absorption and fluorescence measurements from a single combustion event

NASA Astrophysics Data System (ADS)

Cizdziel, James V.; Tolbert, Candice; Brown, Garry

2010-02-01

A Direct Mercury Analyzer (DMA) based on sample combustion, concentration of mercury by amalgamation with gold, and cold vapor atomic absorption spectrometry (CVAAS) was coupled to a mercury-specific cold vapor atomic fluorescence spectrometer (CVAFS). The purpose was to evaluate combustion-AFS, a technique which is not commercially available, for low-level analysis of mercury in environmental and biological samples. The experimental setup allowed for comparison of dual measurements of mercury (AAS followed by AFS) for a single combustion event. The AFS instrument control program was modified to properly time capture of mercury from the DMA, avoiding deleterious combustion products from reaching its gold traps. Calibration was carried out using both aqueous solutions and solid reference materials. The absolute detection limits for mercury were 0.002 ng for AFS and 0.016 ng for AAS. Recoveries for reference materials ranged from 89% to 111%, and the precision was generally found to be <10% relative standard deviation (RSD). The two methods produced similar results for samples of hair, finger nails, coal, soil, leaves and food stuffs. However, for samples with mercury near the AAS detection limit (e.g., filter paper spotted with whole blood and segments of tree rings) the signal was still quantifiable with AFS, demonstrating the lower detection limit and greater sensitivity of AFS. This study shows that combustion-AFS is feasible for the direct analysis of low levels of mercury in solid samples that would otherwise require time-consuming and contamination-prone digestion.

Diagnostic value of highly-sensitive chimerism analysis after allogeneic stem cell transplantation.

PubMed

Sellmann, Lea; Rabe, Kim; Bünting, Ivonne; Dammann, Elke; Göhring, Gudrun; Ganser, Arnold; Stadler, Michael; Weissinger, Eva M; Hambach, Lothar

2018-05-02

Conventional analysis of host chimerism (HC) frequently fails to detect relapse before its clinical manifestation in patients with hematological malignancies after allogeneic stem cell transplantation (allo-SCT). Quantitative PCR (qPCR)-based highly-sensitive chimerism analysis extends the detection limit of conventional (short tandem repeats-based) chimerism analysis from 1 to 0.01% host cells in whole blood. To date, the diagnostic value of highly-sensitive chimerism analysis is hardly defined. Here, we applied qPCR-based chimerism analysis to 901 blood samples of 71 out-patients with hematological malignancies after allo-SCT. Receiver operating characteristics (ROC) curves were calculated for absolute HC values and for the increments of HC before relapse. Using the best cut-offs, relapse was detected with sensitivities of 74 or 85% and specificities of 69 or 75%, respectively. Positive predictive values (PPVs) were only 12 or 18%, but the respective negative predictive values were 98 or 99%. Relapse was detected median 38 or 45 days prior to clinical diagnosis, respectively. Considering also durations of steadily increasing HC of more than 28 days improved PPVs to more than 28 or 59%, respectively. Overall, highly-sensitive chimerism analysis excludes relapses with high certainty and predicts relapses with high sensitivity and specificity more than a month prior to clinical diagnosis.

Analysis of penicillin G in milk by liquid chromatography.

PubMed

Boison, J O; Keng, L J; MacNeil, J D

1994-01-01

A liquid chromatographic (LC) method that was previously developed for penicillin G residues in animal tissues has been adapted to milk and milk products. After protein precipitation with sodium tungstate, samples are applied to a C18 solid-phase extraction cartridge, from which penicillin is eluted, derivatized with 1,2,4-triazole-mercuric chloride solution, and analyzed by isocratic liquid chromatography (LC) on a C18 column with UV detection at 325 nm. Quantitation is done with reference to penicillin V as an internal standard. Penicillin G recoveries were determined to be > 70% on standards fortified at 3-60 ppb. Accuracy approached 100% using the penicillin V internal standard. The detection limit for penicillin G residues was 3 ppb in fluid milk. Samples may be confirmed by thermospray/LC at concentrations approaching the detection limit of the UV method.

A simple high performance liquid chromatography method for analyzing paraquat in soil solution samples.

PubMed

Ouyang, Ying; Mansell, Robert S; Nkedi-Kizza, Peter

2004-01-01

A high performance liquid chromatography (HPLC) method with UV detection was developed to analyze paraquat (1,1'-dimethyl-4,4'-dipyridinium dichloride) herbicide content in soil solution samples. The analytical method was compared with the liquid scintillation counting (LSC) method using 14C-paraquat. Agreement obtained between the two methods was reasonable. However, the detection limit for paraquat analysis was 0.5 mg L(-1) by the HPLC method and 0.05 mg L(-1) by the LSC method. The LSC method was, therefore, 10 times more precise than the HPLC method for solution concentrations less than 1 mg L(-1). In spite of the high detection limit, the UC (nonradioactive) HPLC method provides an inexpensive and environmentally safe means for determining paraquat concentration in soil solution compared with the 14C-LSC method.

Amino acid analysis in mammalian cell culture media containing serum and high glucose concentrations by anion exchange chromatography and integrated pulsed amperometric detection.

PubMed

Genzel, Yvonne; König, Susanne; Reichl, Udo

2004-12-01

The direct separation detection of amino acids by anion exchange chromatography with integrated pulsed amperometric detection was optimized for the analysis of typical mammalian cell culture broth samples. Existing gradient elution conditions were adapted, considering the additions of peptone (2 g/L) and 10 vol% fetal calf serum to the medium as well as changing concentrations of glucose from 5.5 g/L up to complete consumption. Samples had to be analyzed in two dilutions with water (1:33.3 and 1:200) due to the strongly varying amino acid concentrations in the samples as a result of the medium composition and cell metabolism. The method was validated in a linear working range for the most common amino acids (2.5-7.5 and 1.25-3.75 microM for cystine/cysteine with 15 microl injection volume). The relative standard deviation of the method for all amino acids was less than 5%, with detection limits of less than 0.6 microM and quantitation limits of less than 1.6 microM. As an example, data for the amino acid composition of different media used for the production of inactivated influenza vaccines in cell culture are shown.

A dynamical approach in exploring the unknown mass in the Solar system using pulsar timing arrays

NASA Astrophysics Data System (ADS)

Guo, Y. J.; Lee, K. J.; Caballero, R. N.

2018-04-01

The error in the Solar system ephemeris will lead to dipolar correlations in the residuals of pulsar timing array for widely separated pulsars. In this paper, we utilize such correlated signals, and construct a Bayesian data-analysis framework to detect the unknown mass in the Solar system and to measure the orbital parameters. The algorithm is designed to calculate the waveform of the induced pulsar-timing residuals due to the unmodelled objects following the Keplerian orbits in the Solar system. The algorithm incorporates a Bayesian-analysis suit used to simultaneously analyse the pulsar-timing data of multiple pulsars to search for coherent waveforms, evaluate the detection significance of unknown objects, and to measure their parameters. When the object is not detectable, our algorithm can be used to place upper limits on the mass. The algorithm is verified using simulated data sets, and cross-checked with analytical calculations. We also investigate the capability of future pulsar-timing-array experiments in detecting the unknown objects. We expect that the future pulsar-timing data can limit the unknown massive objects in the Solar system to be lighter than 10-11-10-12 M⊙, or measure the mass of Jovian system to a fractional precision of 10-8-10-9.

Capillary electrophoresis method with UV-detection for analysis of free amino acids concentrations in food.

PubMed

Omar, Mei Musa Ali; Elbashir, Abdalla Ahmed; Schmitz, Oliver J

2017-01-01

Simple and inexpensive capillary electrophoresis with UV-detection method (CE-UV) was optimized and validated for determination of six amino acids namely (alanine, asparagine, glutamine, proline, serine and valine) for Sudanese food. Amino acids in the samples were derivatized with 4-chloro-7-nitro-2,1,3-benzoxadiazole (NBD-Cl) prior to CE-UV analysis. Labeling reaction conditions (100mM borate buffer at pH 8.5, labeling reaction time 60min, temperature 70°C and NBD-Cl concentration 40mM) were systematically investigated. The optimal conditions for the separation were 100mM borate buffer at pH 9.7 and detected at 475nm. The method was validated in terms of linearity, limit of detection (LOD), limit of quantification (LOQ), precision (repeatability) (RSD%) and accuracy (recovery). Good linearity was achieved for all amino acids (r(2)>0.9981) in the concentration range of 2.5-40mg/L. The LODs in the range of 0.32-0.56mg/L were obtained. Recoveries of amino acids ranging from 85% to 108%, (n=3) were obtained. The validated method was successfully applied for the determination of amino acids for Sudanese food samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

An optimized method for neurotransmitters and their metabolites analysis in mouse hypothalamus by high performance liquid chromatography-Q Exactive hybrid quadrupole-orbitrap high-resolution accurate mass spectrometry.

PubMed

Yang, Zong-Lin; Li, Hui; Wang, Bing; Liu, Shu-Ying

2016-02-15

Neurotransmitters (NTs) and their metabolites are known to play an essential role in maintaining various physiological functions in nervous system. However, there are many difficulties in the detection of NTs together with their metabolites in biological samples. A new method for NTs and their metabolites detection by high performance liquid chromatography coupled with Q Exactive hybrid quadruple-orbitrap high-resolution accurate mass spectrometry (HPLC-HRMS) was established in this paper. This method was a great development of the applying of Q Exactive MS in the quantitative analysis. This method enabled a rapid quantification of ten compounds within 18min. Good linearity was obtained with a correlation coefficient above 0.99. The concentration range of the limit of detection (LOD) and the limit of quantitation (LOQ) level were 0.0008-0.05nmol/mL and 0.002-25.0nmol/mL respectively. Precisions (relative standard deviation, RSD) of this method were at 0.36-12.70%. Recovery ranges were between 81.83% and 118.04%. Concentrations of these compounds in mouse hypothalamus were detected by Q Exactive LC-MS technology with this method. Copyright © 2016 Elsevier B.V. All rights reserved.

Solid-Phase Spectrophotometric Analysis of 1-Naphthol Using Silica Functionalized with m-Diazophenylarsonic Acid

NASA Astrophysics Data System (ADS)

Zaitseva, Nataliya; Alekseev, Sergei; Zaitsev, Vladimir; Raks, Viktoria

2016-03-01

The m-aminophenylarsonic acid (m-APAA) was immobilized onto the silica gel surface with covalently grafted quaternary ammonium groups via ion exchange. The diazotization of ion-bonded m-APAA resulted in a new solid-phase spectrophotometric reagent for detection of 1-naphtol in environmental water samples. The procedure of solid-phase spectrophotometric analysis is characterized by 20 μg L-1 limit of detection (LOD) of 1-naphtol, up to 2000 concentration factor, and insensitivity to the presence of natural water components as well as to 30-fold excess of phenol, resorcinol, and catechol.

Simultaneous Proteomic Discovery and Targeted Monitoring using Liquid Chromatography, Ion Mobility Spectrometry, and Mass Spectrometry*

PubMed Central

Burnum-Johnson, Kristin E.; Nie, Song; Casey, Cameron P.; Monroe, Matthew E.; Orton, Daniel J.; Ibrahim, Yehia M.; Gritsenko, Marina A.; Clauss, Therese R. W.; Shukla, Anil K.; Moore, Ronald J.; Purvine, Samuel O.; Shi, Tujin; Qian, Weijun; Liu, Tao; Baker, Erin S.; Smith, Richard D.

2016-01-01

Current proteomic approaches include both broad discovery measurements and quantitative targeted analyses. In many cases, discovery measurements are initially used to identify potentially important proteins (e.g. candidate biomarkers) and then targeted studies are employed to quantify a limited number of selected proteins. Both approaches, however, suffer from limitations. Discovery measurements aim to sample the whole proteome but have lower sensitivity, accuracy, and quantitation precision than targeted approaches, whereas targeted measurements are significantly more sensitive but only sample a limited portion of the proteome. Herein, we describe a new approach that performs both discovery and targeted monitoring (DTM) in a single analysis by combining liquid chromatography, ion mobility spectrometry and mass spectrometry (LC-IMS-MS). In DTM, heavy labeled target peptides are spiked into tryptic digests and both the labeled and unlabeled peptides are detected using LC-IMS-MS instrumentation. Compared with the broad LC-MS discovery measurements, DTM yields greater peptide/protein coverage and detects lower abundance species. DTM also achieved detection limits similar to selected reaction monitoring (SRM) indicating its potential for combined high quality discovery and targeted analyses, which is a significant step toward the convergence of discovery and targeted approaches. PMID:27670688

Paramagnetic particles coupled with an automated flow injection analysis as a tool for influenza viral protein detection.

PubMed

Krejcova, Ludmila; Dospivova, Dana; Ryvolova, Marketa; Kopel, Pavel; Hynek, David; Krizkova, Sona; Hubalek, Jaromir; Adam, Vojtech; Kizek, Rene

2012-11-01

Currently, the influenza virus infects millions of individuals every year. Since the influenza virus represents one of the greatest threats, it is necessary to develop a diagnostic technique that can quickly, inexpensively, and accurately detect the virus to effectively treat and control seasonal and pandemic strains. This study presents an alternative to current detection methods. The flow-injection analysis-based biosensor, which can rapidly and economically analyze a wide panel of influenza virus strains by using paramagnetic particles modified with glycan, can selectively bind to specific viral A/H5N1/Vietnam/1203/2004 protein-labeled quantum dots. Optimized detection of cadmium sulfide quantum dots (CdS QDs)-protein complexes connected to paramagnetic microbeads was performed using differential pulse voltammetry on the surface of a hanging mercury drop electrode (HMDE) and/or glassy carbon electrode (GCE). Detection limit (3 S/N) estimations based on cadmium(II) ions quantification were 0.1 μg/mL or 10 μg/mL viral protein at HMDE or GCE, respectively. Viral protein detection was directly determined using differential pulse voltammetry Brdicka reaction. The limit detection (3 S/N) of viral protein was estimated as 0.1 μg/mL. Streptavidin-modified paramagnetic particles were mixed with biotinylated selective glycan to modify their surfaces. Under optimized conditions (250 μg/mL of glycan, 30-min long interaction with viral protein, 25°C and 400 rpm), the viral protein labeled with quantum dots was selectively isolated and its cadmium(II) content was determined. Cadmium was present in detectable amounts of 10 ng per mg of protein. Using this method, submicrogram concentrations of viral proteins can be identified. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

ANALYSIS OF SELECTED CHEMICAL GROUPS BY LIQUID CHROMATOGRAPHY/MASS SPECTROMETRY

EPA Science Inventory

The use of the moving-belt liquid chromatographic interface in combination with mass spectrometry was evaluated for determining detection limits of selected members of various chemical classes. mong the chemical classes examined were benzidines, nitrosoamines, anilines, nitroarom...

Fast determination of octinoxate and oxybenzone uv filters in swimming pool waters by gas chromatography/mass spectrometry after solid-phase microextraction.

PubMed

Yılmazcan, Ö; Kanakaki, C; Izgi, B; Rosenberg, E

2015-07-01

A fast gas chromatography/mass spectrometry method was developed and validated for the analysis of the potential endocrine disrupters octinoxate and oxybenzone in swimming pool water samples based on the solvent-free solid-phase microextraction technique. The low-pressure gas chromatography/mass spectrometry method used for the fast identification of UV filter substances was compared to a conventional method in terms of sensitivity and speed. The fast method proposed resulted in 2 min runs, leading to an eightfold decrease in the total analysis time and a sevenfold improvement in detection limits. The main parameters affecting the solid-phase microextraction process were also studied in detail and the optimized conditions were as follows: fiber coating, polyacrylate; extraction mode, direct immersion; extraction temperature, 25°C; sample volume, 5 mL; extraction time 45 min; pH 6.5. Under the optimized conditions, a linear response was obtained in the concentration range of 0.5-25 μg/L with correlation coefficients in the range 0.990-0.999. The limits of detection were 0.17-0.29 μg/L, and the recoveries were 80-83%. Combined method uncertainty was assessed and found to be less than 7% for both analytes for concentrations equal to or higher than 5 μg/L. Pool water samples were analyzed to demonstrate the applicability of the proposed method. Neither octinoxate nor oxybenzone were detected in the swimming pool water samples at concentrations above the respective limits of detection. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimization of the solvent-based dissolution method to sample volatile organic compound vapors for compound-specific isotope analysis.

PubMed

Bouchard, Daniel; Wanner, Philipp; Luo, Hong; McLoughlin, Patrick W; Henderson, James K; Pirkle, Robert J; Hunkeler, Daniel

2017-10-20

The methodology of the solvent-based dissolution method used to sample gas phase volatile organic compounds (VOC) for compound-specific isotope analysis (CSIA) was optimized to lower the method detection limits for TCE and benzene. The sampling methodology previously evaluated by [1] consists in pulling the air through a solvent to dissolve and accumulate the gaseous VOC. After the sampling process, the solvent can then be treated similarly as groundwater samples to perform routine CSIA by diluting an aliquot of the solvent into water to reach the required concentration of the targeted contaminant. Among solvents tested, tetraethylene glycol dimethyl ether (TGDE) showed the best aptitude for the method. TGDE has a great affinity with TCE and benzene, hence efficiently dissolving the compounds during their transition through the solvent. The method detection limit for TCE (5±1μg/m 3 ) and benzene (1.7±0.5μg/m 3 ) is lower when using TGDE compared to methanol, which was previously used (385μg/m 3 for TCE and 130μg/m 3 for benzene) [2]. The method detection limit refers to the minimal gas phase concentration in ambient air required to load sufficient VOC mass into TGDE to perform δ 13 C analysis. Due to a different analytical procedure, the method detection limit associated with δ 37 Cl analysis was found to be 156±6μg/m 3 for TCE. Furthermore, the experimental results validated the relationship between the gas phase TCE and the progressive accumulation of dissolved TCE in the solvent during the sampling process. Accordingly, based on the air-solvent partitioning coefficient, the sampling methodology (e.g. sampling rate, sampling duration, amount of solvent) and the final TCE concentration in the solvent, the concentration of TCE in the gas phase prevailing during the sampling event can be determined. Moreover, the possibility to analyse for TCE concentration in the solvent after sampling (or other targeted VOCs) allows the field deployment of the sampling method without the need to determine the initial gas phase TCE concentration. The simplified field deployment approach of the solvent-based dissolution method combined with the conventional analytical procedure used for groundwater samples substantially facilitates the application of CSIA to gas phase studies. Copyright © 2017 Elsevier B.V. All rights reserved.

Restricted Replication of Xenotropic Murine Leukemia Virus-Related Virus in Pigtailed Macaques

PubMed Central

Del Prete, Gregory Q.; Kearney, Mary F.; Spindler, Jon; Wiegand, Ann; Chertova, Elena; Roser, James D.; Estes, Jacob D.; Hao, Xing Pei; Trubey, Charles M.; Lara, Abigail; Lee, KyeongEun; Chaipan, Chawaree; Bess, Julian W.; Nagashima, Kunio; Keele, Brandon F.; Macallister, Rhonda; Smedley, Jeremy; Pathak, Vinay K.; KewalRamani, Vineet N.; Coffin, John M.

2012-01-01

Although xenotropic murine leukemia virus-related virus (XMRV) has been previously linked to prostate cancer and myalgic encephalomyelitis/chronic fatigue syndrome, recent data indicate that results interpreted as evidence of human XMRV infection reflect laboratory contamination rather than authentic in vivo infection. Nevertheless, XMRV is a retrovirus of undefined pathogenic potential that is able to replicate in human cells. Here we describe a comprehensive analysis of two male pigtailed macaques (Macaca nemestrina) experimentally infected with XMRV. Following intravenous inoculation with >1010 RNA copy equivalents of XMRV, viral replication was limited and transient, peaking at ≤2,200 viral RNA (vRNA) copies/ml plasma and becoming undetectable by 4 weeks postinfection, though viral DNA (vDNA) in peripheral blood mononuclear cells remained detectable through 119 days of follow-up. Similarly, vRNA was not detectable in lymph nodes by in situ hybridization despite detectable vDNA. Sequencing of cell-associated vDNA revealed extensive G-to-A hypermutation, suggestive of APOBEC-mediated viral restriction. Consistent with limited viral replication, we found transient upregulation of type I interferon responses that returned to baseline by 2 weeks postinfection, no detectable cellular immune responses, and limited or no spread to prostate tissue. Antibody responses, including neutralizing antibodies, however, were detectable by 2 weeks postinfection and maintained throughout the study. Both animals were healthy for the duration of follow-up. These findings indicate that XMRV replication and spread were limited in pigtailed macaques, predominantly by APOBEC-mediated hypermutation. Given that human APOBEC proteins restrict XMRV infection in vitro, human XMRV infection, if it occurred, would be expected to be characterized by similarly limited viral replication and spread. PMID:22238316

Feasibility of shutter-speed DCE-MRI for improved prostate cancer detection.

PubMed

Li, Xin; Priest, Ryan A; Woodward, William J; Tagge, Ian J; Siddiqui, Faisal; Huang, Wei; Rooney, William D; Beer, Tomasz M; Garzotto, Mark G; Springer, Charles S

2013-01-01

The feasibility of shutter-speed model dynamic-contrast-enhanced MRI pharmacokinetic analyses for prostate cancer detection was investigated in a prebiopsy patient cohort. Differences of results from the fast-exchange-regime-allowed (FXR-a) shutter-speed model version and the fast-exchange-limit-constrained (FXL-c) standard model are demonstrated. Although the spatial information is more limited, postdynamic-contrast-enhanced MRI biopsy specimens were also examined. The MRI results were correlated with the biopsy pathology findings. Of all the model parameters, region-of-interest-averaged K(trans) difference [ΔK(trans) ≡ K(trans)(FXR-a) - K(trans)(FXL-c)] or two-dimensional K(trans)(FXR-a) vs. k(ep)(FXR-a) values were found to provide the most useful biomarkers for malignant/benign prostate tissue discrimination (at 100% sensitivity for a population of 13, the specificity is 88%) and disease burden determination. (The best specificity for the fast-exchange-limit-constrained analysis is 63%, with the two-dimensional plot.) K(trans) and k(ep) are each measures of passive transcapillary contrast reagent transfer rate constants. Parameter value increases with shutter-speed model (relative to standard model) analysis are larger in malignant foci than in normal-appearing glandular tissue. Pathology analyses verify the shutter-speed model (FXR-a) promise for prostate cancer detection. Parametric mapping may further improve pharmacokinetic biomarker performance. Copyright © 2012 Wiley Periodicals, Inc.

Application of a SERS-based lateral flow immunoassay strip for the rapid and sensitive detection of staphylococcal enterotoxin B

NASA Astrophysics Data System (ADS)

Hwang, Joonki; Lee, Sangyeop; Choo, Jaebum

2016-06-01

A novel surface-enhanced Raman scattering (SERS)-based lateral flow immunoassay (LFA) biosensor was developed to resolve problems associated with conventional LFA strips (e.g., limits in quantitative analysis and low sensitivity). In our SERS-based biosensor, Raman reporter-labeled hollow gold nanospheres (HGNs) were used as SERS detection probes instead of gold nanoparticles. With the proposed SERS-based LFA strip, the presence of a target antigen can be identified through a colour change in the test zone. Furthermore, highly sensitive quantitative evaluation is possible by measuring SERS signals from the test zone. To verify the feasibility of the SERS-based LFA strip platform, an immunoassay of staphylococcal enterotoxin B (SEB) was performed as a model reaction. The limit of detection (LOD) for SEB, as determined with the SERS-based LFA strip, was estimated to be 0.001 ng mL-1. This value is approximately three orders of magnitude more sensitive than that achieved with the corresponding ELISA-based method. The proposed SERS-based LFA strip sensor shows significant potential for the rapid and sensitive detection of target markers in a simplified manner.A novel surface-enhanced Raman scattering (SERS)-based lateral flow immunoassay (LFA) biosensor was developed to resolve problems associated with conventional LFA strips (e.g., limits in quantitative analysis and low sensitivity). In our SERS-based biosensor, Raman reporter-labeled hollow gold nanospheres (HGNs) were used as SERS detection probes instead of gold nanoparticles. With the proposed SERS-based LFA strip, the presence of a target antigen can be identified through a colour change in the test zone. Furthermore, highly sensitive quantitative evaluation is possible by measuring SERS signals from the test zone. To verify the feasibility of the SERS-based LFA strip platform, an immunoassay of staphylococcal enterotoxin B (SEB) was performed as a model reaction. The limit of detection (LOD) for SEB, as determined with the SERS-based LFA strip, was estimated to be 0.001 ng mL-1. This value is approximately three orders of magnitude more sensitive than that achieved with the corresponding ELISA-based method. The proposed SERS-based LFA strip sensor shows significant potential for the rapid and sensitive detection of target markers in a simplified manner. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr07243c

Fiber type-specific analysis of AMPK isoforms in human skeletal muscle: advancement in methods via capillary nanoimmunoassay.

PubMed

Tobias, Irene S; Lazauskas, Kara K; Arevalo, Jose A; Bagley, James R; Brown, Lee E; Galpin, Andrew J

2018-04-01

Human skeletal muscle is a heterogeneous mixture of multiple fiber types (FT). Unfortunately, present methods for FT-specific study are constrained by limits of protein detection in single-fiber samples. These limitations beget compensatory resource-intensive procedures, ultimately dissuading investigators from pursuing FT-specific research. Additionally, previous studies neglected hybrid FT, confining their analyses to only pure FT. Here we present novel methods of protein detection across a wider spectrum of human skeletal muscle FT using fully automated capillary nanoimmunoassay (CNIA) technology. CNIA allowed a ~20-fold-lower limit of 5'-AMP-activated protein kinase (AMPK) detection compared with Western blotting. We then performed FT-specific assessment of AMPK expression as a proof of concept. Individual human muscle fibers were mechanically isolated, dissolved, and myosin heavy chain (MHC) fiber typed via SDS-PAGE. Single-fiber samples were combined in pairs and grouped into MHC I, MHC I/IIa, MHC IIa, and MHC IIa/IIx for expression analysis of AMPK isoforms α 1 , α 2 , β 1 , β 2 , γ 2 , and γ 3 with a tubulin loading control. Significant FT-specific differences were found for α 2 (1.7-fold higher in MHC IIa and MHC IIa/IIx vs. others), γ 2 (2.5-fold higher in MHC IIa vs. others), and γ 3 (2-fold higher in MHC IIa and 4-fold higher in MHC IIa/IIx vs. others). Development of a protocol that combines the efficient and sensitive CNIA technology with comprehensive SDS-PAGE fiber typing marks an important advancement in FT-specific research because it allows more precise study of the molecular mechanisms governing metabolism, adaptation, and regulation in human muscle. NEW & NOTEWORTHY We demonstrate the viability of applying capillary nanoimmunoassay technology to the study of fiber type-specific protein analysis in human muscle fibers. This novel technique enables a ~20-fold-lower limit of protein detection compared with traditional Western blotting methods. Combined with SDS-PAGE methods of fiber typing, we apply this technique to compare 5'-AMP-activated protein kinase isoform expression in myosin heavy chain (MHC) I, MHC I/IIa, MHC IIa, and MHC IIa/IIx fiber types.

Determination of quality parameters from statistical analysis of routine TLD dosimetry data.

PubMed

German, U; Weinstein, M; Pelled, O

2006-01-01

Following the as low as reasonably achievable (ALARA) practice, there is a need to measure very low doses, of the same order of magnitude as the natural background, and the limits of detection of the dosimetry systems. The different contributions of the background signals to the total zero dose reading of thermoluminescence dosemeter (TLD) cards were analysed by using the common basic definitions of statistical indicators: the critical level (L(C)), the detection limit (L(D)) and the determination limit (L(Q)). These key statistical parameters for the system operated at NRC-Negev were quantified, based on the history of readings of the calibration cards in use. The electronic noise seems to play a minor role, but the reading of the Teflon coating (without the presence of a TLD crystal) gave a significant contribution.

Transient isotachophoresis-capillary zone electrophoresis with contactless conductivity and ultraviolet detection for the analysis of paralytic shellfish toxins in mussel samples.

PubMed

Abdul Keyon, Aemi S; Guijt, Rosanne M; Bolch, Christopher J S; Breadmore, Michael C

2014-10-17

The accumulation of paralytic shellfish toxins (PSTs) in contaminated shellfish is a serious health risk making early detection important to improve shellfish safety and biotoxin management. Capillary electrophoresis (CE) has been proven as a high resolution separation technique compatible with miniaturization, making it an attractive choice in the development of portable instrumentation for early, on-site detection of PSTs. In this work, capillary zone electrophoresis (CZE) with capacitively coupled contactless conductivity detector (C(4)D) and UV detection were examined with counter-flow transient isotachophoresis (tITP) to improve the sensitivity and deal with the high conductivity sample matrix. The high sodium concentration in the sample was used as the leading ion while l-alanine was used as the terminating electrolyte (TE) and background electrolyte (BGE) in which the toxins were separated. Careful optimization of the injected sample volume and duration of the counter-flow resulted in limit of detections (LODs) ranging from 74.2 to 1020 ng/mL for tITP-CZE-C(4)D and 141 to 461 ng/mL for tITP-CZE-UV, an 8-97 fold reduction compared to conventional CZE. The LODs were adequate for the analysis of PSTs in shellfish samples close to the regulatory limit. Intra-day and inter-day repeatability values (percentage relative standard deviation, n=3) of tITP-CZE-C(4)D and tITP-CZE-UV methods for both migration time and peak height were in the range of 0.82-11% and 0.76-10%, respectively. The developed method was applied to the analysis of a contaminated mussel sample and validated against an Association of Official Analytical Chemists (AOAC)-approved method for PSTs analysis by high performance liquid chromatography (HPLC) with fluorescence detection (FLD) after pre-column oxidation of the sample. The method presented has potential for incorporation in to field-deployable devices for the early detection of PSTs on-site. Copyright © 2014 Elsevier B.V. All rights reserved.

Rapid ultra-trace analysis of sucralose in multiple-origin aqueous samples by online solid-phase extraction coupled to high-resolution mass spectrometry.

PubMed

Batchu, Sudha Rani; Ramirez, Cesar E; Gardinali, Piero R

2015-05-01

Because of its widespread consumption and its persistence during wastewater treatment, the artificial sweetener sucralose has gained considerable interest as a proxy to detect wastewater intrusion into usable water resources. The molecular resilience of this compound dictates that coastal and oceanic waters are the final recipient of this compound with unknown effects on ecosystems. Furthermore, no suitable methodologies have been reported for routine, ultra-trace detection of sucralose in seawater as the sensitivity of traditional liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis is limited by a low yield of product ions upon collision-induced dissociation (CID). In this work, we report the development and field test of an alternative analysis tool for sucralose in environmental waters, with enough sensitivity for the proper quantitation and confirmation of this analyte in seawater. The methodology is based on automated online solid-phase extraction (SPE) and high-resolving-power orbitrap MS detection. Operating in full scan (no CID), detection of the unique isotopic pattern (100:96:31 for [M-H](-), [M-H+2](-), and [M-H+4](-), respectively) was used for ultra-trace quantitation and analyte identification. The method offers fast analysis (14 min per run) and low sample consumption (10 mL per sample) with method detection and confirmation limits (MDLs and MCLs) of 1.4 and 5.7 ng/L in seawater, respectively. The methodology involves low operating costs due to virtually no sample preparation steps or consumables. As an application example, samples were collected from 17 oceanic and estuarine sites in Broward County, FL, with varying salinity (6-40 PSU). Samples included the ocean outfall of the Southern Regional Wastewater Treatment Plant (WWTP) that serves Hollywood, FL. Sucralose was detected above MCL in 78% of the samples at concentrations ranging from 8 to 148 ng/L, with the exception of the WWTP ocean outfall (at pipe end, 28 m below the surface) where the measured concentration was 8418 ± 3813 ng/L. These results demonstrate the applicability of this monitoring tool for the trace-level detection of this wastewater marker in very dilute environmental waters.

Sensitive and inexpensive digital DNA analysis by microfluidic enrichment of rolling circle amplified single-molecules.

PubMed

Kühnemund, Malte; Hernández-Neuta, Iván; Sharif, Mohd Istiaq; Cornaglia, Matteo; Gijs, Martin A M; Nilsson, Mats

2017-05-05

Single molecule quantification assays provide the ultimate sensitivity and precision for molecular analysis. However, most digital analysis techniques, i.e. droplet PCR, require sophisticated and expensive instrumentation for molecule compartmentalization, amplification and analysis. Rolling circle amplification (RCA) provides a simpler means for digital analysis. Nevertheless, the sensitivity of RCA assays has until now been limited by inefficient detection methods. We have developed a simple microfluidic strategy for enrichment of RCA products into a single field of view of a low magnification fluorescent sensor, enabling ultra-sensitive digital quantification of nucleic acids over a dynamic range from 1.2 aM to 190 fM. We prove the broad applicability of our analysis platform by demonstrating 5-plex detection of as little as ∼1 pg (∼300 genome copies) of pathogenic DNA with simultaneous antibiotic resistance marker detection, and the analysis of rare oncogene mutations. Our method is simpler, more cost-effective and faster than other digital analysis techniques and provides the means to implement digital analysis in any laboratory equipped with a standard fluorescent microscope. © The Author(s) 2017. Published by Oxford University Press on behalf of Nucleic Acids Research.

Development of a dynamic headspace gas chromatography-mass spectrometry method for on-site analysis of sulfur mustard degradation products in sediments.

PubMed

Magnusson, R; Nordlander, T; Östin, A

2016-01-15

Sampling teams performing work at sea in areas where chemical munitions may have been dumped require rapid and reliable analytical methods for verifying sulfur mustard leakage from suspected objects. Here we present such an on-site analysis method based on dynamic headspace GC-MS for analysis of five cyclic sulfur mustard degradation products that have previously been detected in sediments from chemical weapon dumping sites: 1,4-oxathiane, 1,3-dithiolane, 1,4-dithiane, 1,4,5-oxadithiephane, and 1,2,5-trithiephane. An experimental design involving authentic Baltic Sea sediments spiked with the target analytes was used to develop an optimized protocol for sample preparation, headspace extraction and analysis that afforded recoveries of up to 60-90%. The optimized method needs no organic solvents, uses only two grams of sediment on a dry weight basis and involves a unique sample presentation whereby sediment is spread uniformly as a thin layer inside the walls of a glass headspace vial. The method showed good linearity for analyte concentrations of 5-200 ng/g dw, good repeatability, and acceptable carry-over. The method's limits of detection for spiked sediment samples ranged from 2.5 to 11 μg/kg dw, with matrix interference being the main limiting factor. The instrumental detection limits were one to two orders of magnitude lower. Full-scan GC-MS analysis enabled the use of automated mass spectral deconvolution for rapid identification of target analytes. Using this approach, analytes could be identified in spiked sediment samples at concentrations down to 13-65 μg/kg dw. On-site validation experiments conducted aboard the research vessel R/V Oceania demonstrated the method's practical applicability, enabling the successful identification of four cyclic sulfur mustard degradation products at concentrations of 15-308μg/kg in sediments immediately after being collected near a wreck at the Bornholm Deep dumpsite in the Baltic Sea. Copyright © 2015 Elsevier B.V. All rights reserved.

Support vector machine as a binary classifier for automated object detection in remotely sensed data

NASA Astrophysics Data System (ADS)

Wardaya, P. D.

2014-02-01

In the present paper, author proposes the application of Support Vector Machine (SVM) for the analysis of satellite imagery. One of the advantages of SVM is that, with limited training data, it may generate comparable or even better results than the other methods. The SVM algorithm is used for automated object detection and characterization. Specifically, the SVM is applied in its basic nature as a binary classifier where it classifies two classes namely, object and background. The algorithm aims at effectively detecting an object from its background with the minimum training data. The synthetic image containing noises is used for algorithm testing. Furthermore, it is implemented to perform remote sensing image analysis such as identification of Island vegetation, water body, and oil spill from the satellite imagery. It is indicated that SVM provides the fast and accurate analysis with the acceptable result.

Trend Detection and Bivariate Frequency Analysis for Nonstrationary Rainfall Data

NASA Astrophysics Data System (ADS)

Joo, K.; Kim, H.; Shin, J. Y.; Heo, J. H.

2017-12-01

Multivariate frequency analysis has been developing for hydro-meteorological data such as rainfall, flood, and drought. Particularly, the copula has been used as a useful tool for multivariate probability model which has no limitation on deciding marginal distributions. The time-series rainfall data can be characterized to rainfall event by inter-event time definition (IETD) and each rainfall event has a rainfall depth and rainfall duration. In addition, nonstationarity in rainfall event has been studied recently due to climate change and trend detection of rainfall event is important to determine the data has nonstationarity or not. With the rainfall depth and duration of a rainfall event, trend detection and nonstationary bivariate frequency analysis has performed in this study. 62 stations from Korea Meteorological Association (KMA) over 30 years of hourly recorded data used in this study and the suitability of nonstationary copula for rainfall event has examined by the goodness-of-fit test.

Efficient Enrichment and Analysis of Vicinal-Diol-Containing Flavonoid Molecules Using Boronic-Acid-Functionalized Particles and Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry.

PubMed

Kim, Eunjin; Kang, Hyunook; Choi, Insung; Song, Jihyeon; Mok, Hyejung; Jung, Woong; Yeo, Woon-Seok

2018-05-09

Detection and quantitation of flavonoids are relatively difficult compared to those of other small-molecule analytes because flavonoids undergo rapid metabolic processes, resulting in their elimination from the body. Here, we report an efficient enrichment method for facilitating the analysis of vicinal-diol-containing flavonoid molecules using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. In our strategy, boronic-acid-functionalized polyacrylamide particles were used, where boronic acids bound to vicinal diols to form boronate monoesters at basic pH. This complex remained intact during the enrichment processes, and the vicinal-diol-containing flavonoids were easily separated by centrifugation and subsequent acidic treatments. The selectivity and limit of detection of our strategy were confirmed by mass spectrometry analysis, and the validity was assessed by performing the detection and quantitation of quercetin in mouse organs.

Quality Analysis of Chlorogenic Acid and Hyperoside in Crataegi fructus

PubMed Central

Weon, Jin Bae; Jung, Youn Sik; Ma, Choong Je

2016-01-01

Background: Crataegi fructus is a herbal medicine for strong stomach, sterilization, and alcohol detoxification. Chlorogenic acid and hyperoside are the major compounds in Crataegi fructus. Objective: In this study, we established novel high-performance liquid chromatography (HPLC)-diode array detection analysis method of chlorogenic acid and hyperoside for quality control of Crataegi fructus. Materials and Methods: HPLC analysis was achieved on a reverse-phase C18 column (5 μm, 4.6 mm × 250 mm) using water and acetonitrile as mobile phase with gradient system. The method was validated for linearity, precision, and accuracy. About 31 batches of Crataegi fructus samples collected from Korea and China were analyzed by using HPLC fingerprint of developed HPLC method. Then, the contents of chlorogenic acid and hyperoside were compared for quality evaluation of Crataegi fructus. Results: The results have shown that the average contents (w/w %) of chlorogenic acid and hyperoside in Crataegi fructus collected from Korea were 0.0438% and 0.0416%, respectively, and the average contents (w/w %) of 0.0399% and 0.0325%, respectively. Conclusion: In conclusion, established HPLC analysis method was stable and could provide efficient quality evaluation for monitoring of commercial Crataegi fructus. SUMMARY Quantitative analysis method of chlorogenic acid and hyperoside in Crataegi fructus is developed by high.performance liquid chromatography.(HPLC).diode array detectionEstablished HPLC analysis method is validated with linearity, precision, and accuracyThe developed method was successfully applied for quantitative analysis of Crataegi fructus sample collected from Korea and China. Abbreviations used: HPLC: High-performance liquid chromatography, GC: Gas chromatography, MS: Mass spectrometer, LOD: Limits of detection, LOQ: Limits of quantification, RSD: Relative standard deviation, RRT: Relative retention time, RPA: Relation peak area. PMID:27076744

A miniaturised image based fluorescence detection system for point-of-care-testing of cocaine abuse

NASA Astrophysics Data System (ADS)

Walczak, Rafał; Krüger, Jan; Moynihan, Shane

2015-08-01

In this paper, we describe a miniaturised image-based fluorescence detection system and demonstrate its viability as a highly sensitive tool for point-of-care-analysis of drugs of abuse in human sweat with a focus on monitor individuals for drugs of abuse. Investigations of miniaturised and low power optoelectronic configurations and methodologies for real-time image analysis were successfully carried out. The miniaturised fluorescence detection system was validated against a reference detection system under controlled laboratory conditions by analysing spiked sweat samples in dip stick and then strip with sample pad. As a result of the validation studies, a 1 ng mL-1 limit of detection of cocaine in sweat and full agreement of test results with the reference detection system can be reported. Results of the investigations open the way towards a detection system that integrates a hand-held fluorescence reader and a wearable skinpatch, and which can collect and in situ analyse sweat for the presence of cocaine at any point for up to tenths hours.

DNA nanomechanics allows direct digital detection of complementary DNA and microRNA targets.

PubMed

Husale, Sudhir; Persson, Henrik H J; Sahin, Ozgur

2009-12-24

Techniques to detect and quantify DNA and RNA molecules in biological samples have had a central role in genomics research. Over the past decade, several techniques have been developed to improve detection performance and reduce the cost of genetic analysis. In particular, significant advances in label-free methods have been reported. Yet detection of DNA molecules at concentrations below the femtomolar level requires amplified detection schemes. Here we report a unique nanomechanical response of hybridized DNA and RNA molecules that serves as an intrinsic molecular label. Nanomechanical measurements on a microarray surface have sufficient background signal rejection to allow direct detection and counting of hybridized molecules. The digital response of the sensor provides a large dynamic range that is critical for gene expression profiling. We have measured differential expressions of microRNAs in tumour samples; such measurements have been shown to help discriminate between the tissue origins of metastatic tumours. Two hundred picograms of total RNA is found to be sufficient for this analysis. In addition, the limit of detection in pure samples is found to be one attomolar. These results suggest that nanomechanical read-out of microarrays promises attomolar-level sensitivity and large dynamic range for the analysis of gene expression, while eliminating biochemical manipulations, amplification and labelling.

Modern Directions for Potentiometric Sensors

PubMed Central

Bakker, Eric; Chumbimuni-Torres, Karin

2009-01-01

This paper gives an overview of the newest developments of polymeric membrane ion-selective electrodes. A short essence of the underlying theory is given, emphasizing how the electromotive force may be used to assess binding constants of the ionophore, and how the selectivity and detection limit are related to the underlying membrane processes. The recent developments in lowering the detection limits of ISEs are described, including recent approaches of developing all solid state ISEs, and breakthroughs in detecting ultra-small quantities of ions at low concentrations. These developments have paved the way to use potentiometric sensors as in ultra-sensitive affinity bioanalysis in conjunction with nanoparticle labels. Recent results establish that potentiometry compares favorably to electrochemical stripping analysis. Other new developments with ion-selective electrodes are also described, including the concept of backside calibration potentiometry, controlled current coulometry, pulsed chronopotentiometry, and localized flash titration with ion-selective membranes to design sensors for the direct detection of total acidity without net sample perturbation. These developments have further opened the field for exciting new possibilities and applications. PMID:19890473

Surface Plasmon Resonance Based Sensitive Immunosensor for Benzaldehyde Detection

NASA Astrophysics Data System (ADS)

Onodera, Takeshi; Shimizu, Takuzo; Miura, Norio; Matsumoto, Kiyoshi; Toko, Kiyoshi

Fragrant compounds used to add flavor to beverages remain in the manufacturing line after the beverage manufacturing process. Line cleanliness before the next manufacturing cycle is difficult to estimate by sensory analysis, making excessive washing necessary. A new measurement system to determine line cleanliness is desired. In this study, we attempted to detect benzaldehyde (Bz) using an anti-Bz monoclonal antibody (Bz-Ab) and a surface plasmon resonance (SPR) sensor. We fabricated two types of sensor chips using self-assembled monolayers (SAMs) and investigated which sensor surface exhibited higher sensitivity. In addition, anti-Bz antibody conjugated with horseradish peroxidase (HRP-Bz-Ab) was used to enhance the SPR signal. A detection limit of ca. 9ng/mL (ppb) was achieved using an immobilized 4-carboxybenzaldehyde sensor surface using SAMs containing ethylene glycol. When the HRP-Bz-Ab concentration was reduced to 30ng/mL, a detection limit of ca. 4ng/mL (ppb) was achieved for Bz.

Collection and analysis of NASA clean room air samples

NASA Technical Reports Server (NTRS)

Sheldon, L. S.; Keever, J.

1985-01-01

The environment of the HALOE assembly clean room at NASA Langley Research Center is analyzed to determine the background levels of airborne organic compounds. Sampling is accomplished by pumping the clean room air through absorbing cartridges. For volatile organics, cartridges are thermally desorbed and then analyzed by gas chromatography and mass spectrometry, compounds are identified by searching the EPA/NIH data base using an interactive operator INCOS computer search algorithm. For semivolatile organics, cartridges are solvent entracted and concentrated extracts are analyzed by gas chromatography-electron capture detection, compound identification is made by matching gas chromatogram retention times with known standards. The detection limits for the semivolatile organics are; 0.89 ng cu m for dioctylphlhalate (DOP) and 1.6 ng cu m for polychlorinated biphenyls (PCB). The detection limit for volatile organics ranges from 1 to 50 parts per trillion. Only trace quantities of organics are detected, the DOP levels do not exceed 2.5 ng cu m and the PCB levels do not exceed 454 ng cu m.

Autism and urinary exogenous neuropeptides: development of an on-line SPE-HPLC-tandem mass spectrometry method to test the opioid excess theory.

PubMed

Dettmer, K; Hanna, D; Whetstone, P; Hansen, R; Hammock, B D

2007-08-01

Autism is a complex neurodevelopmental disorder with unknown etiology. One hypothesis regarding etiology in autism is the "opioid peptide excess" theory that postulates that excessive amounts of exogenous opioid-like peptides derived from dietary proteins are detectable in urine and that these compounds may be pathophysiologically important in autism. A selective LC-MS/MS method was developed to analyze gliadinomorphin, beta-casomorphin, deltorphin 1, and deltorphin 2 in urine. The method is based on on-line SPE extraction of the neuropeptides from urine, column switching, and subsequent HPLC analysis. A limit of detection of 0.25 ng/mL was achieved for all analytes. Analyte recovery rates from urine ranged between 78% and 94%, with relative standard deviations of 0.2-6.8%. The method was used to screen 69 urine samples from children with and without autism spectrum disorders for the occurrence of neuropeptides. The target neuropeptides were not detected above the detection limit in either sample set.

Optofluidic laser for dual-mode sensitive biomolecular detection with a large dynamic range

NASA Astrophysics Data System (ADS)

Wu, Xiang; Oo, Maung Kyaw Khaing; Reddy, Karthik; Chen, Qiushu; Sun, Yuze; Fan, Xudong

2014-04-01

Enzyme-linked immunosorbent assay (ELISA) is a powerful method for biomolecular analysis. The traditional ELISA employing light intensity as the sensing signal often encounters large background arising from non-specific bindings, material autofluorescence and leakage of excitation light, which deteriorates its detection limit and dynamic range. Here we develop the optofluidic laser-based ELISA, where ELISA occurs inside a laser cavity. The laser onset time is used as the sensing signal, which is inversely proportional to the enzyme concentration and hence the analyte concentration inside the cavity. We first elucidate the principle of the optofluidic laser-based ELISA, and then characterize the optofluidic laser performance. Finally, we present the dual-mode detection of interleukin-6 using commercial ELISA kits, where the sensing signals are simultaneously obtained by the traditional and the optofluidic laser-based ELISA, showing a detection limit of 1 fg ml-1 (38 aM) and a dynamic range of 6 orders of magnitude.

Market analysis of food products for detection of allergenic walnut (Juglans regia) and pecan (Carya illinoinensis) by real-time PCR.

PubMed

López-Calleja, Inés María; de la Cruz, Silvia; González, Isabel; García, Teresa; Martín, Rosario

2015-06-15

Two real-time polymerase chain reaction (PCR)-based assays for detection of walnut (Juglans regia) and pecan (Carya illinoinensis) traces in a wide range of processed foods are described here. The method consists on a real-time PCR assay targeting the ITS1 region, using a nuclease (TaqMan) probe labeled with FAM and BBQ. The method was positive for walnut and pecan respectively, and negative for all other heterologous plants and animals tested. Using a series of model samples with defined raw walnut in wheat flour and heat-treated walnut in wheat flour with a range of concentrations of 0.1-100,000 mg kg(-1), a practical detection limit of 0.1 mg kg(-1) of walnut content was estimated. Identical binary mixtures were done for pecan, reaching the same limit of detection of 0.1 mg kg(-1). The assay was successfully trialed on a total of 232 commercial foodstuffs. Copyright © 2015 Elsevier Ltd. All rights reserved.

Advances in SAW gas sensors based on the condensate-adsorption effect.

PubMed

Liu, Jiuling; Wang, Wen; Li, Shunzhou; Liu, Minghua; He, Shitang

2011-01-01

A surface-acoustic-wave (SAW) gas sensor with a low detection limit and fast response for volatile organic compounds (VOCs) based on the condensate-adsorption effect detection is developed. In this sensor a gas chromatography (GC) column acts as the separator element and a dual-resonator oscillator acts as the detector element. Regarding the surface effective permittivity method, the response mechanism analysis, which relates the condensate-adsorption effect, is performed, leading to the sensor performance prediction prior to fabrication. New designs of SAW resonators, which act as feedback of the oscillator, are devised in order to decrease the insertion loss and to achieve single-mode control, resulting in superior frequency stability of the oscillator. Based on the new phase modulation approach, excellent short-term frequency stability (±3 Hz/s) is achieved with the SAW oscillator by using the 500 MHz dual-port resonator as feedback element. In a sensor experiment investigating formaldehyde detection, the implemented SAW gas sensor exhibits an excellent threshold detection limit as low as 0.38 pg.

Lectin functionalized ZnO nanoarrays as a 3D nano-biointerface for bacterial detection.

PubMed

Zheng, Laibao; Wan, Yi; Qi, Peng; Sun, Yan; Zhang, Dun; Yu, Liangmin

2017-05-15

The detection of pathogenic bacteria is essential in various fields, such as food safety, water environmental analysis, or clinical diagnosis. Although rapid and selective techniques have been achieved based on the fast and specific binding of recognitions elements and target, the sensitive detection of bacterial pathogens was limited by their low targets-binding efficiency. The three-dimensional (3D) nano-biointerface, compared with the two-dimensional (2D) flat substrate, has a much higher binding capacity, which can offer more reactive sites to bind with bacterial targets, resulting in a great improvement of detection sensitivity. Herein, a lectin functionalized ZnO nanorod (ZnO-NR) array has been fabricated and employed as a 3D nano-biointerface for Escherichia coli (E. coli) capture and detection by multivalent binding of concanavalin A (ConA) with polysaccharides on the cellular surface of E. coli. The 3D lectin functionalized ZnO-NR array-based assay shows reasonable detection limit and efficiently expanded linear range (1.0×10 3 to 1.0×10 7 cfumL -1 ) for pathogen detection. The platform has a potential for further applications and provides an excellent sensitivity approach for detection of pathogenic bacteria. Copyright © 2017 Elsevier B.V. All rights reserved.

Finite-size analysis of the detectability limit of the stochastic block model

NASA Astrophysics Data System (ADS)

Young, Jean-Gabriel; Desrosiers, Patrick; Hébert-Dufresne, Laurent; Laurence, Edward; Dubé, Louis J.

2017-06-01

It has been shown in recent years that the stochastic block model is sometimes undetectable in the sparse limit, i.e., that no algorithm can identify a partition correlated with the partition used to generate an instance, if the instance is sparse enough and infinitely large. In this contribution, we treat the finite case explicitly, using arguments drawn from information theory and statistics. We give a necessary condition for finite-size detectability in the general SBM. We then distinguish the concept of average detectability from the concept of instance-by-instance detectability and give explicit formulas for both definitions. Using these formulas, we prove that there exist large equivalence classes of parameters, where widely different network ensembles are equally detectable with respect to our definitions of detectability. In an extensive case study, we investigate the finite-size detectability of a simplified variant of the SBM, which encompasses a number of important models as special cases. These models include the symmetric SBM, the planted coloring model, and more exotic SBMs not previously studied. We conclude with three appendices, where we study the interplay of noise and detectability, establish a connection between our information-theoretic approach and random matrix theory, and provide proofs of some of the more technical results.

Development and Measurements of a Mid-Infrared Multi-Gas Sensor System for CO, CO₂ and CH₄ Detection.

PubMed

Dong, Ming; Zheng, Chuantao; Miao, Shuzhuo; Zhang, Yu; Du, Qiaoling; Wang, Yiding; Tittel, Frank K

2017-09-27

A multi-gas sensor system was developed that uses a single broadband light source and multiple carbon monoxide (CO), carbon dioxide (CO₂) and methane (CH₄) pyroelectric detectors by use of the time division multiplexing (TDM) technique. A stepper motor-based rotating system and a single-reflection spherical optical mirror were designed and adopted to realize and enhance multi-gas detection. Detailed measurements under static detection mode (without rotation) and dynamic mode (with rotation) were performed to study the performance of the sensor system for the three gas species. Effects of the motor rotating period on sensor performances were also investigated and a rotation speed of 0.4π rad/s was required to obtain a stable sensing performance, corresponding to a detection period of ~10 s to realize one round of detection. Based on an Allan deviation analysis, the 1 σ detection limits under static operation are 2.96, 4.54 and 2.84 parts per million in volume (ppmv) for CO, CO₂ and CH₄, respectively and the 1 σ detection limits under dynamic operations are 8.83, 8.69 and 10.29 ppmv for the three gas species, respectively. The reported sensor has potential applications in various fields requiring CO, CO₂ and CH₄ detection such as in coal mines.

Laser-induced fluorescence spectroscopy for improved chemical analysis

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

Gelbwachs, J.A.

1983-09-01

This report summarizes the progress achieved over the past five years in the laser-induced fluorescence spectroscopy (LIFS) for improved chemical analysis program. Our initial efforts yielded significantly lower detection limits for trace elemental analysis by the use of both cw and pulsed laser excitations. New methods of LIFS were developed that were shown to overcome many of the traditional limitations to LIFS techniques. LIFS methods have been applied to yield fundamental scientific data that further the understanding of forces between atoms and other atoms and molecules. In recent work, two-photon ionization was combined with LIFS and applied, for the firstmore » time, to the study of energy transfer in ions.« less

A Sensitive DNA Capacitive Biosensor Using Interdigitated Electrodes

PubMed Central

Wang, Lei; Veselinovic, Milena; Yang, Lang; Geiss, Brian J.; Dandy, David S.; Chen, Tom

2017-01-01

This paper presents a label-free affinity-based capacitive biosensor using interdigitated electrodes. Using an optimized process of DNA probe preparation to minimize the effect of contaminants in commercial thiolated DNA probe, the electrode surface was functionalized with the 24-nucleotide DNA probes based on the West Nile virus sequence (Kunjin strain). The biosensor has the ability to detect complementary DNA fragments with a detection limit down to 20 DNA target molecules (1.5 aM range), making it suitable for a practical point-of-care (POC) platform for low target count clinical applications without the need for amplification. The reproducibility of the biosensor detection was improved with efficient covalent immobilization of purified single-stranded DNA probe oligomers on cleaned gold microelectrodes. In addition to the low detection limit, the biosensor showed a dynamic range of detection from 1 μL−1 to 105 μL−1 target molecules (20 to 2 million targets), making it suitable for sample analysis in a typical clinical application environment. The binding results presented in this paper were validated using fluorescent oligomers. PMID:27619528

Multiplexed BioCD for prostate specific antigen detection

NASA Astrophysics Data System (ADS)

Wang, Xuefeng; Zhao, Ming; Nolte, David D.

2008-02-01

Specific protein concentrations in human body fluid can serve as diagnostic markers for some diseases, and a quantitative and high-throughput technique for multiplexed protein detection would speed up diagnosis and facilitate medical research. For this purpose, our group developed the BioCD, a spinning-disc interferometric biosensor on which antibody is immobilized. The detection system adopts a common-path scheme making it ultra stable. The scaling mass sensitivity is below 10 pg/mm for protein surface density. A 25000-spot antibody BioCD was fabricated to measure the concentration of prostate specific antigen (PSA), a protein indicating prostate cancer if its level is high. Statistical analysis of our immunoassay results projects that the detection limit of PSA would reach 20 pg/ml in a 2 mg/ml background solution. For future prospects, a multiplexed BioCD can be produced for simultaneous diagnosis of diverse diseases. For instance, 100 markers above 200 pg/ml could be measured on a single disc given that the detection limit is inversely proportional to square root of the number of spots.

Development of a lab-on-chip electrochemical immunosensor for detection of Polycyclic Aromatic Hydrocarbons (PAH) in environmental water

NASA Astrophysics Data System (ADS)

Felemban, Shifa; Vazquez, Patricia; Dehnert, Jan; Goridko, Vadim; Tijero, Maria; Moore, Eric

2017-06-01

The work described in this manuscript focuses on how the integration of immunoassay techniques in combination with electrochemical detection can provide a portable and very accurate solution for detection of water pollutants that are detrimental for human health. In particular, we focus our work on the quantification of polycyclic aromatic hydrocarbons (PAHs) in polluted water. Our integrative approach facilitates a real-time detection of this family of organic compounds, by reducing the time of analysis to less than one hour. Additionally, the use of a lab-on-a-chip platform delivers a portable solution that could be used in situ. Optimization of a displacement assay that investigates the presence and concentration of Benzo[a]pyrene in water, allows with the miniaturization of the standard ELISA format into a highly accurate system that provides fast results. The limits of detection obtained are comparable to those of available state-of-the art tools, and achieve the values set by European Drinking Water Directive, 0.10ng/l, as the limit for PAHs in drinking water.

Comprehensive sample analysis using high performance liquid chromatography with multi-detection.

PubMed

Pravadali, Sercan; Bassanese, Danielle N; Conlan, Xavier A; Francis, Paul S; Smith, Zoe M; Terry, Jessica M; Shalliker, R Andrew

2013-11-25

Herein we assess the separation space offered by a liquid chromatography system with an optimised uni-dimensional separation for the determination of the key chemical entities in the highly complex matrix of a tobacco leaf extract. Multiple modes of detection, including UV-visible absorbance, chemiluminescence (acidic potassium permanganate, manganese(IV), and tris(2,2'-bipyridine)ruthenium(III)), mass spectrometry and DPPH radical scavenging were used in an attempt to systematically reduce the data complexity of the sample whilst obtaining a greater degree of molecule-specific information. A large amount of chemical data was obtained, but several limitations in the ability to assign detector responses to particular compounds, even with the aid of complementary detection systems, were observed. Thirty-three compounds were detected via MS on the tobacco extract and 12 out of 32 compounds gave a peak height ratio (PHR) greater than 0.33 on one or more detectors. This paper serves as a case study of these limitations, illustrating why multidimensional chromatography is an important consideration when developing a comprehensive chemical detection system. Copyright © 2013 Elsevier B.V. All rights reserved.

An automatic device for detection and classification of malaria parasite species in thick blood film.

PubMed

Kaewkamnerd, Saowaluck; Uthaipibull, Chairat; Intarapanich, Apichart; Pannarut, Montri; Chaotheing, Sastra; Tongsima, Sissades

2012-01-01

Current malaria diagnosis relies primarily on microscopic examination of Giemsa-stained thick and thin blood films. This method requires vigorously trained technicians to efficiently detect and classify the malaria parasite species such as Plasmodium falciparum (Pf) and Plasmodium vivax (Pv) for an appropriate drug administration. However, accurate classification of parasite species is difficult to achieve because of inherent technical limitations and human inconsistency. To improve performance of malaria parasite classification, many researchers have proposed automated malaria detection devices using digital image analysis. These image processing tools, however, focus on detection of parasites on thin blood films, which may not detect the existence of parasites due to the parasite scarcity on the thin blood film. The problem is aggravated with low parasitemia condition. Automated detection and classification of parasites on thick blood films, which contain more numbers of parasite per detection area, would address the previous limitation. The prototype of an automatic malaria parasite identification system is equipped with mountable motorized units for controlling the movements of objective lens and microscope stage. This unit was tested for its precision to move objective lens (vertical movement, z-axis) and microscope stage (in x- and y-horizontal movements). The average precision of x-, y- and z-axes movements were 71.481 ± 7.266 μm, 40.009 ± 0.000 μm, and 7.540 ± 0.889 nm, respectively. Classification of parasites on 60 Giemsa-stained thick blood films (40 blood films containing infected red blood cells and 20 control blood films of normal red blood cells) was tested using the image analysis module. By comparing our results with the ones verified by trained malaria microscopists, the prototype detected parasite-positive and parasite-negative blood films at the rate of 95% and 68.5% accuracy, respectively. For classification performance, the thick blood films with Pv parasite was correctly classified with the success rate of 75% while the accuracy of Pf classification was 90%. This work presents an automatic device for both detection and classification of malaria parasite species on thick blood film. The system is based on digital image analysis and featured with motorized stage units, designed to easily be mounted on most conventional light microscopes used in the endemic areas. The constructed motorized module could control the movements of objective lens and microscope stage at high precision for effective acquisition of quality images for analysis. The analysis program could accurately classify parasite species, into Pf or Pv, based on distribution of chromatin size.

SAMPLING AND ANALYSIS OF MERCURY IN CRUDE OIL

EPA Science Inventory

Sampling and analytical procedures used to determine total mercury content in crude oils were examined. Three analytical methods were compared with respect to accuracy, precision and detection limit. The combustion method and a commercial extraction method were found adequate to...

40 CFR Appendix B to Part 136 - Definition and Procedure for the Determination of the Method Detection Limit-Revision 1.11

Code of Federal Regulations, 2010 CFR

2010-07-01

... calculated method detection limit. To insure that the estimate of the method detection limit is a good...) where: MDL = the method detection limit t(n-1,1- α=.99) = the students' t value appropriate for a 99... Determination of the Method Detection Limit-Revision 1.11 B Appendix B to Part 136 Protection of Environment...

A Simple Method for Rapid Depletion of Rubisco from Soybean (Glycine max) Leaf for Proteomic Analysis of Lower Abundance Proteins

USDA-ARS?s Scientific Manuscript database

2-DE analysis of complex plant proteomes has limited dynamic resolution because only abundant proteins can be detected. Proteomic assessment of the low abundance proteins within leaf tissue is difficult when it is comprised of 30 – 50% of the CO2 fixation enzyme Rubisco. Resolution can be improved t...

A gold nanoparticle-based semi-quantitative and quantitative ultrasensitive paper sensor for the detection of twenty mycotoxins

NASA Astrophysics Data System (ADS)

Kong, Dezhao; Liu, Liqiang; Song, Shanshan; Suryoprabowo, Steven; Li, Aike; Kuang, Hua; Wang, Libing; Xu, Chuanlai

2016-02-01

A semi-quantitative and quantitative multi-immunochromatographic (ICA) strip detection assay was developed for the simultaneous detection of twenty types of mycotoxins from five classes, including zearalenones (ZEAs), deoxynivalenols (DONs), T-2 toxins (T-2s), aflatoxins (AFs), and fumonisins (FBs), in cereal food samples. Sensitive and specific monoclonal antibodies were selected for this assay. The semi-quantitative results were obtained within 20 min by the naked eye, with visual limits of detection for ZEAs, DONs, T-2s, AFs and FBs of 0.1-0.5, 2.5-250, 0.5-1, 0.25-1 and 2.5-10 μg kg-1, and cut-off values of 0.25-1, 5-500, 1-10, 0.5-2.5 and 5-25 μg kg-1, respectively. The quantitative results were obtained using a hand-held strip scan reader, with the calculated limits of detection for ZEAs, DONs, T-2s, AFs and FBs of 0.04-0.17, 0.06-49, 0.15-0.22, 0.056-0.49 and 0.53-1.05 μg kg-1, respectively. The analytical results of spiked samples were in accordance with the accurate content in the simultaneous detection analysis. This newly developed ICA strip assay is suitable for the on-site detection and rapid initial screening of mycotoxins in cereal samples, facilitating both semi-quantitative and quantitative determination.A semi-quantitative and quantitative multi-immunochromatographic (ICA) strip detection assay was developed for the simultaneous detection of twenty types of mycotoxins from five classes, including zearalenones (ZEAs), deoxynivalenols (DONs), T-2 toxins (T-2s), aflatoxins (AFs), and fumonisins (FBs), in cereal food samples. Sensitive and specific monoclonal antibodies were selected for this assay. The semi-quantitative results were obtained within 20 min by the naked eye, with visual limits of detection for ZEAs, DONs, T-2s, AFs and FBs of 0.1-0.5, 2.5-250, 0.5-1, 0.25-1 and 2.5-10 μg kg-1, and cut-off values of 0.25-1, 5-500, 1-10, 0.5-2.5 and 5-25 μg kg-1, respectively. The quantitative results were obtained using a hand-held strip scan reader, with the calculated limits of detection for ZEAs, DONs, T-2s, AFs and FBs of 0.04-0.17, 0.06-49, 0.15-0.22, 0.056-0.49 and 0.53-1.05 μg kg-1, respectively. The analytical results of spiked samples were in accordance with the accurate content in the simultaneous detection analysis. This newly developed ICA strip assay is suitable for the on-site detection and rapid initial screening of mycotoxins in cereal samples, facilitating both semi-quantitative and quantitative determination. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr09171c

Comparison of different amino acid derivatives and analysis of rat brain microdialysates by liquid chromatography tandem mass spectrometry.

PubMed

Uutela, Päivi; Ketola, Raimo A; Piepponen, Petteri; Kostiainen, Risto

2009-02-09

The efficiencies of three derivatisation reagents that react with either the amine (9-fluorenylmethyl chloroformate (FMOC)) or the carboxylic acid group (butanol) of amino acid or with both types of functional groups (propyl chloroformate) were compared in the analysis of amino acids by liquid chromatography-electrospray-tandem mass spectrometry (LC-ESI-MS/MS). Separation of 20 amino acids derivatised with these three reagents was studied on reversed-phase chromatography. Linearity, repeatability and limits of detection of the LC-ESI-MS/MS method were determined by analysing FMOC-, butanol- and propyl chloroformate-derivatised lysine, beta-aminobutyric acid, threonine and glutamic acid. The limits of detection for the derivatised amino acids (7.5-75fmol) were as much as 2-60 times lower than those of the corresponding underivatised molecules. The best linearity was observed for amino acids derivatised with propyl chloroformate or butanol (r(2)=0.996-0.999, range=100-8500nmolL(-1)). Propyl chloroformate was the best suited of the reagents tested for the analysis of amino acids with LC-MS/MS and was used for the analysis of amino acids in rat brain microdialysis samples.

Material limitations on the detection limit in refractometry.

PubMed

Skafte-Pedersen, Peder; Nunes, Pedro S; Xiao, Sanshui; Mortensen, Niels Asger

2009-01-01

We discuss the detection limit for refractometric sensors relying on high-Q optical cavities and show that the ultimate classical detection limit is given by min {Δn} ≳ η, with n + iη being the complex refractive index of the material under refractometric investigation. Taking finite Q factors and filling fractions into account, the detection limit declines. As an example we discuss the fundamental limits of silicon-based high-Q resonators, such as photonic crystal resonators, for sensing in a bio-liquid environment, such as a water buffer. In the transparency window (λ ≳ 1100 nm) of silicon the detection limit becomes almost independent on the filling fraction, while in the visible, the detection limit depends strongly on the filling fraction because the silicon absorbs strongly.

Simultaneous detection of creatine and creatinine using a sequential injection analysis/biosensor system.

PubMed

Stefan-van Staden, Raluca-Ioana; Bokretsion, Rahel Girmai; van Staden, Jacobus F; Aboul-Enein, Hassan Y

2006-01-01

Carbon paste based biosensors for the determination of creatine and creatinine have been integrated into a sequential injection system. Applying the multi-enzyme sequence of creatininase (CA), and/or creatinase (CI) and sarcosine oxidase (SO), hydrogen peroxide has been detected amperometrically. The linear concentration ranges are of pmol/L to nmol/L magnitude, with very low limits of detection. The proposed SIA system can be utilized reliably for the on-line simultaneous detection of creatine and creatinine in pharmaceutical products, as well as in serum samples, with a rate of 34 samples per hour and RSD values better than 0.16% (n=10).

Receiver operating characteristic analysis. Application to the study of quantum fluctuation effects in optic nerve of Rana pipiens

PubMed Central

1975-01-01

Receiver operating characteristic (ROC) analysis of nerve messages is described. The hypothesis that quantum fluctuations provide the only limit to the ability of frog ganglion cells to signal luminance change information is examined using ROC analysis. In the context of ROC analysis, the quantum fluctuation hypothesis predicts (a) the detectability of a luminance change signal should rise proportionally to the size of the change, (b) detectability should decrease as the square root of background, an implication of which is the deVries-Rose law, and (c) ROC curves should exhibit a shape particular to underlying Poisson distributions. Each of these predictions is confirmed for the responses of dimming ganglion cells to brief luminance decrements at scotopic levels, but none could have been tested using classical nerve message analysis procedures. PMID:172597

Adaptive non-interventional heuristics for covariation detection in causal induction: model comparison and rational analysis.

PubMed

Hattori, Masasi; Oaksford, Mike

2007-09-10

In this article, 41 models of covariation detection from 2 × 2 contingency tables were evaluated against past data in the literature and against data from new experiments. A new model was also included based on a limiting case of the normative phi-coefficient under an extreme rarity assumption, which has been shown to be an important factor in covariation detection (McKenzie & Mikkelsen, 2007) and data selection (Hattori, 2002; Oaksford & Chater, 1994, 2003). The results were supportive of the new model. To investigate its explanatory adequacy, a rational analysis using two computer simulations was conducted. These simulations revealed the environmental conditions and the memory restrictions under which the new model best approximates the normative model of covariation detection in these tasks. They thus demonstrated the adaptive rationality of the new model. 2007 Cognitive Science Society, Inc.

The fabrication of magnetic particle-based chemiluminescence immunoassay for human epididymis protein-4 detection in ovarian cancer.

PubMed

Fu, Xiaoling; Liu, Yangyang; Qiu, Ruiyun; Foda, Mohamed F; Zhang, Yong; Wang, Tao; Li, Jinshan

2018-03-01

The magnetic particles have a significant influence on the immunoassay detection and cancer therapy. Herein, the chemiluminescence immunoassay combined with the magnetic particles (MPCLIA) was presented for the clinical determination and analysis of human epididymis protein 4 (HE4) in the human serum. Under the optimized experiment conditions, the secure MPCLIA method can detect HE4 in the broader range of 0-1000 pmol/L, with a lower detection limit of 1.35 pmol/L. The satisfactory recovery rate of the method in the serum ranged from 83.62% to 105.10%, which was well within the requirement of clinical analysis. Moreover, the results showed the good correlation with enzyme-linked immunosorbent assay (ELISA), with the correlation coefficient of 0.9589. This proposed method has been successfully applied to the clinical determination of HE4 in the human serum.

Effect of modulation of the particle size distributions in the direct solid analysis by total-reflection X-ray fluorescence

NASA Astrophysics Data System (ADS)

Fernández-Ruiz, Ramón; Friedrich K., E. Josue; Redrejo, M. J.

2018-02-01

The main goal of this work was to investigate, in a systematic way, the influence of the controlled modulation of the particle size distribution of a representative solid sample with respect to the more relevant analytical parameters of the Direct Solid Analysis (DSA) by Total-reflection X-Ray Fluorescence (TXRF) quantitative method. In particular, accuracy, uncertainty, linearity and detection limits were correlated with the main parameters of their size distributions for the following elements; Al, Si, P, S, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, As, Se, Rb, Sr, Ba and Pb. In all cases strong correlations were finded. The main conclusion of this work can be resumed as follows; the modulation of particles shape to lower average sizes next to a minimization of the width of particle size distributions, produce a strong increment of accuracy, minimization of uncertainties and limit of detections for DSA-TXRF methodology. These achievements allow the future use of the DSA-TXRF analytical methodology for development of ISO norms and standardized protocols for the direct analysis of solids by mean of TXRF.

Analysis of biogenic amines using corona discharge ion mobility spectrometry.

PubMed

Hashemian, Z; Mardihallaj, A; Khayamian, T

2010-05-15

A new method based on corona discharge ion mobility spectrometry (CD-IMS) was developed for the analysis of biogenic amines including spermidine, spermine, putrescine, and cadaverine. The ion mobility spectra of the compounds were obtained with and without n-Nonylamine used as the reagent gas. The high proton affinity of n-Nonylamine prevented ion formation from compounds with a proton affinity lower than that of n-Nonylamine and, therefore, enhanced its selectivity. It was also realized that the ion mobility spectrum of n-Nonylamine varied with its concentration. A sample injection port of a gas chromatograph was modified and used as the sample introduction system into the CD-IMS. The detection limits, dynamic ranges, and analytical parameters of the compounds with and without using the reagent gas were obtained. The detection limits and dynamic ranges of the compounds were about 2ng and 2 orders of magnitude, respectively. The wide dynamic range of CD-IMS originates from the high current of the corona discharge. The results revealed the high capability of the CD-IMS for the analysis of biogenic amines.

Laser-based absorption spectroscopy as a technique for rapid in-line analysis of respired gas concentrations of O2 and CO2

PubMed Central

Cummings, Beth; Hamilton, Michelle L.; Ciaffoni, Luca; Pragnell, Timothy R.; Peverall, Rob; Ritchie, Grant A. D.; Hancock, Gus

2011-01-01

The use of sidestream analyzers for respired gas analysis is almost universal. However, they are not ideal for measurements of respiratory gas exchange because the analyses are both temporally dissociated from measurements of respiratory flow and also not generally conducted under the same physical conditions. This study explores the possibility of constructing an all optical, fast response, in-line breath analyzer for oxygen and carbon dioxide. Using direct absorption spectroscopy with a diode laser operating at a wavelength near 2 μm, measurements of expired carbon dioxide concentrations were obtained with an absolute limit of detection of 0.04% at a time resolution of 10 ms. Simultaneously, cavity enhanced absorption spectroscopy at a wavelength near 760 nm was employed to obtain measurements of expired oxygen concentrations with an absolute limit of detection of 0.26% at a time resolution of 10 ms. We conclude that laser-based absorption spectroscopy is a promising technology for in-line analysis of respired carbon dioxide and oxygen concentrations. PMID:21512147

Laser-based absorption spectroscopy as a technique for rapid in-line analysis of respired gas concentrations of O2 and CO2.

PubMed

Cummings, Beth; Hamilton, Michelle L; Ciaffoni, Luca; Pragnell, Timothy R; Peverall, Rob; Ritchie, Grant A D; Hancock, Gus; Robbins, Peter A

2011-07-01

The use of sidestream analyzers for respired gas analysis is almost universal. However, they are not ideal for measurements of respiratory gas exchange because the analyses are both temporally dissociated from measurements of respiratory flow and also not generally conducted under the same physical conditions. This study explores the possibility of constructing an all optical, fast response, in-line breath analyzer for oxygen and carbon dioxide. Using direct absorption spectroscopy with a diode laser operating at a wavelength near 2 μm, measurements of expired carbon dioxide concentrations were obtained with an absolute limit of detection of 0.04% at a time resolution of 10 ms. Simultaneously, cavity enhanced absorption spectroscopy at a wavelength near 760 nm was employed to obtain measurements of expired oxygen concentrations with an absolute limit of detection of 0.26% at a time resolution of 10 ms. We conclude that laser-based absorption spectroscopy is a promising technology for in-line analysis of respired carbon dioxide and oxygen concentrations.

Cryogenic Collection of Complete Subsurface Samples for Molecular Biological Analysis

DTIC Science & Technology

2012-05-01

Nitrate was analyzed by ion chromatography ( Dionex IC25) and had a detection limit of 0.01 mg/L. Fluorescein was measured using a flow-through...dissolved oxygen (DO) with a flow through electrode, Nitrate by ion chromatography , and fluorescein with a flow through fluorometer. 1.9 LARGE...measured by headspace gas chromatography (HP 7694 Headspace Sampler attached to an HP 5890 GC with an FID detector). The GC method had a detection

Upper limits on the 21 cm power spectrum at z = 5.9 from quasar absorption line spectroscopy

NASA Astrophysics Data System (ADS)

Pober, Jonathan C.; Greig, Bradley; Mesinger, Andrei

2016-11-01

We present upper limits on the 21 cm power spectrum at z = 5.9 calculated from the model-independent limit on the neutral fraction of the intergalactic medium of x_{H I} < 0.06 + 0.05 (1σ ) derived from dark pixel statistics of quasar absorption spectra. Using 21CMMC, a Markov chain Monte Carlo Epoch of Reionization analysis code, we explore the probability distribution of 21 cm power spectra consistent with this constraint on the neutral fraction. We present 99 per cent confidence upper limits of Δ2(k) < 10-20 mK2 over a range of k from 0.5 to 2.0 h Mpc-1, with the exact limit dependent on the sampled k mode. This limit can be used as a null test for 21 cm experiments: a detection of power at z = 5.9 in excess of this value is highly suggestive of residual foreground contamination or other systematic errors affecting the analysis.

A review of electrochemiluminescence (ECL) in and for microfluidic analytical devices.

PubMed

Kirschbaum, Stefanie E K; Baeumner, Antje J

2015-05-01

The concept and realization of microfluidic total analysis systems (microTAS) have revolutionized the analytical process by integrating the whole breadth of analytical techniques into miniaturized systems. Paramount for efficient and competitive microTAS are integrated detection strategies, which lead to low limits of detection while reducing the sample volume. The concept of electrochemiluminescence (ECL) has been intriguing ever since its introduction based on Ru(bpy)3 (2+) by Tokel and Bard [1] (J Am Chem Soc 1853:2862-2863, 1972), especially because of its immense sensitivity, nonexistent auto-luminescent background signal, and simplicity in experimental design. Therefore, integrating ECL detection into microTAS is a logical consequence to achieve simple, yet highly sensitive, sensors. However, published microanalytical devices employing ECL detection focus in general on traditional ECL chemistry and have yet to take advantage of advances made in standard bench-top ECL strategies. This review will therefore focus on the most recent advancements in microfluidic ECL approaches, but also evaluate the potential impact of bench-top ECL research progress that would further improve performance and lower limits of detection of micro analytical ECL systems, ensuring their desirability as detection principle for microTAS applications.

Remote-controlled robotic platform ORPHEUS as a new tool for detection of bacteria in the environment.

PubMed

Nejdl, Lukas; Kudr, Jiri; Cihalova, Kristyna; Chudobova, Dagmar; Zurek, Michal; Zalud, Ludek; Kopecny, Lukas; Burian, Frantisek; Ruttkay-Nedecky, Branislav; Krizkova, Sona; Konecna, Marie; Hynek, David; Kopel, Pavel; Prasek, Jan; Adam, Vojtech; Kizek, Rene

2014-08-01

Remote-controlled robotic systems are being used for analysis of various types of analytes in hostile environment including those called extraterrestrial. The aim of our study was to develop a remote-controlled robotic platform (ORPHEUS-HOPE) for bacterial detection. For the platform ORPHEUS-HOPE a 3D printed flow chip was designed and created with a culture chamber with volume 600 μL. The flow rate was optimized to 500 μL/min. The chip was tested primarily for detection of 1-naphthol by differential pulse voltammetry with detection limit (S/N = 3) as 20 nM. Further, the way how to capture bacteria was optimized. To capture bacterial cells (Staphylococcus aureus), maghemite nanoparticles (1 mg/mL) were prepared and modified with collagen, glucose, graphene, gold, hyaluronic acid, and graphene with gold or graphene with glucose (20 mg/mL). The most up to 50% of the bacteria were captured by graphene nanoparticles modified with glucose. The detection limit of the whole assay, which included capturing of bacteria and their detection under remote control operation, was estimated as 30 bacteria per μL. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A fully automated microfluidic-based electrochemical sensor for real-time bacteria detection.

PubMed

Altintas, Zeynep; Akgun, Mete; Kokturk, Guzin; Uludag, Yildiz

2018-02-15

A fully automated microfluidic-based electrochemical biosensor was designed and manufactured for pathogen detection. The quantification of Escherichia coli was investigated with standard and nanomaterial amplified immunoassays in the concentration ranges of 0.99 × 10 4 3.98 × 10 9 cfu mL -1 and 103.97 × 10 7 cfu mL -1 which resulted in detection limits of 1.99 × 10 4 cfu mL -1 and 50 cfu mL -1 , respectively. The developed methodology was then applied for E. coli quantification in water samples using nanomaterial modified assay. Same detection limit for E. coli was achieved for real sample analysis with a little decrease on the sensor signal. Cross-reactivity studies were conducted by testing Shigella, Salmonella spp., Salmonella typhimurium and Staphylococcus aureus on E. coli specific antibody surface that confirmed the high specificity of the developed immunoassays. The sensor surface could be regenerated multiple times which significantly reduces the cost of the system. Our custom-designed biosensor is capable of detecting bacteria with high sensitivity and specificity, and can serve as a promising tool for pathogen detection. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of a laser induced breakdown spectrometer for detection of toxic elements in cosmetic products

NASA Astrophysics Data System (ADS)

Maganda, Yasin Wandhami

In this research work we developed a highly sensitive analytical Laser Induced Breakdown Spectrometer to detect toxic elements in commercially available cosmetic products. These products are frequently used by many all over the world, therefore there is an increasing demand to determine concentration levels of toxic elements present in them because they cause dangerous diseases and most of them are highly carcinogenic and life threatening. Laser Induced Breakdown Spectroscopy (LIBS) was applied for spectroscopic analysis of cosmetic products such as tooth paste, synthetic hair dye, kohl eyeliners and talcum powder samples. These samples were purchased from the local market within the kingdom of Saudi Arabia. The LIBS method is based on spectroscopic analysis of plasma resulting from the interaction of a high power pulsed laser radiations with a sample medium. In order to improve the sensitivity of the spectrometer, the dependence of the LIBS signal intensity and plasma parameters such as temperature (T) and electron density (ne) on gate/time delay, laser fluence and wavelength of the excitation source for plasma generated under ambient conditions were studied. During this work Nd: YAG lasers having 266nm, 532 nm and 1064 nm wavelengths operating in Q-switch mode were used as the excitation sources in combination with a spectrograph having a gated ICCD camera. Boltzmann plots and stark broadening for the recorded spectral lines were used to estimate the plasma temperature and electron density respectively. Temporal evolution of the plasma temperature and electron density showed a t-2 dependence. On the other hand plasma temperature and electron density increased with increase in laser fluence but leveled off at higher fluencies. It is worth noting that in both cases 266 nm and 1064 nm excitation wavelengths consistently had the highest and lowest values respectively. Therefore a 266 nm wavelength Nd: YAG laser excitation source was selected to develop a highly sensitive Laser Induced Breakdown spectrometer to detect and quantify the fluoride (F), lead (Pb) and chromium (Cr) content in commercially available toothpaste, synthetic hair dye, kohl eyeliners and talcum powder samples. The experimental parameters such as gate/ delays and laser fluencies were optimized to achieve an optically thin and in local thermodynamic equilibrium plasma (L.T.E) which improved the limit of detection of our spectrometer. The choice of the parameters was validated using the Mcwhirter criterion. For fluoride detection in the toothpaste samples, a strong atomic transition line of fluorine at 731.102 nm was used as the marker line. The LIBS system was able to detect fluoride concentration levels in the range of 1300 - 1750 ppm with a detection limit of 156ppm.In the synthetic hair dye, chromium was detected using a strong atomic transition of chromium (Cr) at a wavelength 427.5 nm as the spectral marker line and the spectrometer with a detection limit of 1.2 ppm was able to detect chromium concentration levels in the range of 5-11 ppm. These results achieved with our LIBS system were compared with those obtained using a standard detection method such as ICP-MS. The results obtained are in excellent agreement with ICP-MS. Lead (Pb) and Chromium (Cr) in kohl were detected using atomic transitions at wavelengths of 405.7 nm and 425.4 nm respectively as the spectral marker lines. The system was calibrated for these toxic metals and it was able to detect Lead and Chromium in the range of 5-14 ppm and 4-9 ppm with detection limits of 1ppm and 2 ppm respectively. The LIBS results were compared with those obtained using ICP-MS and were in good agreement yielding a relative accuracy in the range 0.05-0.3 which is acceptable. Lead (Pb) and Chromium (Cr) levels in talcum powder samples were detected and quantified using strong transitions at wavelengths of 405.7 nm and 425.4 nm respectively. The LIBS system detected lead and chromium in the range of 15-17 ppm and 23-29 ppm with limits of detection of 1.96 ppm and 1.72 ppm respectively. The concentration levels of fluoride, lead and chromium detected using our LIBS system exceeded the permissible limits set by the Environmental agency and other regulatory organization and hence frequent use of such cosmetic products can be hazardous to human health. The LIBS spectrometer developed through this research work can be applied for analysis of many other samples like pharmaceutical, polymers, iron, volcanic eruption and geological samples for mineral quantification.

Large strain cruciform biaxial testing for FLC detection

NASA Astrophysics Data System (ADS)

Güler, Baran; Efe, Mert

2017-10-01

Selection of proper test method, specimen design and analysis method are key issues for studying formability of sheet metals and detection of their forming limit curves (FLC). Materials with complex microstructures may need an additional micro-mechanical investigation and accurate modelling. Cruciform biaxial test stands as an alternative to standard tests as it achieves frictionless, in-plane, multi-axial stress states with a single sample geometry. In this study, we introduce a small-scale (less than 10 cm) cruciform sample allowing micro-mechanical investigation at stress states ranging from plane strain to equibiaxial. With successful specimen design and surface finish, large forming limit strains are obtained at the test region of the sample. The large forming limit strains obtained by experiments are compared to the values obtained from Marciniak-Kuczynski (M-K) local necking model and Cockroft-Latham damage model. This comparison shows that the experimental limiting strains are beyond the theoretical values, approaching to the fracture strain of the two test materials: Al-6061-T6 aluminum alloy and DC-04 high formability steel.

Determination of Total Petroleum Hydrocarbons in Australian Groundwater Through the Improvised Gas Chromatography-Flame Ionization Detection Technique.

PubMed

Faustorilla, Maria Vilma; Chen, Zuliang; Dharmarajan, Rajarathnam; Naidu, Ravendra

2017-09-01

Assessment of total petroleum hydrocarbons (TPHs) from contaminated sites demands routine and reliable measurement at trace levels. However, the detection limits of these methods need to be improved. This study developed the programmable temperature vaporization-large volume injection (PTV-LVI) method to quantify TPHs through gas chromatography-flame ionization detection. This configuration enhances the method sensitivity for trace level detections through large volume injections and pre-concentration of analytes along the injection liner. The method was evaluated for the three commonly observed hydrocarbon fractions: C10-C14, C15-C28 and C29-C36. In comparison with conventional injection methods (splitless and pulsed splitless), PTV-LVI showed R2 values > 0.999 with enhanced limits of detection and limits of quantification values. The method was applied to real samples for routine environmental monitoring of TPHs in an Australian contaminated site characterized by refueling station. Analysis of groundwater samples in the area showed a wide range of TPH concentrations as follows: 66-1,546,000 (C10-C14), 216-22,762 (C15-C28) and 105-2,103 (C29-C36) μg/L. This method has detected trace levels, thereby measuring a wider concentration range of TPHs. These more accurate measurements can lead to the appropriate application of risk assessments and remediation techniques. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Development and validation of a solid-phase extraction method coupled to liquid chromatography with fluorescence detection for the determination of fluoroquinolone residues in powdered infant formulae. Application to the analysis of samples from the Spanish and Latin American market.

PubMed

Rodriguez, E; Moreno-Bondi, M C; Marazuela, M D

2008-10-31

This paper describes a new method for the effective extraction, clean-up and chromatographic analysis of residues of four fluoroquinolones (ciprofloxacin, enrofloxacin, danofloxacin and sarafloxacin) in powdered infant formulae and follow-on preparations. Samples were reconstituted following the manufacturer's recommendations and treated with trichloroacetic acid in methanol 10% (w/v) for deproteinization. Two solid-phase extraction cartridges have been evaluated for sample clean-up and preconcentration, Strata Screen A and Strata X and the later provided the best recoveries for all the analytes tested. Chromatographic analysis has been carried out using a polar endcapped column (AQUA C(18)) and fluorescence detection, with lomefloxacin (LOME) as internal standard. Method validation has been performed according to European Commission Decision 2002/657/EC criteria, in terms of linearity, recovery, precision, specificity, decision limit (CC(alpha)) and detection capability (CC(beta)). Typical recoveries ranged between 70 and 110% at levels below and above the maximum residue limits of the target analytes in bovine milk, with an excellent intralab reproducibility (RSDs<7%). Matrix effects did not significantly affect method accuracy, as evidenced by analyzing different brands of milk. The method has been successfully applied to the analysis of 100 samples of infant and follow-on formulae of the Spanish and Latin American market, using LC-MS/MS as confirmatory technique.

Sample preparation for arsenic speciation analysis in baby food by generation of substituted arsines with atomic absorption spectrometry detection.

PubMed

Huber, Charles S; Vale, Maria Goreti R; Dessuy, Morgana B; Svoboda, Milan; Musil, Stanislav; Dědina, Jiři

2017-12-01

A slurry sampling procedure for arsenic speciation analysis in baby food by arsane generation, cryogenic trapping and detection with atomic absorption spectrometry is presented. Several procedures were tested for slurry preparation, including different reagents (HNO 3 , HCl and tetramethylammonium hydroxide - TMAH) and their concentrations, water bath heating and ultrasound-assisted agitation. The best results for inorganic arsenic (iAs) and dimethylarsinate (DMA) were reached when using 3molL -1 HCl under heating and ultrasound-assisted agitation. The developed method was applied for the analysis of five porridge powder and six baby meal samples. The trueness of the method was checked with a certified reference material (CRM) of total arsenic (tAs), iAs and DMA in rice (ERM-BC211). Arsenic recoveries (mass balance) for all samples and CRM were performed by the determination of the tAs by inductively coupled plasma mass spectrometry (ICP-MS) after microwave-assisted digestion and its comparison against the sum of the results from the speciation analysis. The relative limits of detection were 0.44, 0.24 and 0.16µgkg -1 for iAs, methylarsonate and DMA, respectively. The concentrations of the most toxic arsenic species (iAs) in the analyzed baby food samples ranged between 4.2 and 99µgkg -1 which were below the limits of 300, 200 and 100µgkg -1 set by the Brazilian, Chinese and European legislation, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Label-free and high-sensitive detection for genetic point mutation based on hyperspectral interferometry

NASA Astrophysics Data System (ADS)

Fu, Rongxin; Li, Qi; Zhang, Junqi; Wang, Ruliang; Lin, Xue; Xue, Ning; Su, Ya; Jiang, Kai; Huang, Guoliang

2016-10-01

Label free point mutation detection is particularly momentous in the area of biomedical research and clinical diagnosis since gene mutations naturally occur and bring about highly fatal diseases. In this paper, a label free and high sensitive approach is proposed for point mutation detection based on hyperspectral interferometry. A hybridization strategy is designed to discriminate a single-base substitution with sequence-specific DNA ligase. Double-strand structures will take place only if added oligonucleotides are perfectly paired to the probe sequence. The proposed approach takes full use of the inherent conformation of double-strand DNA molecules on the substrate and a spectrum analysis method is established to point out the sub-nanoscale thickness variation, which benefits to high sensitive mutation detection. The limit of detection reach 4pg/mm2 according to the experimental result. A lung cancer gene point mutation was demonstrated, proving the high selectivity and multiplex analysis capability of the proposed biosensor.

Updating Landsat-derived land-cover maps using change detection and masking techniques

NASA Technical Reports Server (NTRS)

Likens, W.; Maw, K.

1982-01-01

The California Integrated Remote Sensing System's San Bernardino County Project was devised to study the utilization of a data base at a number of jurisdictional levels. The present paper discusses the implementation of change-detection and masking techniques in the updating of Landsat-derived land-cover maps. A baseline landcover classification was first created from a 1976 image, then the adjusted 1976 image was compared with a 1979 scene by the techniques of (1) multidate image classification, (2) difference image-distribution tails thresholding, (3) difference image classification, and (4) multi-dimensional chi-square analysis of a difference image. The union of the results of methods 1, 3 and 4 was used to create a mask of possible change areas between 1976 and 1979, which served to limit analysis of the update image and reduce comparison errors in unchanged areas. The techniques of spatial smoothing of change-detection products, and of combining results of difference change-detection algorithms are also shown to improve Landsat change-detection accuracies.

Antibiotic Resistance Gene Detection in the Microbiome Context.

PubMed

Do, Thi Thuy; Tamames, Javier; Stedtfeld, Robert D; Guo, Xueping; Murphy, Sinead; Tiedje, James M; Walsh, Fiona

2018-06-01

Within the past decade, microbiologists have moved from detecting single antibiotic resistance genes (ARGs) to detecting all known resistance genes within a sample due to advances in next generation sequencing. This has provided a wealth of data on the variation and relative abundances of ARGs present in a total bacterial population. However, to use these data in terms of therapy or risk to patients, they must be analyzed in the context of the background microbiome. Using a quantitative PCR ARG chip and 16S rRNA amplicon sequencing, we have sought to identify the ARGs and bacteria present in a fecal sample of a healthy adult using genomic tools. Of the 42 ARGs detected, 12 fitted into the ResCon1 category of ARGs: cfxA, cphA, bacA, sul3, aadE, bla TEM , aphA1, aphA3, aph(2')-Id, aacA/aphd, catA1, and vanC. Therefore, we describe these 12 genes as the core resistome of this person's fecal microbiome and the remaining 30 ARGs as descriptors of the microbial population within the fecal microbiome. The dominant phyla and genera agree with those previously detected in the greatest abundances in fecal samples of healthy humans. The majority of the ARGs detected were associated with the presence of specific bacterial taxa, which were confirmed using microbiome analysis. We acknowledge the limitations of the data in the context of the limited sample set. However, the principle of combining qPCR and microbiome analysis was shown to be helpful to identify the association of the ARGs with specific taxa.

In vivo flow cytometry for blood cell analysis using differential epi-detection of forward scattered light

NASA Astrophysics Data System (ADS)

Paudel, Hari P.; Jung, Yookyung; Raphael, Anthony; Alt, Clemens; Wu, Juwell; Runnels, Judith; Lin, Charles P.

2018-02-01

The present standard of blood cell analysis is an invasive procedure requiring the extraction of patient's blood, followed by ex-vivo analysis using a flow cytometer or a hemocytometer. We are developing a noninvasive optical technique that alleviates the need for blood extraction. For in-vivo blood analysis we need a high speed, high resolution and high contrast label-free imaging technique. In this proceeding report, we reported a label-free method based on differential epi-detection of forward scattered light, a method inspired by Jerome Mertz's oblique back-illumination microscopy (OBM) (Ford et al, Nat. Meth. 9(12) 2012). The differential epi-detection of forward light gives phase contrast image at diffraction-limited resolution. Unlike reflection confocal microscopy (RCM), which detects only sharp refractive index variation and suffers from speckle noise, this technique is suitable for detection of subtle variation of refractive index in biological tissue and it provides the shape and the size of cells. A custom built high speed electronic detection circuit board produces a real-time differential signal which yields image contrast based on phase gradient in the sample. We recorded blood flow in-vivo at 17.2k lines per second in line scan mode, or 30 frames per second (full frame), or 120 frame per second (quarter frame) in frame scan mode. The image contrast and speed of line scan data recording show the potential of the system for noninvasive blood cell analysis.

An event-specific method for the detection and quantification of ML01, a genetically modified Saccharomyces cerevisiae wine strain, using quantitative PCR.

PubMed

Vaudano, Enrico; Costantini, Antonella; Garcia-Moruno, Emilia

2016-10-03

The availability of genetically modified (GM) yeasts for winemaking and, in particular, transgenic strains based on the integration of genetic constructs deriving from other organisms into the genome of Saccharomyces cerevisiae, has been a reality for several years. Despite this, their use is only authorized in a few countries and limited to two strains: ML01, able to convert malic acid into lactic acid during alcoholic fermentation, and ECMo01 suitable for reducing the risk of carbamate production. In this work we propose a quali-quantitative culture-independent method for the detection of GM yeast ML01 in commercial preparations of ADY (Active Dry Yeast) consisting of efficient extraction of DNA and qPCR (quantitative PCR) analysis based on event-specific assay targeting MLC (malolactic cassette), and a taxon-specific S. cerevisiae assay detecting the MRP2 gene. The ADY DNA extraction methodology has been shown to provide good purity DNA suitable for subsequent qPCR. The MLC and MRP2 qPCR assay showed characteristics of specificity, dynamic range, limit of quantification (LOQ) limit of detection (LOD), precision and trueness, which were fully compliant with international reference guidelines. The method has been shown to reliably detect 0.005% (mass/mass) of GM ML01 S. cerevisiae in commercial preparations of ADY. Copyright © 2016 Elsevier B.V. All rights reserved.

Enhanced Detection of Chromosomal Abnormalities in Chronic Lymphocytic Leukemia by Conventional Cytogenetics Using CpG Oligonucleotide in Combination with Pokeweed Mitogen and Phorbol Myristate Acetate

PubMed Central

Muthusamy, Natarajan; Breidenbach, Heather; Andritsos, Leslie; Flynn, Joseph; Jones, Jeffrey; Ramanunni, Asha; Mo, Xiaokui; Jarjoura, David; Byrd, John C.; Heerema, Nyla A.

2011-01-01

Reproducible cytogenetic analysis in CLL has been limited by the inability to obtain reliable metaphase cells for analysis. CpG oligonucleotide and cytokine stimulation have been shown to improve metaphase analysis of CLL cytogenetic abnormalities, but is limited by variability in the cytokine receptor levels, stability and biological activity of the cytokine in culture conditions and high costs associated with these reagents. We report here use of a novel, stable CpG, GNKG168 along with pokeweed mitogen (PWM) and phorbol 12-myristate 13-acetate (PMA) for conventional cytogenetic assessment in CLL. We demonstrate that the combined use of GNKG168+PWM/PMA increased the sensitivity of detection of chromosomal abnormalities compared to PWM/PMA (n=207, odds ratio=2.2, p=0.0002) and GNKG168 (n=219, odds ratio=1.5, p=0.0452). Further, a significant increase in sensitivity to detect complexity ≥3 with GNKG168+PWM/PMA compared to GNKG168 alone (odds ratio 8.0, p=0.0022) or PWM/PMA alone (odds ratio 9.6, p=0.0007) was observed. The trend toward detection of higher complexity was significantly greater with GNKG168+PWM/PMA compared to GNKG168 alone (p=0.0412). The increased sensitivity was mainly attributed to the addition of PWM/PMA with GNKG168 because GNKG168 alone showed no difference in sensitivity for detection of complex abnormalities (p=0.17). Comparison of fluorescence in situ hybridization (FISH) results with karyotypic results showed a high degree of consistency, although some complex karyotypes were present in cases with no adverse FISH abnormality. These studies provide evidence for potential use of GNKG168 in combination with PWM and PMA in karyotypic analysis of CLL patient samples to better identify chromosomal abnormalities for risk stratification. PMID:21494579

Visual saliency detection based on in-depth analysis of sparse representation

NASA Astrophysics Data System (ADS)

Wang, Xin; Shen, Siqiu; Ning, Chen

2018-03-01

Visual saliency detection has been receiving great attention in recent years since it can facilitate a wide range of applications in computer vision. A variety of saliency models have been proposed based on different assumptions within which saliency detection via sparse representation is one of the newly arisen approaches. However, most existing sparse representation-based saliency detection methods utilize partial characteristics of sparse representation, lacking of in-depth analysis. Thus, they may have limited detection performance. Motivated by this, this paper proposes an algorithm for detecting visual saliency based on in-depth analysis of sparse representation. A number of discriminative dictionaries are first learned with randomly sampled image patches by means of inner product-based dictionary atom classification. Then, the input image is partitioned into many image patches, and these patches are classified into salient and nonsalient ones based on the in-depth analysis of sparse coding coefficients. Afterward, sparse reconstruction errors are calculated for the salient and nonsalient patch sets. By investigating the sparse reconstruction errors, the most salient atoms, which tend to be from the most salient region, are screened out and taken away from the discriminative dictionaries. Finally, an effective method is exploited for saliency map generation with the reduced dictionaries. Comprehensive evaluations on publicly available datasets and comparisons with some state-of-the-art approaches demonstrate the effectiveness of the proposed algorithm.

Information theoretic analysis of canny edge detection in visual communication

NASA Astrophysics Data System (ADS)

Jiang, Bo; Rahman, Zia-ur

2011-06-01

In general edge detection evaluation, the edge detectors are examined, analyzed, and compared either visually or with a metric for specific an application. This analysis is usually independent of the characteristics of the image-gathering, transmission and display processes that do impact the quality of the acquired image and thus, the resulting edge image. We propose a new information theoretic analysis of edge detection that unites the different components of the visual communication channel and assesses edge detection algorithms in an integrated manner based on Shannon's information theory. The edge detection algorithm here is considered to achieve high performance only if the information rate from the scene to the edge approaches the maximum possible. Thus, by setting initial conditions of the visual communication system as constant, different edge detection algorithms could be evaluated. This analysis is normally limited to linear shift-invariant filters so in order to examine the Canny edge operator in our proposed system, we need to estimate its "power spectral density" (PSD). Since the Canny operator is non-linear and shift variant, we perform the estimation for a set of different system environment conditions using simulations. In our paper we will first introduce the PSD of the Canny operator for a range of system parameters. Then, using the estimated PSD, we will assess the Canny operator using information theoretic analysis. The information-theoretic metric is also used to compare the performance of the Canny operator with other edge-detection operators. This also provides a simple tool for selecting appropriate edgedetection algorithms based on system parameters, and for adjusting their parameters to maximize information throughput.

Sensitive indoor air monitoring of formaldehyde and other carbonyl compounds using the 2,4-dinitrophenylhydrazine method.

PubMed

Sandner, F; Dott, W; Hollender, J

2001-03-01

The toxic potential of formaldehyde and other aliphatic/aromatic carbonyl compounds requires the determination of even low amounts of these compounds in indoor air. The existing DFG-method for workplace monitoring using adsorption at 2,4-dinitrophenylhydrazine (DNPH)-coated sorbents followed by HPLC-UV/DAD analysis of the extract was modified in order to decrease detection limits. The improvement included an increase in volume and rate of the air sampling, testing applicability of different adsorption materials and a decrease of the extraction volume of the hydrazones. 13 DNPH-derivatives could be separated well on a RP18-column followed by UV/DAD-detection at 365 nm. Recovery rates of 70-100% were determined (apart from acetone with 19%) using dynamically produced artifical carbonyl atmospheres. Detection limits of 0.05-0.4 microgram/m3 were reached by this method which are sufficient for indoor air monitoring.

Essential Limitations of the Standard THz TDS Method for Substance Detection and Identification and a Way of Overcoming Them

PubMed Central

Trofimov, Vyacheslav A.; Varentsova, Svetlana A.

2016-01-01

Low efficiency of the standard THz TDS method of the detection and identification of substances based on a comparison of the spectrum for the signal under investigation with a standard signal spectrum is demonstrated using the physical experiments conducted under real conditions with a thick paper bag as well as with Si-based semiconductors under laboratory conditions. In fact, standard THz spectroscopy leads to false detection of hazardous substances in neutral samples, which do not contain them. This disadvantage of the THz TDS method can be overcome by using time-dependent THz pulse spectrum analysis. For a quality assessment of the standard substance spectral features presence in the signal under analysis, one may use time-dependent integral correlation criteria. PMID:27070617

Essential Limitations of the Standard THz TDS Method for Substance Detection and Identification and a Way of Overcoming Them.

PubMed

Trofimov, Vyacheslav A; Varentsova, Svetlana A

2016-04-08

Low efficiency of the standard THz TDS method of the detection and identification of substances based on a comparison of the spectrum for the signal under investigation with a standard signal spectrum is demonstrated using the physical experiments conducted under real conditions with a thick paper bag as well as with Si-based semiconductors under laboratory conditions. In fact, standard THz spectroscopy leads to false detection of hazardous substances in neutral samples, which do not contain them. This disadvantage of the THz TDS method can be overcome by using time-dependent THz pulse spectrum analysis. For a quality assessment of the standard substance spectral features presence in the signal under analysis, one may use time-dependent integral correlation criteria.

Improved PCR-Based Detection of Soil Transmitted Helminth Infections Using a Next-Generation Sequencing Approach to Assay Design.

PubMed

Pilotte, Nils; Papaiakovou, Marina; Grant, Jessica R; Bierwert, Lou Ann; Llewellyn, Stacey; McCarthy, James S; Williams, Steven A

2016-03-01

The soil transmitted helminths are a group of parasitic worms responsible for extensive morbidity in many of the world's most economically depressed locations. With growing emphasis on disease mapping and eradication, the availability of accurate and cost-effective diagnostic measures is of paramount importance to global control and elimination efforts. While real-time PCR-based molecular detection assays have shown great promise, to date, these assays have utilized sub-optimal targets. By performing next-generation sequencing-based repeat analyses, we have identified high copy-number, non-coding DNA sequences from a series of soil transmitted pathogens. We have used these repetitive DNA elements as targets in the development of novel, multi-parallel, PCR-based diagnostic assays. Utilizing next-generation sequencing and the Galaxy-based RepeatExplorer web server, we performed repeat DNA analysis on five species of soil transmitted helminths (Necator americanus, Ancylostoma duodenale, Trichuris trichiura, Ascaris lumbricoides, and Strongyloides stercoralis). Employing high copy-number, non-coding repeat DNA sequences as targets, novel real-time PCR assays were designed, and assays were tested against established molecular detection methods. Each assay provided consistent detection of genomic DNA at quantities of 2 fg or less, demonstrated species-specificity, and showed an improved limit of detection over the existing, proven PCR-based assay. The utilization of next-generation sequencing-based repeat DNA analysis methodologies for the identification of molecular diagnostic targets has the ability to improve assay species-specificity and limits of detection. By exploiting such high copy-number repeat sequences, the assays described here will facilitate soil transmitted helminth diagnostic efforts. We recommend similar analyses when designing PCR-based diagnostic tests for the detection of other eukaryotic pathogens.

Comparison of LIDAR system performance for alternative single-mode receiver architectures: modeling and experimental validation

NASA Astrophysics Data System (ADS)

Toliver, Paul; Ozdur, Ibrahim; Agarwal, Anjali; Woodward, T. K.

2013-05-01

In this paper, we describe a detailed performance comparison of alternative single-pixel, single-mode LIDAR architectures including (i) linear-mode APD-based direct-detection, (ii) optically-preamplified PIN receiver, (iii) PINbased coherent-detection, and (iv) Geiger-mode single-photon-APD counting. Such a comparison is useful when considering next-generation LIDAR on a chip, which would allow one to leverage extensive waveguide-based structures and processing elements developed for telecom and apply them to small form-factor sensing applications. Models of four LIDAR transmit and receive systems are described in detail, which include not only the dominant sources of receiver noise commonly assumed in each of the four detection limits, but also additional noise terms present in realistic implementations. These receiver models are validated through the analysis of detection statistics collected from an experimental LIDAR testbed. The receiver is reconfigurable into four modes of operation, while transmit waveforms and channel characteristics are held constant. The use of a diffuse hard target highlights the importance of including speckle noise terms in the overall system analysis. All measurements are done at 1550 nm, which offers multiple system advantages including less stringent eye safety requirements and compatibility with available telecom components, optical amplification, and photonic integration. Ultimately, the experimentally-validated detection statistics can be used as part of an end-to-end system model for projecting rate, range, and resolution performance limits and tradeoffs of alternative integrated LIDAR architectures.

Material Limitations on the Detection Limit in Refractometry

PubMed Central

Skafte-Pedersen, Peder; Nunes, Pedro S.; Xiao, Sanshui; Mortensen, Niels Asger

2009-01-01

We discuss the detection limit for refractometric sensors relying on high-Q optical cavities and show that the ultimate classical detection limit is given by min {Δn} ≳ η, with n + iη being the complex refractive index of the material under refractometric investigation. Taking finite Q factors and filling fractions into account, the detection limit declines. As an example we discuss the fundamental limits of silicon-based high-Q resonators, such as photonic crystal resonators, for sensing in a bio-liquid environment, such as a water buffer. In the transparency window (λ ≳ 1100 nm) of silicon the detection limit becomes almost independent on the filling fraction, while in the visible, the detection limit depends strongly on the filling fraction because the silicon absorbs strongly. PMID:22291513

Rapid analysis of perchlorate in drinking water at parts per billion levels using microchip electrophoresis.

PubMed

Gertsch, Jana C; Noblitt, Scott D; Cropek, Donald M; Henry, Charles S

2010-05-01

A microchip capillary electrophoresis (MCE) system has been developed for the determination of perchlorate in drinking water. The United States Environmental Protection Agency (USEPA) recently proposed a health advisory limit for perchlorate in drinking water of 15 parts per billion (ppb), a level requiring large, sophisticated instrumentation, such as ion chromatography coupled with mass spectrometry (IC-MS), for detection. An inexpensive, portable system is desired for routine online monitoring applications of perchlorate in drinking water. Here, we present an MCE method using contact conductivity detection for perchlorate determination. The method has several advantages, including reduced analysis times relative to IC, inherent portability, high selectivity, and minimal sample pretreatment. Resolution of perchlorate from more abundant ions was achieved using zwitterionic, sulfobetaine surfactants, N-hexadecyl-N,N-dimethyl-3-ammonio-1-propane sulfonate (HDAPS) and N-tetradecyl-N,N-dimethyl-3-ammonio-1-propane sulfonate (TDAPS). The system performance and the optimization of the separation chemistry, including the use of these surfactants to resolve perchlorate from other anions, are discussed in this work. The system is capable of detection limits of 3.4 +/- 1.8 ppb (n = 6) in standards and 5.6 +/- 1.7 ppb (n = 6) in drinking water.

The application of LANDSAT-1 imagery for monitoring strip mines in the new river watershed in northeast Tennessee, part 2

NASA Technical Reports Server (NTRS)

Shahrokhi, F. (Principal Investigator); Sharber, L. A.

1977-01-01

The author has identified the following significant results. LANDSAT imagery and supplementary aircraft photography of the New River drainage basin were subjected to a multilevel analysis using conventional photointerpretation methods, densitometric techniques, multispectral analysis, and statistical tests to determine the accuracy of LANDSAT-1 imagery for measuring strip mines of common size. The LANDSAT areas were compared with low altitude measurements. The average accuracy over all the mined land sample areas mapped from LANDSAT-1 was 90%. The discrimination of strip mine subcategories is somewhat limited on LANDSAT imagery. A mine site, whether active or inactive, can be inferred by lack of vegetation, by shape, or image texture. Mine ponds are difficult or impossible to detect because of their small size and turbidity. Unless bordered and contrasted with vegetation, haulage roads are impossible to delineate. Preparation plants and refuge areas are not detectable. Density slicing of LANDSAT band 7 proved most useful in the detection of reclamation progress within the mined areas. For most state requirements for year-round monitoring of surface mined land, LANDSAT is of limited value. However, for periodic updating of regional surface maps, LANDSAT may provide sufficient accuracies for some users.

Separation and determination of epinephrine and dopamine in traditional Chinese medicines by micellar electrokinetic capillary chromatography with laser induced fluorescence detection.

PubMed

Dong, Yuming; Chen, Hongli; Chen, Yonglei; Hui, Yang; Chen, Xingguo; Hu, Zhide

2006-08-01

A micellar electrokinetic capillary chromatography method with laser-induced fluorescence detection was developed for the analysis of epinephrine and dopamine after derivatization with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole. The optimum derivatization conditions were: 30 mM sodium borate (pH adjusted to 8.0 with 1.0 M HCl), reaction time 30 min at 60 degrees C. Baseline separation was achieved within 14 min with a running buffer composed of 10 mM sodium borate + 25 mM sodium dodecyl sulfate (pH adjusted to 9.5 with 0.1 M NaOH) and an applied voltage of 15 kV. Good linearity relationships (correlation coefficients: 0.9991 for epinephrine and 0.9985 for dopamine) between peak areas and concentrations of the analytes were obtained. The detection limits and quantification limits for epinephrine and dopamine were 0.0038 mg/L and 0.013 mg/L, and 0.065 mg/L and 0.020 mg/L, respectively. The method was applied to the analysis of the two compounds in two Chinese medicines with recoveries in the range of 92.6-108.7%.

Trace element analysis by EPMA in geosciences: detection limit, precision and accuracy

NASA Astrophysics Data System (ADS)

Batanova, V. G.; Sobolev, A. V.; Magnin, V.

2018-01-01

Use of the electron probe microanalyser (EPMA) for trace element analysis has increased over the last decade, mainly because of improved stability of spectrometers and the electron column when operated at high probe current; development of new large-area crystal monochromators and ultra-high count rate spectrometers; full integration of energy-dispersive / wavelength-dispersive X-ray spectrometry (EDS/WDS) signals; and the development of powerful software packages. For phases that are stable under a dense electron beam, the detection limit and precision can be decreased to the ppm level by using high acceleration voltage and beam current combined with long counting time. Data on 10 elements (Na, Al, P, Ca, Ti, Cr, Mn, Co, Ni, Zn) in olivine obtained on a JEOL JXA-8230 microprobe with tungsten filament show that the detection limit decreases proportionally to the square root of counting time and probe current. For all elements equal or heavier than phosphorus (Z = 15), the detection limit decreases with increasing accelerating voltage. The analytical precision for minor and trace elements analysed in olivine at 25 kV accelerating voltage and 900 nA beam current is 4 - 18 ppm (2 standard deviations of repeated measurements of the olivine reference sample) and is similar to the detection limit of corresponding elements. To analyse trace elements accurately requires careful estimation of background, and consideration of sample damage under the beam and secondary fluorescence from phase boundaries. The development and use of matrix reference samples with well-characterised trace elements of interest is important for monitoring and improving of the accuracy. An evaluation of the accuracy of trace element analyses in olivine has been made by comparing EPMA data for new reference samples with data obtained by different in-situ and bulk analytical methods in six different laboratories worldwide. For all elements, the measured concentrations in the olivine reference sample were found to be identical (within internal precision) to reference values, suggesting that achieved precision and accuracy are similar. The spatial resolution of EPMA in a silicate matrix, even at very extreme conditions (accelerating voltage 25 kV), does not exceed 7 - 8 μm and thus is still better than laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) or secondary ion mass spectrometry (SIMS) of similar precision. These make the electron microprobe an indispensable method with applications in experimental petrology, geochemistry and cosmochemistry.

Reflectance measurements for the detection and mapping of soil limitations

NASA Technical Reports Server (NTRS)

Benson, L. A.; Frazee, C. J.

1973-01-01

During 1971 and 1972 research was conducted on two fallow fields in the proposed Oahe Irrigation Project to investigate the relationship between the tonal variations observed on aerial photographs and the principal soil limitations of the area. A grid sampling procedure was used to collected detailed field data during the 1972 growing season. The field data was compared to imagery collected on May 14, 1971 at 3050 meters altitude. The imagery and field data were initially evaluated by a visual analysis. Correlation and regression analysis revealed a highly significant correlation and regression analysis revealed a highly significant correlation between the digitized color infrared film data and soil properties such as organic matter content, color, depth to carbonates, bulk density and reflectivity. Computer classification of the multiemulsion film data resulted in maps delineating the areas containing claypan and erosion limitations. Reflectance data from the red spectral band provided the best results.

Detecting transitions in protein dynamics using a recurrence quantification analysis based bootstrap method.

PubMed

Karain, Wael I

2017-11-28

Proteins undergo conformational transitions over different time scales. These transitions are closely intertwined with the protein's function. Numerous standard techniques such as principal component analysis are used to detect these transitions in molecular dynamics simulations. In this work, we add a new method that has the ability to detect transitions in dynamics based on the recurrences in the dynamical system. It combines bootstrapping and recurrence quantification analysis. We start from the assumption that a protein has a "baseline" recurrence structure over a given period of time. Any statistically significant deviation from this recurrence structure, as inferred from complexity measures provided by recurrence quantification analysis, is considered a transition in the dynamics of the protein. We apply this technique to a 132 ns long molecular dynamics simulation of the β-Lactamase Inhibitory Protein BLIP. We are able to detect conformational transitions in the nanosecond range in the recurrence dynamics of the BLIP protein during the simulation. The results compare favorably to those extracted using the principal component analysis technique. The recurrence quantification analysis based bootstrap technique is able to detect transitions between different dynamics states for a protein over different time scales. It is not limited to linear dynamics regimes, and can be generalized to any time scale. It also has the potential to be used to cluster frames in molecular dynamics trajectories according to the nature of their recurrence dynamics. One shortcoming for this method is the need to have large enough time windows to insure good statistical quality for the recurrence complexity measures needed to detect the transitions.

Sea-urchin-like Fe3O4@C@Ag particles: an efficient SERS substrate for detection of organic pollutants

NASA Astrophysics Data System (ADS)

Ye, Yingjie; Chen, Jin; Ding, Qianqian; Lin, Dongyue; Dong, Ronglu; Yang, Liangbao; Liu, Jinhuai

2013-06-01

Ag-coated sea-urchin-like Fe3O4@C core-shell particles can be synthesized by a facile one-step solvothermal method, followed by deposition of high-density Ag nanoparticles onto the carbon surface through an in situ growth process, respectively. The as-synthesized Ag-coated Fe3O4@C particles can be used as a surface-enhanced Raman scattering (SERS) substrate holding reproducible properties under an external magnetic force. The magnetic function of the particles allows concentrating the composite particles into small spatial regions, which can be exploited to decrease the amount of material per analysis while improving its SERS detection limit. In contrast to the traditional SERS substrates, the present Fe3O4@C@Ag particles hold the advantages of enrichment of organic pollutants for improving SERS detection limit and recycled utilization.Ag-coated sea-urchin-like Fe3O4@C core-shell particles can be synthesized by a facile one-step solvothermal method, followed by deposition of high-density Ag nanoparticles onto the carbon surface through an in situ growth process, respectively. The as-synthesized Ag-coated Fe3O4@C particles can be used as a surface-enhanced Raman scattering (SERS) substrate holding reproducible properties under an external magnetic force. The magnetic function of the particles allows concentrating the composite particles into small spatial regions, which can be exploited to decrease the amount of material per analysis while improving its SERS detection limit. In contrast to the traditional SERS substrates, the present Fe3O4@C@Ag particles hold the advantages of enrichment of organic pollutants for improving SERS detection limit and recycled utilization. Electronic supplementary information (ESI) available: Additional XRD patterns and SEM images of Fe3O4@C particles, SERS spectra of 4-ATP and 4-MPY using Fe3O4@C@Ag particles as the active substrates, magnetic behaviour of Fe3O4@C and Fe3O4@C@Ag particles. See DOI: 10.1039/c3nr01273e

Development and application of a multi-targeting reference plasmid as calibrator for analysis of five genetically modified soybean events.

PubMed

Pi, Liqun; Li, Xiang; Cao, Yiwei; Wang, Canhua; Pan, Liangwen; Yang, Litao

2015-04-01

Reference materials are important in accurate analysis of genetically modified organism (GMO) contents in food/feeds, and development of novel reference plasmid is a new trend in the research of GMO reference materials. Herein, we constructed a novel multi-targeting plasmid, pSOY, which contained seven event-specific sequences of five GM soybeans (MON89788-5', A2704-12-3', A5547-127-3', DP356043-5', DP305423-3', A2704-12-5', and A5547-127-5') and sequence of soybean endogenous reference gene Lectin. We evaluated the specificity, limit of detection and quantification, and applicability of pSOY in both qualitative and quantitative PCR analyses. The limit of detection (LOD) was as low as 20 copies in qualitative PCR, and the limit of quantification (LOQ) in quantitative PCR was 10 copies. In quantitative real-time PCR analysis, the PCR efficiencies of all event-specific and Lectin assays were higher than 90%, and the squared regression coefficients (R(2)) were more than 0.999. The quantification bias varied from 0.21% to 19.29%, and the relative standard deviations were from 1.08% to 9.84% in simulated samples analysis. All the results demonstrated that the developed multi-targeting plasmid, pSOY, was a credible substitute of matrix reference materials, and could be used as a reliable reference calibrator in the identification and quantification of multiple GM soybean events.

Limited genomic heterogeneity of circulating melanoma cells in advanced stage patients

NASA Astrophysics Data System (ADS)

Ruiz, Carmen; Li, Julia; Luttgen, Madelyn S.; Kolatkar, Anand; Kendall, Jude T.; Flores, Edna; Topp, Zheng; Samlowski, Wolfram E.; McClay, Edward; Bethel, Kelly; Ferrone, Soldano; Hicks, James; Kuhn, Peter

2015-02-01

Purpose. Circulating melanoma cells (CMCs) constitute a potentially important representation of time-resolved tumor biology in patients. To date, genomic characterization of CMCs has been limited due to the lack of a robust methodology capable of identifying them in a format suitable for downstream characterization. Here, we have developed a methodology to detect intact CMCs that enables phenotypic, morphometric and genomic analysis at the single cell level. Experimental design. Blood samples from 40 metastatic melanoma patients and 10 normal blood donors were prospectively collected. A panel of 7 chondroitin sulfate proteoglycan 4 (CSPG4)-specific monoclonal antibodies (mAbs) was used to immunocytochemically label CMCs. Detection was performed by automated digital fluorescence microscopy and multi-parametric computational analysis. Individual CMCs were captured by micromanipulation for whole genome amplification and copy number variation (CNV) analysis. Results. Based on CSPG4 expression and nuclear size, 1-250 CMCs were detected in 22 (55%) of 40 metastatic melanoma patients (0.5-371.5 CMCs ml-1). Morphometric analysis revealed that CMCs have a broad spectrum of morphologies and sizes but exhibit a relatively homogeneous nuclear size that was on average 1.5-fold larger than that of surrounding PBMCs. CNV analysis of single CMCs identified deletions of CDKN2A and PTEN, and amplification(s) of TERT, BRAF, KRAS and MDM2. Furthermore, novel chromosomal amplifications in chr12, 17 and 19 were also found. Conclusions. Our findings show that CSPG4 expressing CMCs can be found in the majority of advanced melanoma patients. High content analysis of this cell population may contribute to the design of effective personalized therapies in patients with melanoma.

Fluorogenic Ag+–Tetrazolate Aggregation Enables Efficient Fluorescent Biological Silver Staining

PubMed Central

Xie, Sheng; Wong, Alex Y. H.; Kwok, Ryan T. K.; Li, Ying; Su, Huifang; Lam, Jacky W. Y.

2018-01-01

Abstract Silver staining, which exploits the special bioaffinity and the chromogenic reduction of silver ions, is an indispensable visualization method in biology. It is a most popular method for in‐gel protein detection. However, it is limited by run‐to‐run variability, background staining, inability for protein quantification, and limited compatibility with mass spectroscopic (MS) analysis; limitations that are largely attributed to the tricky chromogenic visualization. Herein, we reported a novel water‐soluble fluorogenic Ag+ probe, the sensing mechanism of which is based on an aggregation‐induced emission (AIE) process driven by tetrazolate‐Ag+ interactions. The fluorogenic sensing can substitute the chromogenic reaction, leading to a new fluorescence silver staining method. This new staining method offers sensitive detection of total proteins in polyacrylamide gels with a broad linear dynamic range and robust operations that rival the silver nitrate stain and the best fluorescent stains. PMID:29575702

An analysis of I/O efficient order-statistic-based techniques for noise power estimation in the HRMS sky survey's operational system

NASA Technical Reports Server (NTRS)

Zimmerman, G. A.; Olsen, E. T.

1992-01-01

Noise power estimation in the High-Resolution Microwave Survey (HRMS) sky survey element is considered as an example of a constant false alarm rate (CFAR) signal detection problem. Order-statistic-based noise power estimators for CFAR detection are considered in terms of required estimator accuracy and estimator dynamic range. By limiting the dynamic range of the value to be estimated, the performance of an order-statistic estimator can be achieved by simpler techniques requiring only a single pass of the data. Simple threshold-and-count techniques are examined, and it is shown how several parallel threshold-and-count estimation devices can be used to expand the dynamic range to meet HRMS system requirements with minimal hardware complexity. An input/output (I/O) efficient limited-precision order-statistic estimator with wide but limited dynamic range is also examined.

Solid phase microextraction applied to the analysis of organophosphorus insecticides in fruits.

PubMed

Fytianos, K; Raikos, N; Theodoridis, G; Velinova, Z; Tsoukali, H

2006-12-01

Trace amounts of organophosphorus pesticides (OPs) were determined in various fruits by headspace solid phase microextraction (HS-SPME) and gas chromatography-nitrogen phosphorous detection (GC-NPD). Sampling from the headspace enhanced method selectivity, whereas at the same time improved fiber life time and method sensitivity. Diazinon, parathion, methyl parathion, malathion and fenithrothion were determined in various fruits: more than 150 samples of 21 types of fruits were studied. SPME-GC-NPD provided a useful and very efficient analytical tool: method linearity ranged from 1.2 to 700 ng/ml. Limits of detection (LODs) and quantitation (LOQs) ranged from 0.03 to 3 ng/ml and 0.12 to 10 ng/ml respectively, values well below the residue limits set by the EU. Less than 2% of the samples were found positive containing amounts higher than the EU limits. The effect of fruit peeling and washing was also investigated.

[Radioactive cesium analysis in radiation-tainted beef by gamma-ray spectrometry with germanium semiconductor detector].

PubMed

Minatani, Tomiaki; Nagai, Hiroyuki; Nakamura, Masashi; Otsuka, Kimihito; Sakai, Yoshimichi

2012-01-01

The detection limit and precision of radioactive cesium measurement in beef by gamma-ray spectrometry with a germanium semiconductor detector were evaluated. Measurement for 2,000 seconds using a U-8 container (100 mL) provided a detection limit of radioactive cesium (the sum of 134Cs and 137Cs) of around 20 Bq/kg. The 99% confidence interval of the measurement of provisional maximum residue limit level (491 Bq/kg) samples ranged from 447 to 535 Bq/kg. Beef is heterogeneous, containing muscle and complex fat layers. Depending on the sampled parts, the measurement value is variable. It was found that radioactive cesium content of the muscle layer was clearly different from that of fat, and slight differences were observed among parts of the sample (SD=16.9 Bq/kg), even though the same region (neck block) of beef sample was analyzed.

Detection and Quantification of 8-Hydroxy-2′-Deoxyguanosine in Alzheimer’s Transgenic Mouse Urine using Capillary Electrophoresis

PubMed Central

Zhang, Cheng; Nestorova, Gergana; Rissman, Robert A.; Feng, June

2013-01-01

8-Hydroxy-2′-deoxyguanosine (8-OHdG) is one of the major forms of oxidative deoxyribonucleic acid (DNA) damage, and is commonly analyzed as an excellent marker of DNA lesions. The purpose of this study was to develop a sensitive method to accurately and rapidly quantify the 8-OHdG by using capillary electrophoresis with laser-induced fluorescence detection (CE-LIF). The method involved the use of specific antibody to detect DNA lesions (8-OHdG) and consecutive fluorescence labeling. Next, the urine sample with 8-OHdG fluorescently labeled along with other constituents was resolved by capillary electrophoretic system and the lesion of interest was detected using fluorescence detector. The limit of detection was 0.18 fmol, which is sufficient sensitivity for detection and quantification of 8-OHdG in untreated urine samples. The relative standard deviation (RSD) was found to be 11.32 % for migration time, and 5.52 % for peak area. To demonstrate the utility of this method, the urinary concentration of 8-OHdG in an Alzheimer’s transgenic mouse model was determined. Collectively, our results indicate that this methodology offers great advantages such as high separation efficiency, good selectivity, low limit of detection (LOD), simplicity and low cost of analysis. PMID:23712533

Immunochromatographic strip assay for the rapid and sensitive detection of Salmonella Typhimurium in artificially contaminated tomato samples.

PubMed

Shukla, Shruti; Leem, Hyerim; Lee, Jong-Suk; Kim, Myunghee

2014-06-01

This study was designed to confirm the applicability of a liposome-based immunochromatographic assay for the rapid detection of Salmonella enterica subsp. enterica serovar Typhimurium (Salmonella Typhimurium) in artificially contaminated tomato samples. To determine the detection limit and pre-enrichment incubation time (10, 12, and 18 h pre-enrichment in 1% buffered peptone water), the tests were performed with different cell numbers of Salmonella Typhimurium (3 × 10(0), 3 × 10(1), 3 × 10(2), and 3 × 10(3) CFU·mL(-1)) inoculated into 25 g of crushed tomato samples. The assay was able to detect as few as 30 Salmonella Typhimurium cells per 25 g of tomato samples (1.2 cells·g(-1)) after 12 h pre-enrichment incubation. Moreover, when the developed assay was compared with traditional morphological and biochemical culture-based methods as well as colloidal gold nanoparticle-based commercial test strips, the developed assay yielded positive results for the detection of Salmonella Typhimurium within a shorter period time. These findings confirm that the developed assay may have practical application for the sensitive detection of Salmonella Typhimurium in various food samples, including raw vegetables, with a relatively low detection limit and shorter analysis time.

Label-free virus detection using silicon photonic microring resonators

PubMed Central

McClellan, Melinda S.; Domier, Leslie L; Bailey, Ryan C.

2013-01-01

Viruses represent a continual threat to humans through a number of mechanisms, which include disease, bioterrorism, and destruction of both plant and animal food resources. Many contemporary techniques used for the detection of viruses and viral infections suffer from limitations such as the need for extensive sample preparation or the lengthy window between infection and measurable immune response, for serological methods. In order to develop a method that is fast, cost-effective, and features reduced sample preparation compared to many other virus detection methods, we report the application of silicon photonic microring resonators for the direct, label-free detection of intact viruses in both purified samples as well as in a complex, real-world analytical matrix. As a model system, we demonstrate the quantitative detection of Bean pod mottle virus, a pathogen of great agricultural importance, with a limit of detection of 10 ng/mL. By simply grinding a small amount of leaf sample in buffer with a mortar and pestle, infected leaves can be identified over a healthy control with a total analysis time of less than 45 min. Given the inherent scalability and multiplexing capability of the semiconductor-based technology, we feel that silicon photonic microring resonators are well-positioned as a promising analytical tool for a number of viral detection applications. PMID:22138465

Characterization of x-ray framing cameras for the National Ignition Facility using single photon pulse height analysis.

PubMed

Holder, J P; Benedetti, L R; Bradley, D K

2016-11-01

Single hit pulse height analysis is applied to National Ignition Facility x-ray framing cameras to quantify gain and gain variation in a single micro-channel plate-based instrument. This method allows the separation of gain from detectability in these photon-detecting devices. While pulse heights measured by standard-DC calibration methods follow the expected exponential distribution at the limit of a compound-Poisson process, gain-gated pulse heights follow a more complex distribution that may be approximated as a weighted sum of a few exponentials. We can reproduce this behavior with a simple statistical-sampling model.

Simultaneous analysis of tea catechins, caffeine, gallic acid, theanine and ascorbic acid by micellar electrokinetic capillary chromatography.

PubMed

Aucamp, J P; Hara, Y; Apostolides, Z

2000-04-21

A micellar electrokinetic capillary chromatography (MEKC) method for the simultaneous analysis of five tea catechins, theanine, caffeine, gallic acid and ascorbic acid has been developed. The catechins are (-)-epicatechin, (+)-catechin, (-)-epigallocatechin, (-)-epicatechin gallate and (-)-epigallocatechin gallate. p-Nitrophenol serves as both reference and internal standard. All the components are separated within 13 min with a 57 cm uncoated fused-silica column. On-column detection was carried out at 200 nm. This method has been used to measure these compounds in fresh tea leaves and tea liquor. The limit of detection for all analytes ranged from 1 to 20 microg/ml.

Reconnaissance of chemical and physical characteristics of selected bottom sediments of the Caloosahatchee River and estuary, tributaries, and contiguous bays, Lee County, Florida, July 20-30, 1998

USGS Publications Warehouse

Fernandez, Mario; Marot, M.E.; Holmes, C.W.

1999-01-01

This report summarizes a reconnaissance study, conducted July 20-30, 1998, of chemical and physical characteristics of recently deposited bottom sediments in the Caloosahatchee River and Estuary. Recently deposited sediments were identified using an isotopic chronometer, Beryllium-7 (7Be), a short-lived radioisotope. Fifty-nine sites were sampled in an area that encompasses the Caloosahatchee River (River) about three miles upstream from the Franklin Lock (S-79), the entire tidally affected length of the river (estuary), and the contiguous water bodies of Matlacha Pass, San Carlos Bay, Estero Bay, Tarpon Bay, and Pine Island Sound in Lee County, Florida. Bottom sediments were sampled for 7Be at 59 sites. From the results of the 7Be analysis, 30 sites were selected for physical and chemical analysis. Sediments were analyzed for particle size, total organic carbon (TOC), trace elements, and toxic organic compounds, using semiquantitative methods for trace elements and organic compounds. The semiquantitative scans of trace elements indicated that cadmium, copper, lead, and zinc concentrations, when normalized to aluminum, were above the natural background range at 24 of 30 sites. Particle size and TOC were used to characterize sediment deposition patterns and organic content. Pesticides, polychlorinated biphenyls (PCBs), and carcinogenic polycyclic aromatic hydrocarbons (CaPAHs) were determined at 30 sites using immunoassay analysis. The semiquantitative immunoassay analyses of toxic organic compounds indicated that all of the samples contained DDT, cyclodienes as chlordane (pesticides), and CaPAHs. PCBs were not detected. Based on analyses of the 30 sites, sediments at 10 of these sites were analyzed for selected trace elements and toxic organic compounds, including pesticides, PCBs, and PAHs, using quantitative laboratory procedures. No arsenic or cadmium was detected. Zinc was detected at two sites with concentrations greater than the lower limit of the range of sediment contaminant concentrations that are usually or always associated with adverse effects (Florida Department of Environmental Protection's Sediment Quality Assessment Guidelines). Organochlorine pesticides were detected at four sites at concentrations below the reporting limits; there were no organophosphorus pesticides or PCBs detected. PAHs were detected at eight sites; however, only four sites had concentrations above the reporting limit.

Analysis of acrylamide in food products by in-line preconcentration capillary zone electrophoresis.

PubMed

Bermudo, Elisabet; Núñez, Oscar; Puignou, Luis; Galceran, Maria Teresa

2006-09-29

Two in-line preconcentration capillary zone electrophoresis (CZE) methods (field amplified sample injection (FASI) and stacking with sample matrix removal (LVSS)) have been evaluated for the analysis of acrylamide (AA) in foodstuffs. To allow the determination of AA by CZE, it was derivatized using 2-mercaptobenzoic acid. For FASI, the optimum conditions were water at pH > or = 10 adjusted with NH3 as sample solvent, 35 s hydrodynamic injection (0.5 psi) of a water plug, 35 s of electrokinetic injection (-10 kV) of the sample, and 6s hydrodynamic injection (0.5 psi) of another water plug to prevent AA removal by EOF. In stacking with sample matrix removal, the reversal time was found to be around 3.3 min. A 40 mM phosphate buffer (pH 8.5) was used as carrier electrolyte for CZE separation in both cases. For both FASI and LVSS methods, linear calibration curves over the range studied (10-1000 microg L(-1) and 25-1000 microg L(-1), respectively), limit of detection (LOD) on standards (1 microg L(-1) for FASI and 7 microg L(-1) for LVSS), limit of detection on samples (3 ng g(-1) for FASI and 20 ng g(-1) for LVSS) and both run-to-run (up to 14% for concentration and 0.8% for time values) and day-to-day precisions (up to 16% and 5% for concentration and time values, respectively) were established. Due to the lower detection limits obtained with the FASI-CZE this method was applied to the analysis of AA in different foodstuffs such as biscuits, cereals, crisp bread, snacks and coffee, and the results were compared with those obtained by LC-MS/MS.

Sources of Safety Data and Statistical Strategies for Design and Analysis: Postmarket Surveillance.

PubMed

Izem, Rima; Sanchez-Kam, Matilde; Ma, Haijun; Zink, Richard; Zhao, Yueqin

2018-03-01

Safety data are continuously evaluated throughout the life cycle of a medical product to accurately assess and characterize the risks associated with the product. The knowledge about a medical product's safety profile continually evolves as safety data accumulate. This paper discusses data sources and analysis considerations for safety signal detection after a medical product is approved for marketing. This manuscript is the second in a series of papers from the American Statistical Association Biopharmaceutical Section Safety Working Group. We share our recommendations for the statistical and graphical methodologies necessary to appropriately analyze, report, and interpret safety outcomes, and we discuss the advantages and disadvantages of safety data obtained from passive postmarketing surveillance systems compared to other sources. Signal detection has traditionally relied on spontaneous reporting databases that have been available worldwide for decades. However, current regulatory guidelines and ease of reporting have increased the size of these databases exponentially over the last few years. With such large databases, data-mining tools using disproportionality analysis and helpful graphics are often used to detect potential signals. Although the data sources have many limitations, analyses of these data have been successful at identifying safety signals postmarketing. Experience analyzing these dynamic data is useful in understanding the potential and limitations of analyses with new data sources such as social media, claims, or electronic medical records data.

The quantitation of 2-oxo-3-hydroxy lysergic acid diethylamide (O-H-LSD) in human urine specimens, a metabolite of LSD: comparative analysis using liquid chromatography-selected ion monitoring mass spectrometry and liquid chromatography-ion trap mass spectrometry.

PubMed

Poch, G K; Klette, K L; Anderson, C

2000-04-01

This paper compares the potential forensic application of two sensitive and rapid procedures (liquid chromatography-mass spectrometry and liquid chromatography-ion trap mass spectrometry) for the detection and quantitation of 2-oxo-3-hydroxy lysergic acid diethylamide (O-H-LSD) a major LSD metabolite. O-H-LSD calibration curves for both procedures were linear over the concentration range 0-8,000 pg/mL with correlation coefficients (r2) greater than 0.99. The observed limit of detection (LOD) and limit of quantitation (LOQ) for O-H-LSD in both procedures was 400 pg/mL. Sixty-eight human urine specimens that had previously been found to contain LSD by gas chromatography-mass spectrometry were reanalyzed by both procedures for LSD and O-H-LSD. These specimens contained a mean concentration of O-H-LSD approximately 16 times higher than the LSD concentration. Because both LC methods produce similar results, either procedure can be readily adapted to O-H-LSD analysis for use in high-volume drug-testing laboratories. In addition, the possibility of significantly increasing the LSD detection time window by targeting this major LSD metabolite for analysis may influence other drug-free workplace programs to test for LSD.

Headspace needle-trap analysis of priority volatile organic compounds from aqueous samples: application to the analysis of natural and waste waters.

PubMed

Alonso, Monica; Cerdan, Laura; Godayol, Anna; Anticó, Enriqueta; Sanchez, Juan M

2011-11-11

Combining headspace (HS) sampling with a needle-trap device (NTD) to determine priority volatile organic compounds (VOCs) in water samples results in improved sensitivity and efficiency when compared to conventional static HS sampling. A 22 gauge stainless steel, 51-mm needle packed with Tenax TA and Carboxen 1000 particles is used as the NTD. Three different HS-NTD sampling methodologies are evaluated and all give limits of detection for the target VOCs in the ng L⁻¹ range. Active (purge-and-trap) HS-NTD sampling is found to give the best sensitivity but requires exhaustive control of the sampling conditions. The use of the NTD to collect the headspace gas sample results in a combined adsorption/desorption mechanism. The testing of different temperatures for the HS thermostating reveals a greater desorption effect when the sample is allowed to diffuse, whether passively or actively, through the sorbent particles. The limits of detection obtained in the simplest sampling methodology, static HS-NTD (5 mL aqueous sample in 20 mL HS vials, thermostating at 50 °C for 30 min with agitation), are sufficiently low as to permit its application to the analysis of 18 priority VOCs in natural and waste waters. In all cases compounds were detected below regulated levels. Copyright © 2011 Elsevier B.V. All rights reserved.

Fast vaporization solid phase microextraction and ion mobility spectrometry: A new approach for determination of creatinine in biological fluids.

PubMed

Jafari, Mostafa; Ebrahimzadeh, Homeira; Banitaba, Mohamma Hossein

2015-11-01

In this work a rapid and simple method for creatinine determination in urine and plasma samples based on aqueous derivatization of creatinine and complete vaporization of sample (as low as 10 µL), followed by ion mobility spectrometry analysis has been proposed. The effect of four important parameters (extraction temperature, total volume of solution, desorption temperature and extraction time) on ion mobility signal has been studied. Under the optimized conditions, the quantitative response of ion mobility spectrometry for creatinine was linear in the range of 0-500 mg L(-1) with a detection limit of 0.6 mg L(-1) in urine and 0-250 mg L(-1) with a detection limit of 2.6 mg L(-1) in plasma sample. The limit of quantitation of creatinine was 2.1 mg L(-1) and 8.7 mg L(-1) in urine and plasma samples, respectively. The relative standard deviation of the method was found to be 13%. The method was successfully applied to the analysis of creatinine in biological samples, showing recoveries from 92% to 104% in urine and 101-110% in plasma samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Performance characteristics of a visual-search human-model observer with sparse PET image data

NASA Astrophysics Data System (ADS)

Gifford, Howard C.

2012-02-01

As predictors of human performance in detection-localization tasks, statistical model observers can have problems with tasks that are primarily limited by target contrast or structural noise. Model observers with a visual-search (VS) framework may provide a more reliable alternative. This framework provides for an initial holistic search that identifies suspicious locations for analysis by a statistical observer. A basic VS observer for emission tomography focuses on hot "blobs" in an image and uses a channelized nonprewhitening (CNPW) observer for analysis. In [1], we investigated this model for a contrast-limited task with SPECT images; herein, a statisticalnoise limited task involving PET images is considered. An LROC study used 2D image slices with liver, lung and soft-tissue tumors. Human and model observers read the images in coronal, sagittal and transverse display formats. The study thus measured the detectability of tumors in a given organ as a function of display format. The model observers were applied under several task variants that tested their response to structural noise both at the organ boundaries alone and over the organs as a whole. As measured by correlation with the human data, the VS observer outperformed the CNPW scanning observer.

Capillary moving-boundary isotachophoresis with electrospray ionization mass-spectrometric detection and hydrogen ion used as essential terminator: Methodology for sensitive analysis of hydroxyderivatives of s-triazine herbicides in waters.

PubMed

Malá, Zdena; Gebauer, Petr

2017-10-06

Capillary isotachophoresis (ITP) is an electrophoretic technique offering high sensitivity due to permanent stacking of the migrating analytes. Its combination with electrospray-ionization mass-spectrometric (ESI-MS) detection is limited by the narrow spectrum of ESI-compatible components but can be compensated by experienced system architecture. This work describes a methodology for sensitive analysis of hydroxyderivatives of s-triazine herbicides, based on implementation of the concepts of moving-boundary isotachophoresis and of H + as essential terminating component into cationic ITP with ESI-MS detection. Theoretical description of such kind of system is given and equations for zone-related boundary mobilities are derived, resulting in a much more general definition of the effective mobility of the terminating H + zone than used so far. Explicit equations allowing direct calculation for selected simple systems are derived. The presented theory allows prediction of stacking properties of particular systems and easy selection of suitable electrolyte setups. A simple ESI-compatible system composed of acetic acid and ammonium with H + and ammonium as a mixed terminator was selected for the analysis of 2-hydroxyatrazine and 2-hydroxyterbutylazine, degradation products of s-triazine herbicides. The proposed method was tested with direct injection without any sample pretreatment and provided excellent linearity and high sensitivity with limits of detection below 100ng/L (0.5nM). Example analyses of unspiked and spiked drinking and river water are shown. Copyright © 2017 Elsevier B.V. All rights reserved.

Simultaneous quantification of the major bile acids in artificial Calculus bovis by high-performance liquid chromatography with precolumn derivatization and its application in quality control.

PubMed

Shi, Yan; Xiong, Jing; Sun, Dongmei; Liu, Wei; Wei, Feng; Ma, Shuangcheng; Lin, Ruichao

2015-08-01

An accurate and sensitive high-performance liquid chromatography method coupled with ultralviolet detection and precolumn derivatization was developed for the simultaneous quantification of the major bile acids in Artificial Calculus bovis, including cholic acid, hyodeoxycholic acid, chenodeoxycholic acid, and deoxycholic acid. The extraction, derivatization, chromatographic separation, and detection parameters were fully optimized. The samples were extracted with methanol by ultrasonic extraction. Then, 2-bromine-4'-nitroacetophenone and 18-crown ether-6 were used for derivatization. The chromatographic separation was performed on an Agilent SB-C18 column (250 × 4.6 mm id, 5 μm) at a column temperature of 30°C and liquid flow rate of 1.0 mL/min using water and methanol as the mobile phase with a gradient elution. The detection wavelength was 263 nm. The method was extensively validated by evaluating the linearity (r(2) ≥ 0.9980), recovery (94.24-98.91%), limits of detection (0.25-0.31 ng) and limits of quantification (0.83-1.02 ng). Seventeen samples were analyzed using the developed and validated method. Then, the amounts of bile acids were analyzed by hierarchical agglomerative clustering analysis and principal component analysis. The results of the chemometric analysis showed that the contents of these compounds reflect the intrinsic quality of artificial Calculus bovis, and two compounds (hyodeoxycholic acid and chenodeoxycholic acid) were the most important markers for quality evaluating. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simplified Paper Format for Detecting HIV Drug Resistance in Clinical Specimens by Oligonucleotide Ligation

PubMed Central

Panpradist, Nuttada; Beck, Ingrid A.; Chung, Michael H.; Kiarie, James N.; Frenkel, Lisa M.; Lutz, Barry R.

2016-01-01

Human immunodeficiency virus (HIV) is a chronic infection that can be managed by antiretroviral treatment (ART). However, periods of suboptimal viral suppression during lifelong ART can select for HIV drug resistant (DR) variants. Transmission of drug resistant virus can lessen or abrogate ART efficacy. Therefore, testing of individuals for drug resistance prior to initiation of treatment is recommended to ensure effective ART. Sensitive and inexpensive HIV genotyping methods are needed in low-resource settings where most HIV infections occur. The oligonucleotide ligation assay (OLA) is a sensitive point mutation assay for detection of drug resistance mutations in HIV pol. The current OLA involves four main steps from sample to analysis: (1) lysis and/or nucleic acid extraction, (2) amplification of HIV RNA or DNA, (3) ligation of oligonucleotide probes designed to detect single nucleotide mutations that confer HIV drug resistance, and (4) analysis via oligonucleotide surface capture, denaturation, and detection (CDD). The relative complexity of these steps has limited its adoption in resource-limited laboratories. Here we describe a simplification of the 2.5-hour plate-format CDD to a 45-minute paper-format CDD that eliminates the need for a plate reader. Analysis of mutations at four HIV-1 DR codons (K103N, Y181C, M184V, and G190A) in 26 blood specimens showed a strong correlation of the ratios of mutant signal to total signal between the paper CDD and the plate CDD. The assay described makes the OLA easier to perform in low resource laboratories. PMID:26751207